TW201100483A - Rubber compounding oil, aromatic compound-containing base oil, and methods for producing same - Google Patents

Abstract

Disclosed is a rubber compounding oil which has a total aromatic fraction of not less than 50% by mass as determined according to ASTM D2007 or ASTM D2549, a flash point of not less than 250 DEG C, a difference between the pour point and the glass transition point of not less than 45 DEG C, a benzo(a)pylene content of not more than 1 ppm by mass, and a total content of the specific aromatic compounds (1)-(8) listed below of not more than 10 ppm by mass. (1) benzo(a)pylene (BaP) (2) benzo(e)pylene (BeP) (3) benzo(a)anthracene (BaA) (4) chrysene (CHR) (5) benzo(b)fluorancene (BbFA) (6) benzo(j)fluorancene (BjFA) (7) benzo(k)fluorancene (BkFA) (8) dibenzo(a,h)anthracene (DBAhA)

Description

201100483 VI. Description of the Invention: [Technical Field of the Invention] The present invention relates to a method for producing a rubber blending oil, an aromatic-containing base oil, and the like. [Prior Art] The high aromatic mineral oil has high affinity with the rubber component, and the rubber composition is excellent in processability, softening property, and economy, and is therefore used for the production of a rubber composition such as natural rubber or synthetic rubber. For example, in a synthetic rubber such as SBR (styrene_butadiene rubber), blended with an extender oil during the synthesis, in a rubber processing product such as a tire, in order to improve the workability or The quality of the rubber-processed product is blended with process oil (for example, Patent Document 1). On the other hand, in Europe, since 2010, the following regulations have been applied: It is forbidden to use DMSO (dimethylsulfoxide, dimethyl sulfoxide) extracts or specific carcinogenic polycyclic aromatic compounds in S. Tire or tire parts. Therefore, the vacuum distillation fraction is extracted with a polar solvent, and the extract of the %• usually has a high content of the polycyclic aromatic component, and as a result of the above, it cannot be used as a rubber blending oil as it is. Therefore, rubber blending oils that meet these requirements are required. As a rubber blending oil which conforms to such a regulation, Patent Document 1 proposes a petroleum-based processing oil having an aromatic hydrocarbon content (CA) of 20 to 35 wt%, a glass separation, and a shift point Tg of _55. (:~-30. (:, dynamic viscosity (i) (TC) is 2〇~5〇mm2/s and the polycyclic aromatic component (pcA) is less than or equal to 3% of the petroleum-based weiwei oil. The petroleum-based processing oil will be blended into the diene rubber to obtain 147202.doc 201100483 Grip rubber for tires, which can satisfy both low fuel consumption and properties, and can improve heat aging resistance or Heat-resistant abrasion resistance. However, it is known that it is a light-weight oil, and a base oil containing a high-grade group containing _ or deasphalted oil (deas-hearted solvent extract) is known (for example, Patent Document 2). The solvent extraction in the distillation column is often in the form of a multi-cycle material group, and it is not possible to use it as a rubber-and-oil combination oil due to the above-mentioned regulations. As a response to this condition, it is known that A method for increasing the yield of an aromatic compound by a hydrogenation treatment of a low aromaticity or a polycyclic aromatic dilution effect. As such methods, there are the following concerns: due to the addition of hydrogenation equipment; Deterioration, or low aromaticity, or secondary production of lubricating base oil

The rate has deteriorated. On the other hand, in order to improve the handling property or the handling property, it is required that the rubber blending oil has a flash point (above 250 ° C) as a target of the fourth petroleum which is a dangerous substance. w In order to improve the low temperature properties of rubber (low temperature elastic modulus, etc.), the glass transition point of the rubber blending oil is lowered. For example, in the middle, a rubber blending oil having a glass transition point of ... 吖 and ^ and lower is proposed. The transfer point of the 吊 hanging glass exhibits the opposite characteristic to the aromatic content. Therefore, it is generally difficult to satisfy both the high aromatic component and the low glass transition point. . For example, a rubber blending oil having an aromatic component of 5% by mass or less and having a glass transition point of less than (for example, / ', Example of Patent Document 3, Comparative Example) cannot be obtained. X also has the following tendency: 147202.doc 201100483 The lower the glass transition point of the rubber blending oil, the not only the aromatic component, but also the lower the flash point. Here, the highly aromatic-containing group usually containing an unpurified extract has a higher 'flow point' and a higher glass transition point. Further, the wetting/month oil base oil obtained by purifying the residue by subjecting to a solvent extraction by polar solvent extraction, although having a lower pour point, has a lower aromatic content and an aniline point. It is particularly difficult to use in the dilution oil used in the manufacture of SBR or the like. Thus, as a method for producing a non-carcinogenic rubber blending oil, for example, a k-process has been prepared, a hydrogenation treatment is carried out to reduce polycyclic aromatics = a method; and a production method (2) is carried out by using a polar solvent. The step of increasing the yield of the extract, and the method of diluting the polycyclic aromatic compound; and the method of the production method (7), the solvent extraction of the vacuum fraction is carried out in two stages of the knife 2). ^ Also, as such a base oil containing aromatics, if the flash point is 25 〇, it becomes a target of the fourth petroleum class of dangerous materials, and the operation becomes easy. The flash point. Further, a rubber blending oil having a lower glass transition point has also been proposed (for example, Patent Documents 1 and 3). 'Where' is proposed in Patent Document 1 as a rubber blending oil blended in a diene rubber, using an aromatic hydrocarbon content (CA) of 20 to 35 wt%, a glass transition point of _ hunger ~ _30 t a petroleum-based oil with a dynamic viscosity (1〇(rc)A2〇~5〇面/S and a polycyclic aromatic component (pCA) of 3% by weight or less. The right will be blended with the second rare rubber. The rubber obtained by processing the oil is used for the tire, and the low fuel consumption and the anti-slip property can be satisfied at the same time, and the heat aging property or the heat and abrasion property of the kiln can be raised. The prior art document patent document patent document 1: Japanese Patent Publication No. 2004-155959, Patent Document 2: Japanese Patent No. 3658155, Patent Document 3: International Publication No. 97/35462, SUMMARY OF THE INVENTION PROBLEMS TO BE SOLVED BY THE INVENTION However, the above manufacturing method (1) There is a tendency that the economy deteriorates with the addition of the hydrogenation apparatus, and the aromatic content of the obtained product decreases; there is a tendency in the production method (2) that the yield of the lubricating base oil obtained from the raffinate is lowered, And its aromatic content is also reduced Low. There is also a tendency in the production method (3): although the density is less than 94.94 g/cm3, the polycyclic aromatic is less, the yield of the extract as a highly aromatic component is greatly reduced, and the fragrance thereof is aromatic. The content of the family is also reduced. Thus, the raffinate and the extract obtained by the polar solvent extraction method, which are divided into raw materials by subtracting M, are respectively produced in high yield with a high flash: low glass transition point, and The method of the aromatic-containing base oil having a high total aromatic component and a specific reduction of the aromatic-containing base oil is particularly effective in obtaining an extract from a rubber blending oil or a substrate thereof: = (4) The method of obtaining the S oil or the base oil and the turbid oily aromatic-containing base oil is still unknown. The non-carcinogenicity paid by the stool is therefore the first object of the present invention. Providing a rubber blending oil and a rubber blending oil which maintain a high total aromatic content of 147202.doc 201100483 and having a high flash point and a low glass transition point, and the content of the specific polycyclic aromatic compound is sufficiently reduced Manufacturing method. Further, the second object of the present invention A raffinate and an extract obtained by a polar solvent extraction method using a vacuum distillation fraction to provide a high flash point, a low glass transition point, a high total aromatic component, and a carcinogenic substance a reduced aromatic-containing base oil; and a method for producing an aromatic-containing base oil capable of producing such an aromatic-containing base oil in high yield. Technical Solution to Problem In the first aspect of the present invention, A rubber blending oil having a total aromatic content of 5% by mass based on ASTM D 2007 or ASTM D 2549. The upper and flash points are 25 (TC or more, and the difference between the flow point and the glass transition point is 45 C or more. The total content of the specific aromatic compound in which the content of benzo(a)pyrene is i or less and the following 1) to 8) is 丨〇 mass 卯 or less. 1) Benzo(a)pyrene (BaP) 2) Benzo(e)pyrene (BeP) 3) Benzo(a)pyrene (BaA) 4) Chopsticks (CHR) 5) Stupid (b) alkadiene苐(BbFA) 6) Stupid (1) Propadiene (BjFA) 7) Benzo(k)propadienyl ruthenium (BkFA) 8) Dibenzo(a,h) oxime (DBAhA) The above-mentioned invention The rubber blended oil maintains a high total aromatic content, and 147202.doc 201100483 has a high flash point and a low glass transition point, and the content of the specific polycyclic aromatic compound is sufficiently reduced. Preferably, the rubber blending oil of the present invention contains at least an aromatic-containing base oil (b) in the aromatic-containing base oil (a) and the aromatic-containing base oil (b); The aromatic base oil (a) contains a raffinate obtained by separating a vacuum distillation residue of an atmospheric crude distillation residue oil of a crude oil by a solvent extraction step or a purified oil thereof, and the dynamic viscosity of 40 C is 6 〇 6 6 〇. 〇mm2/s, aniline point is 7〇. (^ above, by GC (Gas Chromatography, gas chromatography) distillation

The 10% point is 400 to 500. (:, 90% point is 5〇〇~600°C, according to ASTM D 323 8% (^ is 3~20, glass transfer point is _3〇〇c or less; the above-mentioned base oil containing aromatic bismuth (b) The extract or the purified oil thereof is obtained by separating the vacuum distillation fraction of the atmospheric distillation residue oil by a solvent extraction step, and the dynamic viscosity of 4 〇r is 200 mm 2 /s or more, and the aniline point is 9 〇 β (: The density of the following 15 art is 0.94 g/cm or more, and the total aromatic content of the astm D 2549 is 30 or more; the content of the aromatic-containing base oil (4) is "mass (4), and the aromatic-containing base oil Further, in the present invention, it is preferred that the solvent extraction step has a U-volume extraction step and a second solvent extraction step, and a second solvent extraction step at the bottom temperature. The first raffinate and the first extract are obtained by contacting the vacuum distillation fraction with the polar solvent in a first take-up column of 30 to 90 t, the temperature of the column top is higher than the temperature of the bottom of the column, and a second solvent extraction step. In the second extraction tower at the bottom temperature and the tower, the temperature is higher than the first extraction tower (10) or higher, the second extraction tower is The solvent is contacted to obtain the second raffinate and the second extract; the aromatic-containing base oil (b) contains the second extract or its purified oil. 147202.doc 201100483 Further, the present invention provides a rubber blending oil. a manufacturing method comprising blending an aromatic-containing base oil (4) and an aromatic-containing base oil (b): a step: the aromatic-containing base oil (a) comprises a crude oil by a solvent extraction step a raffinate obtained by separating a vacuum distillation residue of atmospheric distillation residue oil or a purified oil thereof, and having a dynamic viscosity of 40 to 600 mm 2 /s at 40 C and an aniline point of 7 〇 0 (: above, by GC distillation 1〇% points are 4〇〇~5〇〇t:, 9〇% points are 500~60 (TC, % according to ASTM D 3238 (^ is 3~2〇, glass transfer defect is _3 (rC below) The aromatic-containing base oil (b) contains the extract obtained by separating the vacuum distillation fraction of the atmospheric distillation residue oil by a solvent extraction step or a purified oil thereof, and 4 (the dynamic viscosity of the TC is 200 mm 2 /s) Above, aniline point

The density of 90C or less, 15C is 0_94 g/cm3 or more, and the total aromatic content of astM D 2549 is 30% by mass or more; the total aromatic content of the above rubber blended oil according to ASTM D 2007 or ASTM D 2549 is 50. Above 〇/〇, the flash point is 25 0. (3 or more, the difference between the flow point and the glass transition point is 45 C or more, the content of benzo (a) hydrazine is 1 mass ppm or less, and the content of the specific aromatic compound of the lower Q 丨) to 8) is The content of the aromatic-containing base oil (a) exceeds 〇 and 95% by mass or less and the content of the aromatic-containing base oil (b) is 5% by mass or more and less than 1% by mass. 1) Benzo(a)pyrene (BaP) 2) Benzo(e)pyrene (BeP) 3) Benzo(a)pyrene (BaA) 4) Chopsticks (CHR) 5) Benzo(b)propadiene (BbFA) 147202.doc -9- 201100483 6) Benzo(1)propadienyl ruthenium (BjFA) 7) Benzo(k)propadienyl (BkFA) 8) Dibenzo(a,h)蒽(DBAhA) The total aromatic component blended by the rubber obtained by the above-described production method of the present invention, and having a high flash point and a low glass transition point: and the content of the specific polycyclic aromatic compound is sufficiently reduced. Further, in the rubber blended oil containing the aromatic-containing base oil (b), the difference between the flow point and the surface transfer point is 45 t or more, particularly, the difference is equal to or higher than the difference, so that the total aromatic component is 50% by mass or more. The flow point is above, and a rubber blending oil having a glass transition point of -45 ° C or less can also be obtained. Further, since the aromatic-containing base oil (b) is not subjected to purification such as dewaxing treatment or hydrogenation treatment, it is also excellent in economy. In a second aspect of the present invention, there is provided a method for producing an aromatic-containing base oil, comprising a second solvent extraction step and a second solvent extraction step; and a solvent extraction step at a bottom temperature of 3 () ~ ah, the first extraction tower with the temperature of the top of the column above the temperature of the bottom of the column, the vacuum distillation fraction of the atmospheric distillation residue of the crude oil is contacted with the polar solvent to obtain the third extract and the third extract, 2 a solvent extraction step, wherein the second raffinate is obtained by contacting the third raffinate with the polar solvent in the second extraction column having a bottom temperature and an overhead temperature higher than 10 ° C higher than the first extraction column; The density with 15t is 〇.94 g/cm3 or more and the total aromatic component is 30 mass. /. The above second extract; the aromatic base-containing base oil contains at least a part of the second extract, the second raffinate or the purified oil thereof, and the total aromatic component is 30% by mass or more. According to the present invention, a high flash point can be produced in a high yield, and the glass transition point H7202.doc -10·201100483 is low. An aromatic group having a high total aromatic component and a sufficiently reduced content of a specific carcinogenic substance. oil. Such an aromatic-containing base oil can be preferably used as a rubber blending oil or a raw material thereof. In the present invention, it is preferred that after the second solvent extraction step, a step of preparing a base oil obtained by subjecting the second raffinate to a purification treatment including a dewaxing treatment to obtain the purified oil; The pour point is -5. 〇 The following aromatic base oils with a stupid amine point of 9 〇 ° C or more, a viscosity index of 9 〇 or more, and a flash point of 250 ° C or more. In the present invention, it is preferred that after the second solvent extraction step, a step of preparing a base oil obtained by subjecting the second residue to a purification treatment including a dewaxing treatment to obtain a purified oil; 4〇t: The dynamic viscosity is 60~120 mm2/s, and the 10% point by GC distillation is 400~460. (:, 90 ° /. The point is 500 ~ 540 ° C of aromatic-containing base oil. In the present invention, it is preferred to: after the second solvent extraction step, has to remove the second raffinate Purification treatment of the soil treatment to obtain a base oil preparation step of the purified oil; thereby producing a purified oil, having a dynamic viscosity of 40 to 250 mm 2 /s at 40 ° C, and a 10% point of 450 to 520 ° by GC distillation C. 90% of the aromatic-containing base oil of 540 to 600 ° C. It is preferred that the aromatic-containing base oil obtained by the production method of the present invention contains at least a part of the second extract, 4〇 The dynamic viscosity of t is 2〇〇mm2/s or more, the flash point is 25〇〇c or more, the flow point is below 3〇〇c, the stupid amine point is below 90°C, and the glass transition point is -3〇°C. Hereinafter, the difference between the flow point and the glass transition point is 50. (: The above. Further, the aromatic-containing base oil may include the second extract. 147202.doc -11 - 201100483 Preferably: by the present invention The aromatic-containing base oil obtained by the production method contains at least a part of the second extract, and the dynamic viscosity of 4〇〇c is 2〇〇mm /s or more and is not 500 mm2 / s, and the glass transfer point is _6 〇 ~ _4 (Γ (:. This S ^ • Xiang Li Ya base oil can be used particularly well as petroleum processing oil or dilution oil 'the above petroleum processing oil Or the diluent oil is blended into at least one of, for example, NR 'natural rubber, various butadiene rubber (BR), various styrene butadiene rubber (SBR), A diene rubber such as an isoprene rubber (IR), a butyl rubber (BR), or any of these mixed rubbers, particularly a diene rubber of a styrene-butadiene copolymer rubber. Further, the aromatic-containing base oil may contain the second extract. Preferably, the aromatic-containing base oil obtained by the production method of the present invention contains at least a part of the second extract, 40. The dynamic viscosity is 500 mm 2 /s or more 'and the glass transition point is _5 〇 _ _ 3 〇 ° C. Such an aromatic-containing base oil can be particularly preferably used for blending into the diene rubber, for example, as described above. Petroleum processing oil or diluent oil. Further, the aromatic-containing base oil may include 2. The extract is preferably a content of benzo(a)pyrene of the aromatic-containing base oil obtained by the production method of the present invention of 1 mass ppm or less, and 1) to 8) shown below. The total content of specific aromatic compounds is 1 〇 mass ppm or less: 1) benzo(a)pyrene (Bap) 2) benzo(e)pyrene (BeP) 3) benzo(a)pyrene (BaA) 4) chopsticks (CHR) 147202.doc •12- 201100483 5) Benzo(b)propadienyl (BbFA) 6) Benzo(1)propadienyl ruthenium (BjFA) 7) Benzo(k)propanedipine (BkFA) 8) Dibenzo (a, h) hui (DBAhA). Since the aromatic-containing base oil is sufficiently reduced in the content of the carcinogenic polycyclic aromatic compound, it can be suitably used as a petroleum-based processing oil or a diluent oil or a base material of a rubber processing product such as a tire. Ο 〇 , The present invention provides an aromatic-containing base oil obtained by the production method having the above characteristics. The base oil of the material group is a high flash point, and the glass transition point is low 'having a high total aromatic component and the content of the carcinogenic substance is sufficiently reduced'. It has excellent as a petroleum processing oil or a diluent oil or a substrate thereof. Features and safety are also excellent. Further, a rubber blending oil containing the aromatic-containing base oil having the above-described third aspect of the present invention is provided. EFFECTS OF THE INVENTION According to the present invention, it is possible to provide a high total aromatic component, a flash point to a low glass transition point, and, a person, an octagonal, a mountain, a < 夕衣方香族 U充 4 Production of a small rubber blending oil and the rubber blending oil / 2 Γ β The rubber blending oil of the present invention is compatible with a rubber or rubber material such as an aromatic vinyl-butadiene rubber:: For example, if the glass transfer point is _57~_4 generation " rubber or rubber material such as lanthanum rubber Μ This ethylene-Ding II is excellent in low temperature properties (4). And / or add oil, it can be used in the field of flash fire St Gu P · 丄 8 o'clock, carcinogenic 147202.doc -13- 201100483 polycyclic aromatic compounds content is fully reduced, so safety is also good. In particular, as described in Patent Document 1, the aromatic hydrocarbon content (Ca) is 20 to 35 mass% (synonym with 0/35 according to ASTM D 3238), and the glass transfer point is -55. °C~-3 (TC, kinetic viscosity (l〇(TC) is 20~50 mm / s rubber blending oil, blended into at least i kinds of such as natural rubber (NR), various butadiene rubber (BR), various styrene butadiene copolymer rubber (SBR), polyisoprene rubber (IR), butyl rubber (BR), and any other mixed rubber such as diene rubber, especially styrene In the diene rubber of the butadiene copolymer rubber, the rubber thus obtained is used for a tire, whereby both low fuel consumption and slip resistance can be satisfied, and the length can be long: heat aging resistance or thermal abrasion resistance of the horse Moreover, according to the present invention, the raffinate and the extract obtained by the polar solvent extraction method which is a raw material for distillation under reduced pressure can provide a high flash point, a low break point of the glass, and a high total aromaticity. An aromatic-containing base oil having a reduced content of a family component and a carcinogenic substance. Further, it can be provided to produce the product in high yield. A method for producing an aromatic-containing base oil containing an aromatic base oil. [Embodiment] Hereinafter, preferred embodiments of the present invention will be described with reference to the drawings. The rubber blending oil of the present embodiment is The rubber has excellent affinity, softening property, flash point, and safety, and the characteristics of the rubber composition such as low fuel consumption, anti-slip property, heat aging resistance, and heat-resistant wear resistance are high. Character. According to ASTM D 2007 (Clay_Gel Meth〇d) aroma 147202.doc •14- 201100483 Group composition: usually 50~90 mass. /, preferably more than 55 mass%, better The 疋57 mass% or more, particularly preferably 6 〇 mass% or more; preferably 80 mass% or less, more preferably 7% by mass or less. According to AST] VI D 2007 (clay glue method) saturation Ingredients: usually 5 to 5 〇 里 〇 / 〇, preferably 1 〇 by mass or more, more preferably 2 〇 by mass or more, more preferably 疋 40% by mass or less, more preferably 3 〇 by mass% Following. According to the polarity of ASTM D 2〇〇7 (clay method) The compound component: usually 〇 is 1 to 2% by mass, preferably 2 parts by mass or more, more preferably 5% by mass or more; more preferably 15% by mass or less, more preferably 12% by mass or less, Particularly preferably, it is 10% by mass or less. The ratio of the saturated component/polar compound component according to ASTM D 2007 (clay method) is usually 0.25 to 5 Å, preferably 1 or more, more preferably 2 Å or more. Particularly preferably, it is 3 or more; preferably 2 Å or less, more preferably (7) or less, particularly preferably 5 or less. The content of benzo(a)pyrene (BaP) is! In the mass ppm or less, the total content of the specific aromatic compound (PAH) of 〇 1) to 8) shown below is 10 ppm by mass or less. By this, it is possible to produce a rubber-pushing oil which is more safer than the fear of carcinogenicity. 1) Benzo(a)pyrene (Bap) 2) Benzo(e)pyrene (BeP) 3) Benzo(a)pyrene (BaA) 4) Chopsticks (CHR) 5) Benzo(b)propadiene (BbFA) 6) Benzo(1)propadienyl ruthenium (BjFA) 147202.doc -15· 201100483 7) Benzo(k)-propene-ene (β^α) 8) Dibenzo (a, h) ) Onion (DBAhA) is stupid in this month and (a) refers to the benzene (4) You (Β#) of the above i), the aroma of the specific 曰 化 化 & & & & & & & & & & & & Family compound (PAH). These specific aromatic compounds can be prepared by separating and concentrating the target component, and preparing a sample to which an internal standard substance is added, and performing quantitative analysis by GC_MS (gas maSsspectrometry). The flash point is 250 C or more, preferably 26 (rc or more, more preferably 280 ° C or higher; preferably 35 〇 t or less, more preferably 32 〇 t > c or less, especially good 3HTC or lower. In addition, the flash point in this specification refers to the flash point of the Kelvin open cup type (cleveland print (3)卩, COC) measured according to JIS K2265. The difference between the moving point and the glass transfer point is preferably 4 5 or more, preferably 50 ° C or more 'better 疋 6 0 C or more' is particularly preferably 6 5 ° C or more; preferably l 〇〇 ° C or less, more preferably 80 ° Below C. The flow point is preferably below 3 0 C. More preferably, it is below 25 ° C; preferably it is above -10 ° C, more preferably above 5 ° C, especially preferably +10 Above °c, particularly preferably +12 · 5 °c or more. Further, the flow point in the specification means a pour point measured according to JIS K2269. The glass transfer point (Tg) is preferably -30 ° C or less. More preferably _4 (TC or less, especially preferably -45 ° C or less, particularly preferably -48 ° C or less, and further preferably -50 ° C or less; preferably -80 ° C or more, Better yet is _60. (: Above, especially good - Above 55 °C.

"Glass transfer point (Tg)" in this specification refers to the temperature rise at a certain temperature increase rate (1 o °c / min) by DSC 147202.doc -16·201100483 (differential scanning calorimeter) The measured glass transition point based on the change in the heat of the glass transition region. The initial temperature is usually set to a temperature lower than or lower than the expected glass transition point by about 30 ° C to 50 ° C, and the temperature is raised after maintaining the initial temperature for a certain period of time. In the present embodiment, 'specifically' can be measured by the following conditions. Device: Thermal analysis system manufactured by TA Instruments, Dsc q1〇〇 Initial temperature: -90 ° C, maintained for 1 〇 minutes Heating rate: 10 ° C / min End temperature: 50 ° C, kept for 1 〇 minutes, according to heat The method of calculating the glass transition point by changing the peak can be determined by the method described in JIS K7 121. The degree of detection of 15C is usually 〇9 g/cm3~l.0 g/cm3, preferably 〇94 g/cm or more 'more preferably 〇945 g/cm3 or more; preferably 〇% g/ Below cm3, more preferably 0.96 g/cm3 or less. The dynamic viscosity of 4〇C is usually 2 00~3000 mm2/s, preferably 3〇〇mm2/s or more, more preferably 4〇〇mm2/s, especially preferably 5〇〇mm2/s or more. It is preferably 2000 mm 2 /s or less, more preferably 1 〇〇〇 or less 'especially _ mm 2 / s or less. In addition, the dynamic viscosity of each temperature referred to in the present specification means the dynamic viscosity of each temperature measured in accordance with JIS K 2 2 8 3 . & The dynamic viscosity at 100 ° C is usually 10 to 100 mm 2 / s, more preferably 15 mmVs or more 'especially better than 2 〇 mm 2 / s; preferably 6 〇 2 or less 'better 50 Mm2/s, especially preferably below 32 mm2/s. 147202.doc -17- 201100483 The aniline point is usually 50 to 100 ° C, preferably 6 〇 t or more, more preferably 65 ° C or more, and particularly preferably 70. (: Above; preferably 9 (rc or less, more preferably 疋85 C or less. Further, the aniline point in the present specification means an aniline point measured in accordance with JIS K 2256-1985. The nitrogen component is usually 0. 01 to 0.2% by mass, preferably 〇〇3% by mass or more, particularly preferably 0.05% by mass or more; more preferably 〇15% by mass or less, more preferably Μ% by mass or less. The nitrogen component in the specification means a nitrogen component of a chemiluminescence method measured in accordance with JIS Κ 2609. The %CN is usually 5 to 30, preferably 1 Å or more, more preferably "above," preferably 25 or less. More preferably, it is 2〇 or less. %Ca is usually 1〇~4〇, the car is better than 17疋, more preferably 2〇; better is “below, better is 30 or less, especially Preferably, it is 25 or less. The %Cp is usually 3〇~85, preferably 4G or more, more preferably it is above; preferably it is below, more preferably 66 or less. Furthermore, 'in this specification' %.,%(:Ν and %. Except for the special case, it is obtained by the method of astm D 3U讧85 (n_d_M ring analysis). The percentage of the carbon number of the alkane relative to the total carbon number, the percentage of the carbon number of the ring burned to the total Wei, and the percentage of the aromatic carbon number to the total carbon number.

The total aromatic component is usually from 3 Torr to 9 9% by mass, preferably 4 Å by mass, more preferably 50% by mass or more, more preferably 8% by mass or less, and preferably 70% by mass. the following. Further, the total aromatic content in the present specification means the content of the aromatics fraction measured in accordance with ASTM D or AS D 2549, unless otherwise specified. The rubber blending oil of the present embodiment contains an aromatic-containing base oil (4) and a 147202.doc -18-201100483 fragrant base oil (b), and the base oil (a) containing the scented aromatic base contains a solvent The extracting step is a raffinate obtained by separating a vacuum distillation fraction of a crude oil atmospheric distillation residue oil or a purified oil thereof, and contains 4 Torr. (: The dynamic viscosity is 6〇~600 mm2/s, the aniline point is 7 (TC or more, 1% by Gc steaming is 400~500°C, 90% is 500~600°C, according to ASTM D 3238 has a %CA of 3 to 20, an aromatic-containing group having a glass transition point of less than jot/the above-mentioned aromatic-containing base oil (b) contains a waste distillation residue by a solvent extraction step The extract obtained by vacuum distillation of the fraction or the purified oil thereof has a dynamic viscosity of 200 mm 2 /s or more and a aniline point of 9 〇. The density below 15 ° C is 〇·94 g/cm 3 or more. The total aromatic component of ASTM D 2549 is 30% by mass or more. Hereinafter, the aromatic-containing base oil (a) (hereinafter referred to as base oil (a)) and the aromatic-containing base oil are hereinafter referred to as hereinafter. The base oil (b) is described. The base oil (a) is preferably a total aromatic obtained by purifying the second raffinate obtained by the second solvent extraction step and the second solvent extraction step. The bismuth component is 30% by mass or more of the aromatic-containing base oil; the first solvent extraction step is at the bottom temperature of 30 to 90. (:, the temperature at the top of the column is higher than the temperature at the bottom of the column. In the extraction tower, the waste reduction steam storage of the crude oil of the atmospheric pressure steaming residue is contacted with the polar solvent to obtain the third extract and the third extract; the second solvent extraction step, the bottom temperature and the tower In the second extraction column having a top temperature higher than 1 〇C higher than the second extraction column, the second raffinate is brought into contact with the polar solvent to obtain a second raffinate having a density of 0.94 g/cm 3 or more at 15 ° C. The total extract is a second extract having a composition of 30% by mass or more. The base oil (a) is preferably subjected to purification treatment of the second raffinate including dewaxing treatment 147202.doc •19·201100483 The aromatic base oil obtained, and preferably has a dynamic viscosity of 40 to 120 mm 2 /s at 40 ° C, a 10% point by GC distillation of 400 to 460 ° C, and a 90% point of 500 to 540 The base oil (al) at °C and/or the dynamic viscosity at 40 °C is 120~250 mm2/s, the 10% point by GC distillation is 45〇~52〇°C, and the 90% point is 540~600Ό. Base oil (a2). Further, the base oil (b) is preferably 4 (TC has a dynamic viscosity of 200 mm 2 /s or more, a flash point of 250 ° C or more, a pour point of 30 ° C or less, and an aniline point. For 90 ° C or less, glass turn The shift point is -3 (the aromatic-containing base oil having a difference of TC or less and a difference between the flow point and the glass transition point of 45 ° C or higher. The base oil (b) is preferably a dynamic viscosity of 4 cmTC of 200 mm 2 /s or more. An aromatic base oil (bl) and/or 4 with a glass transition point of less than 500 mm2/s and a glass transition point of _60~_4〇°c (the dynamic viscosity of the TC is 500 mm2/s or more, and the glass transition point is - Aromatic base oil (b2) at 50 to -30 °C. Preferred properties of the above base oil (a) and base oil (b) are explained in detail. The base point of the base oil (a) is preferably 〇. 〇The following, can be less than _2. Hey. However, from the viewpoint of the manufacturing cost of the rubber blending oil, the flow point of the base oil (a) is more preferably -10 to 2 Torr. (: By using a base oil (_) with a pour point of _l (r), it is easy to obtain a rubber blending oil with a lower break point. The base oil (a) has a better glass transfer point. It is _3 〇 以下 below, better is -5 吖 below '· Better is ah above, better _8 generations or more especially good 疋-70 C or more. If the broken glass transfer point is too high, However, there is a tendency to obtain a low viscosity of the glass transfer point. If the glass transition point is too low, the manufacturing cost will increase due to the necessity of excessive enthalpy and controlled dewaxing conditions. 147202.doc '20- 201100483 The base oil (4) aniline point is preferably 7 (rc or more, more preferably 9 〇. Above ,, especially good is loot: above. It is easy to manufacture the preferred aniline From the viewpoint of a rubber blending oil which is excellent in compatibility with rubber and which maintains the properties of the rubber composition, it is preferably 12 〇t or less. As a composition of the base oil (4), % (^ is preferably 3) ~2〇, more preferably 5~10,%. It is preferably 15~35, more preferably 2〇~3〇. Also, the %cP in the base oil (4) is It is determined by m%Ca and %Cn, preferably 45 to 82, more preferably 60 to 75, particularly preferably 65 to 7 G. It is easy to use the base oil (a) having the above composition. A rubber blending oil having a preferred composition to make it compatible with rubber and maintaining the properties of the rubber composition is preferred. The nitrogen component of the base oil (a) is preferably 〇〇1% by mass or less, more preferably 〇. 〇〇8 mass% or less may be less than 5% by mass. However, if a lubricating base oil having a low degree of purification is used, the manufacturing cost of the rubber blending oil can be reduced, so from the viewpoint of economy, Preferably, it is 〇〇〇 2% by mass or more, more preferably 0.003 mass. / 〇 or more. Q The rubber blending oil has a flash point of 250 ° C or more and is a dangerous substance of the fourth petroleum type. In view of the above, the flash point of the base oil (a) is preferably 25 〇 (>c or more, preferably 2551 or more. Further, the flash point of the base oil (b) can be increased. The flash point of the oil (a) is increased to a necessary amount or more, preferably 290 ° C or less, more preferably 28 (rc or less. 90% of the GC distillation of the base oil (a) It is 5 〇〇. (: Above, preferably 500 to 600 ° C. As a base oil (al) of one aspect of the base oil (4), 510 to 550 ° C can be used as the base oil (a) The base oil (a2) of the aspect can be used at 550 to 590 ° C. In addition, the 1% point of the distillation of the base oil (a) is not particularly limited to 147202.doc -21 - 201100483, and the rubber can be blended. The oil winter flash point is 2501 or more, and it is preferably 4 〇〇 5 5 ° °c, and more preferably 440 to 500 ° C, in addition to the object of the fourth petroleum class. As the base oil (ai), 1 〇 0/ of the gc distillation can be used. The point is 440 to 470 ° C, as the base oil (〇, can use the 10% point of GC distillation is 450~500 ° C. Base oil (a) is preferably the above 1) benzo (a) 芘 ( The content of BaJ>) is 1 ppm by mass or less, and it is preferred that the total cerium content of the specific aromatic compound (pAH) described above is 10 ppm by mass or less. Thereby, a rubber blending oil having sufficiently reduced carcinogenicity and higher safety can be produced. The dynamic viscosity of the base oil (a) at 40 ° C is preferably 6 〇 6 6 mm 2 / s, more preferably 60 〜 300 mm 2 / s, especially preferably 7 〇 ~ 2 〇〇 mm 2 / s . Use 40. (: When the dynamic viscosity is less than 2〇〇〇mm2/s base oil (b), in order to obtain the rubber blending oil with better dynamic viscosity, it is better to use the thief's dynamic viscosity to be better 50~500. Mm2/s, more preferably 6〇~8〇mm2/s base oil (al) and/or 12〇~250 mm2/s base oil (a2). Base oil (4) has no special aromatic content The limit is usually 2 (% by mass or more), preferably 30% by mass or more, more preferably 35% by mass or more, more preferably 50% by mass or less, still more preferably 45% by mass or less. (If the total aromatic component is less than 2% by mass, there is a tendency that it is difficult to obtain a rubber blended with aromatic enamel. In another ancient product, the total aromatic content of the base oil (a) exceeds 50 mass. ❶/.,存*人味』Aberdeen in the following tendency: Emulsification stability is reduced when used as a lubricating base oil, it is difficult to use silkworms ^^ is used in lubricating base oils and rubber blending oils, petroleum purification processing The overall economical reduction. Base oil (8) aniline point is better 4 〇 ~ 9 generation 'better is 147202.doc -22- 201100483 45~70 C, especially good 50 to 65 ° C. When the aniline point is in this range, even if a lubricating base oil having a high aniline point is blended, it is easy to produce a preferred aniline point to make it compatible with rubber and maintain the characteristics of the rubber composition. As a component of the base oil (b), %Ca is preferably 25 to 45, more preferably 30 to 40, and %CN is preferably 5 to 20, more preferably 6 to 12. Further, %Cp is determined by /❶cA, %cN, preferably 35 to 7〇, more preferably 48 to 64. If the composition of the base oil (b) is in the above range, even the blended chain The base oil (a)' having a high degree of alkane can also easily produce a rubber blending oil having a preferable composition to make it compatible with rubber and maintaining the properties of the rubber composition. The nitrogen component of the base oil (b) is preferred. It is 0.01% by mass or more, more preferably 〇·〇5 by mass. /〇 or more, particularly preferably 〇1% by mass or more, particularly preferably 〇.15% by mass or more. The base oil (b) has a high nitrogen content. The nitrogen component of the raffinate obtained by the solvent extraction step is lowered, and the degree of purification of the lubricating base oil is improved. Therefore, all of the reduction can be effectively utilized. In terms of distillate fraction, it is preferred to use a base oil (b) having a high nitrogen content as a rubber blending oil. The base point of the base oil (b) is preferably 30 ° C or lower, more preferably 25 (hereinafter: Further, the base point of the base oil (b) is preferably 5 or more, more preferably i〇c or more 'especially better than 15»c or more 'excellently 2 〇〇c or more. (b) may be an unpurified extract having a high pour point, preferably a glass transition point is lower. The difference between the pour point of the base oil (b) and the glass transfer point (flow point-glass transition point) is better. It is 45 ° C or more, more preferably 50 ° C or more, particularly preferably 55 ° C or more, particularly preferably 60 ΐ: above; preferably i 〇 o ° c or less, more preferably 8 (rc the following. 147202.doc -23- 201100483 The base oil () glass transfer point is preferably _3 〇. [Here, the preferred glass transition point of the aromatic-containing base oil (bl) as a state of the base oil (8) on 疋60 C 且 is ·6()~, as an aromatic containing other aspect The breaking point of the base oil (b2) should be _5〇~_3〇. Further, the base oil (b) is preferably a content of the above-mentioned fluorene (... 芘 (7) 讣) which is ppm or less in the enamel, preferably a specific aromatic compound (PAH) of the above 1} to 8). The total amount of cerium is 1 〇 mass ppm or less. Thereby, a rubber blending oil having a sufficiently reduced carcinogenicity and higher safety can be produced. Further, the flash point of the base oil (b) is not particularly limited, and in order to make the flash point of the rubber blended oil to be more than 250 C or more, it is a target of the fourth petroleum type of the dangerous substance, preferably 250 ° C. The above is more preferably 27 (rc or more, particularly preferably 290 C or more), particularly preferably 3 〇〇. 〇 or more. The total aromatic component of the base oil (b) is preferably 3 〇 by mass%. The above is more preferably 50% by mass or more, particularly preferably 55% by mass or more, particularly preferably 60% by volume or more, more preferably 65% by mass or more; more preferably % by mass or less, more preferably It is 80% by mass or less, and particularly preferably 7% by mass or less. If the total aromatic component of the base oil (b) is less than 5% by mass, it is difficult to obtain the rubber blending oil of the fragrant south. There is a tendency that if the total aromatic component exceeds 9 〇 minus % ', the yield of the extract deteriorates, which is not economically advantageous. Then, the preferred method for producing the rubber blending oil of the present invention is preferred. The embodiment will be described. In the present embodiment, 'the first solvent 147202.doc having the base oil (a) and the base oil (b) is produced. 24-201100483 Extraction step and second solvent extraction step, and blending step of blending the prepared base oil (5) and base oil (b). First, a first solvent extraction step for producing base oil (4) and base oil (8) And the second solvent extraction step will be described. - 帛1 solvent extraction step, in the first extraction column at the bottom of the column at a temperature of 30~90T: at the bottom of the column, the atmospheric distillation of the crude oil The vacuum distillation distillation fraction of the residual oil is contacted with the polar solvent to obtain the third extract and the first extract. The second solvent is extracted (four), and the ratio of the bottom temperature to the top temperature is higher than that of the first extraction tower. The second extraction column t above °C, the first raffinate is brought into contact with the polar solvent, and the second raffinate is obtained and the density at 15 ° C is 〇.94 g/cm 3 or more and the total aromatic component is 3 〇. The second extract of the mass % or more. The following describes the details of each step. (First Solvent Extraction Step) FIG. 1 is a first solvent extraction step for explaining the method for producing a rubber blending oil in the present embodiment. And a step diagram of the second solvent extraction step. In the first solvent extraction step, 'first' The vacuum distillation fraction of the crude oil steam distillation residue oil is convectively contacted with the polar solvent in the first extraction column 30 having a bottom temperature of 30 to 90 ° C and a column top temperature higher than the bottom temperature. Further, it is separated into a working residue and a first extract. The polar solvent is supplied from the pipe 34 to the second extraction column 30. On the other hand, the vacuum distillation fraction is supplied to the [extraction column 30] through the pipe 16. Vacuum distillation The fraction is a fraction obtained by introducing a normal crude distillation residue of a crude oil into a vacuum distillation apparatus. The vacuum distillation fraction is not particularly limited, and a light lubricating oil fraction, a medium lubricating oil fraction, and a heavy lubricating oil can be used. A fraction, or a mixture of these, or all of the reduced pressure distillation fractions. For the purpose of raising the flash point of the aromatic-containing base oil of the final 147202.doc -25·201100483, and the aromatic-containing base oil having an appropriate viscosity range without increasing the viscosity, for example, Use 200~1500 N, preferably 25〇~12〇〇N', more preferably 3〇〇~6〇〇n or 600~1200 N lube fraction. In addition, "n" in the present specification means a neutral oil obtained by distilling a distillation residue under reduced pressure. For example, if it is 3 〇〇N, it means 10 (TF (37.8t) has a viscosity of 300 Saibo seconds ( Sayb〇h second, SUS) ° In the present embodiment, the base oil (a) is 200 to 1500 N, preferably 250 to 600 N or 600 to 1200 N, more preferably 300 to 45 Å] ^ or 7〇〇~1〇〇〇N viscosity' is preferred to select a vacuum distillation fraction. The temperature of the bottom of the i-th extraction column used in the first solvent extraction step is preferably 30 to 90 ° C. Preferably, it is 50 to 70. Preferably, it is 55 to 65: The temperature of the top of the first extraction column 30 is higher than the temperature of the bottom of the column, preferably 10 to 50 ° C, more preferably high. 15~40°C, especially good is 25~35t:. Specifically, the temperature at the top of the tower is preferably 60~12 (TC, more preferably 80~10 (rc, especially good is 85~95) °C. As for the solvent ratio in the first solvent extraction step, it is preferably 〇5 to 3, more preferably 疋0.7 to 2, particularly preferably 1 to 丨5. Further, the solvent ratio in the present specification ” refers to the volume ratio of solvent to raw material (solvent volume) / raw material volume). Under the above conditions, the internal polar solvent in the i-th extraction column 3 is convectively contacted with the reduced-pressure rectification fraction, and the first extract is obtained from the bottom of the i-extraction column 3 through the pipe U. a mixture with a polar solvent, a mixture of the ith raffinate and the polar solvent is obtained from the top of the column through the pipe 36. Further, the mixture is taken from a mixture of the polar solvent and the polar solvent. In the fractionation column, the first extract and the polar solvent are separately divided. Further, the mixture of the i-th residue and the polar solvent may be fractionated into a third-stage raffinate and a polar solvent in a fractionation tower not shown, or may not be The fractionation is carried out and introduced directly into the second extraction column 40.

In the fractionation column (not shown), the polar solvent fractionated by the first extract and the third residue can be recovered and reused. Examples of the polar solvent include polar solvents such as furfural, phenol, cresol, cyclobutyl hydrazine, N-methylpyrrolidone, dimethyl hydrazine, methyl morpholine, and a glycol solvent. In the present embodiment, it is preferred to use furfural as it is possible to directly use the solvent extraction apparatus of a usual lubricating base oil. As described above, in the first solvent extraction step, the vacuum distillation fraction is separated into the first raffinate and the first extract. The yield of the first raffinate obtained in the first solvent extraction step is preferably 0.5 to 9% by volume, more preferably 60 to 85% by volume, based on the vacuum distillation fraction, and particularly preferably 7〇~8〇 volume%. The yield of the third extract obtained in the first solvent extraction step is based on a vacuum distillation fraction, preferably from 1 to 5 % by volume, more preferably from 15 to 4 % by volume, particularly preferably 20~3〇 volume 0/〇. By extracting a specific aromatic compound (PAH) to be described later on the i-th extract side by the first solvent extraction step, the second extract of the second stage, the second raffinate, and the like can be sufficiently reduced. The content of the specific aromatic compound (pah) of the aromatic-containing base oil obtained "In addition, since the first extract contains a special aromatic compound (PAH)", it is not suitable for lubricating base oil or rubber blending. The tendency to blend oil. Therefore, the yield of the first extract is, for example, 3 Torr. /. In the following, the second raffinate and the second extract which are used as a lubricating base oil or rubber 147202.doc -27- 201100483 rubber blending oil or a substrate thereof can be obtained in high yield, for example, by vacuum distillation under reduced pressure. In the distillation standard, the total amount of the second raffinate and the second extract may be 70% by volume or more. The method for producing the aromatic-containing base oil of the present embodiment can be said to be effective in terms of effective use of resources. Extremely useful. In the second solvent extraction step, the first raffinate obtained in the second solvent extraction step or the mixture of the first raffinate and the polar solvent and the polar solvent are introduced from the pipe 36 and the pipe 44 to the second extraction column 4, respectively. In the crucible, the first raffinate is brought into contact with the polar solvent in the second extraction column 4 crucible. The second extraction column 4 is higher than the third extraction column 30, and the temperature at the bottom of the column and the temperature at the top of the column are each higher than 1 tt. The bottom temperature of the second extraction column 4 used in the second solvent extraction step is higher than the bottom temperature of the i-th extraction column 3 in the first solvent extraction step by 1 〇 t: or more, preferably 10 ° higher. 50 ° C, better is 15 ~ 40t high: ' Especially good is high 20 ~ 3 〇 t:. Specifically, the temperature of the bottom of the second extraction column 4 is preferably from 2 to 40 ° C, more preferably from 60 to 10 (TC, particularly preferably from 8 to 95 C > c. Further, the second extraction The temperature at the top of the column 40 is preferably 10 to 50 ° C higher than the temperature at the bottom of the column, and more preferably 15 to 4 (rc, particularly preferably 25 to 35 ° C. Specifically, The temperature of the top of the second extraction column 4 is preferably from 50 to 150 ° C, more preferably from 80 to 140 ° C, particularly preferably from 11 to 13 ° t: the solvent in the second solvent extraction step. Preferably, it is 1 to 4, more preferably 1.3 to 3.5, particularly preferably h5 to 3·3. The dissolution in the second solvent extraction step is preferably set to the solvent ratio in the first solvent extraction step. 15 times or more. Under the above conditions, the internal polar solvent in the second extraction column 40 is in convective contact with the first raffinate' from the bottom of the second extraction column 40 through the pipe 48 to obtain 147202.doc • 28·201100483 A mixture of the second extract and the polar solvent is obtained, and a mixture of the second raffinate and the polar solvent is obtained from the top of the column through the pipe μ. Further, the mixture of the second extract and the polar solvent is not shown. Guta Zhongde is the second extraction. #与极溶剑. In addition, the mixture of the second residue and the polar solvent is divided into the second residue and the polar solvent in the branch. In the illustrated separation column, the polar solvent separated by the second extract and the second raffinate can be recovered and reused. As described above, in the second solvent extraction step, the first raffinate is separated into The second residue and the second extract. The yield of the second raffinate obtained in the second solvent extraction step is based on the W residue introduced into the second extraction column 40, preferably 5G~ The % of the electromotive product is more preferably from 6 to 85 % by volume, particularly preferably from 70 to 85% by volume. The yield of the second extract obtained in the second solvent extraction step is preferably from 1 G to 50% by volume. Preferably, it is 15 to 4% by volume, particularly preferably 15 to 30% by volume. Further, in the present embodiment, it is not necessary to use another extraction column as the first and second extraction columns, and the column can be used as a separate material. The third extraction tower 30 and the second draw tower 4 are 〇. At this time, the raffinate obtained in the first solvent extraction step (preferably, the polar solvent is removed) is stored in advance. In the temporary storage tank or the like, it is introduced into the second extraction column 4 of the strip (4) of the solvent extraction step, and the second solvent extraction step is performed. This can reduce the excessive equipment investment. In the solvent extraction step, the second residue, the second residue having a density of 0.94 gW or more and a total aromatic component of 3% by mass or more can be obtained. If the density of the 15t of the second extract is 〇94 In the above, 147202.doc -29· 201100483 can be used as a rubber product such as a tire having a high total aromatic content, a sufficiently low aniline point, a high flash point, and a difference between a pour point and a glass transition point. A petroleum-based processing oil or a substrate thereof in the manufacturing process, or a diluent oil or a substrate thereof in the manufacturing process of a dilute rubber. At the same time, it is also possible to obtain a total aromatic component of not more than 3% by mass from the obtained second raffinate in a high yield, and also be used as an aromatic-containing oil as a lubricating base oil, a petroleum-based processing oil, a diluent oil or a substrate thereof. Base oil. Brother 2 strokes of the i 5 it < Yi Ding π疋u WU μ work, Wen Hao is 〇 _95 ~ 1 g / cm3, especially good 〇 · 95 ~ 〇 98 § gas melon 3. Also, a total of ϊλ; 43⁄4 L-7 »L· » ^ Λ ^ . — a g/wu. The aromatic component is preferably 30% by mass or more, more preferably 6% by mass%, particularly preferably 80% by mass or more, more preferably 9% by mass or less. In addition, "the total aromatic component" in this specification is a value measured by c 2549. The % of the second extract measured according to ASTM D 214〇. Preferably, 15 to 35 Å is preferably 2 to 33, and particularly preferably 22 to 32. The second extract preferably has the following properties. Flash point: It is better to be 250. (: Above, better is 26 generations or more; preferably 31 〇. (: below. ' • Flow point: preferably 3 〇 ° C or less, more preferably 1 〇 ~ 3 〇 r. Aniline point: It is better to be thief below, better is 4〇~8吖 is 50~70. (:. ” • Glass transfer point: better _赃 below, better _ next, Especially good is -60 ° C or more. • The difference between the flow point and the surface transfer point (flow point. Breaking point): preferably 147202.doc • 30· 201100483 is above 45 °c, better β, More preferably 疋 50. Above, especially good is 55〇c or more, preferably less than loot, more preferably 8 (rc or less.) • Benzo(a) 芘 content: better 丨 quality Ppm or less. • Total content of specific aromatic compound (PAH): preferably (7) ppm by mass or less. Then, by performing the dephosphorization treatment using the anti-ant apparatus 5 and the hydrogenation by using the second raffinate The lubricating oil base oil used as the purified oil can be obtained by purifying and purifying the gasification finishing treatment of the finishing apparatus. The aromatic content can be obtained as such. The oil (lubricating base oil) is used as the base oil (4). Further, the base oil (4) may be a mixture of two or more aromatic-containing base oils (lubricating base oils) obtained in the above manner. The total aromatic component of the oil (4) is preferably Μ% by mass or more 'better 疋3 0~6 0 质 。. Li, 丄 γ, * M w / 〇 base oil (a) is preferably 200~ 1500 better base oil (4) which is above 250 N and not more than 6〇〇N and base oil (a2) of _~譲N, especially good base oil (4) and/or 700~1〇〇基N base oil (a2). It is possible to contain the above-mentioned eight specific aromatic compounds (pAH) in a vacuum distillation column for obtaining a 500% aromatic-containing base oil. It is difficult to obtain two types of aromatic-containing base oils having a high flash point of two or more different viscosities at the same time. Therefore, it is preferable to use (10) to a base oil (10). And / or Π Π) base oil (a2) to obtain an aromatic-containing base oil. The method for producing an aromatic-containing base oil of the present embodiment may have after the second solvent-cutting step base Preparation step: using at least one selected from the group consisting of the second extract and the second raffinate to obtain an aromatic-containing base oil having a total aromatic content of 147202.doc • 31 - 201100483 % or more. In the case of using at least one selected from the second extract and the second raffinate, an aromatic-containing base oil having a total aromatic component of 3% by mass or more is obtained, and the second raffinate is subjected to dewaxing treatment. Purification treatment, and obtain a purified oil (de-oiled) having a pour point of 9 or less, an aniline point of 9 or more, a viscosity index of 9 G or more, and a flash point of 2 or more, thereby making it aromatic The base oil of the family. As the purification treatment, it is preferred to carry out de-leaking treatment and hydrogenation. Thereby, an aromatic-containing base oil having a total aromatic component of 3% by mass or more can be easily obtained. The purified oil obtained by carrying out the above purification treatment can be preferably used as a base material for a lubricating base oil rubber replacement oil or the like. When the purified oil of, for example, 2 Torr to 15 〇〇N is obtained from the second raffinate, if the second solvent extraction step is carried out using the vacuum distillation fraction corresponding to the viscosity as a raw material, 4 可获得 can be obtained. . . The dynamic viscosity is preferably more than mmVs, more preferably 25〇mm2/s or more, especially preferably 5〇〇〇mm2/s or less, particularly preferably 2〇〇〇mm2/s or less. Extracts. By the above steps, an aromatic-containing base oil (hereinafter referred to as "aromatic-containing base oil a") having a total aromatic component content of 30% by mass or more, and a total aromatic component of 30% by mass or more, and Or the aromatic-containing base oil (hereinafter referred to as "aromatic-containing base oil b") having a total aromatic content of 30% by mass or more is obtained from the second extract. In the base oil preparation step, after extracting an appropriate fraction from the second raffinate and the second extract by appropriate distillation, one of the second raffinate and one of the second extract may be separately made into a base oil ( a), base oil (bp, or not 147202.doc -32- 201100483

Ο It is preferred to obtain a base oil (4) having a desired property and a base oil (b) by appropriately selecting a vacuum distillation amount as a raw material according to the base oil (4) and the base oil (b) required. i product (10) nt, duet). For example, when a lubricating base oil of 300 N or more and less than 600 N as the base oil (a) is obtained, a vacuum distillation fraction corresponding to the fraction may be used as a raw material, and the above-described third and second solvent extraction steps 'and If necessary, a purification step is carried out to obtain a lubricating base oil of 300 N or more and less than 600 N as the base oil (a): and 4 as a base oil (b) is obtained (the dynamic viscosity of the TC is 200 mm 2 /s or more). And less than 5 〇〇 mm 2 / s, preferably 250 to 350 mm Vs, more preferably 25 〇 ~ 3 〇〇 mm 2 / s. Also 'for example, as a base oil (4) 600 ~ 1200 N; In the case of the intermediate oil base oil, the vacuum distillation fraction corresponding to the fraction may be used as a raw material, and after the first and second solvent extraction steps and, as the case may be, the purification treatment, 600 as the base oil (a) may be obtained. ~1200 N lubricating base oil; and as a base oil (b) 40 ° C dynamic viscosity of 5 〇〇 ~ 5 〇〇〇 mm 2 / s, preferably 800 ~ 2000 mm2 / s, more Preferably, it is 900 to 1500 mm 2 /s. The base oil (a) of the present embodiment can be subjected to dewaxing or hydrogen by performing the second raffinate as described above. The base oil (a) (lubricating base oil) has a total aromatic content of 30 mass% or more, preferably 30 to 60 mass%, based on the purification treatment such as finishing. (a), preferably 200 to 1500 N, more preferably 250 N or more and less than 600 N or 600 to 1200 N ' Especially good is 300 to 450 N or 700 to 1000 N of lubricating base The oil is obtained in the form of 147202.doc -33- 201100483. The above-mentioned 8 kinds of specific aromatic compounds (sub) are reduced in the amount of the base oil (4) and the base oil (the high flash point of the f-viscosity are different from each other) b) The view is particularly good for the base oil (4) is ~450 N or 700~1000 N〇 base oil (4) is 600~ι2〇〇N, preferably it is ~(10)(4), in addition to the above specific traits, It is good to have the following traits. • 4 0 C dynamic adhesion Tang · 〗 2 and .120~250 mm / s, preferably 15 〇 ~ 2 〇〇 mm2 / s ° • 10 by GC steaming museum % points: 45 〇 ~ 52 〇χ:, better is ~ ~ times. c. • 90% points by GC steaming hall: 54 〇 ~ 6 〇 (rc, better is winning boots. • Total aroma Family composition (ASTM D 2549): 3 enamel % or more, preferably 疋 35 to 60% by mass, and more preferably 4 〇 to 5 〇 by mass. According to the present embodiment, a specific aromatic compound (a base oil (4) having a pA 特定 content of a specific amount or less and The base oil (8). In the present specification, the "specific aromatic compound (PAH)" means the following eight specific aromatic compounds (PAH). In the base oil (4) and the base oil (8) of the present embodiment, the content of (1) barium (BaP) is 1 mass ppm or less, and the following specific aromatic compounds (1) to 8) can be used ( The total content of PAH) is 1 〇 mass ppm or less. 1) Benzo(a)pyrene(BaP) 2) Stupid (e)芘(BeP) 3) Stupid (a)蒽(B a A) 4)Chopsticks (CHR) 5)Benzene (b)C2 Ethylene (BbFA) 147202.doc -34- 201100483 6) Benzo(1)propadienyl (BjFA) 7) Benzo(k)propadienyl (BkFA) 8) Dibenzo (a, h)蒽(DBAhA) These specific aromatic compounds (PAH) are usually prepared by separating and concentrating the target components, preparing a sample to which an internal standard substance is added, and performing quantitative analysis by analysis.

The base oil (a) and the base oil (b) are suitable as a base material for a lubricating base oil, a rubber blending oil or the like. The base oil (a) is a sufficiently reduced content of the specific aromatic compound (pah), and the flash point is 25 (rc or more, and the pour point is _5t: or less, and thus is also suitable as a lubricating base oil. The aromatic component is 30% by mass or more, and the glass transition point is -2 or less. Therefore, it can be used as a petroleum-based processing oil or a diluent oil or a base material thereof. The base oil (b) is a specific aromatic compound (pAH). Reduced, the sub-flash point is 25 〇t or more, the total aromatic component is 3% by mass or more, and the glass transition point is -3 (TC or less, @ can be used as petroleum processing oil or diluent oil or its base. Using a base oil (a), a base oil (8) or a mixture of the above, for example, a glass transition point of -55 to _3 〇t, a dynamic viscosity (10), and a enthalpy of 2 〇 to 5 〇 _% can be used. It is particularly suitable for blending petroleum-based processing oils or dilute oils with diene rubber. The rounds produced by blending such petroleum-based processing oils or diluent oils into two-diverse rubber meet low fuel consumption and (4) Sex, and can improve heat aging resistance or wear resistance. According to the production method of the present embodiment, an aromatic-containing base oil having a high transfer point and having a high total aromatic component and having a sufficiently reduced content of a cancerous substance of 147202.doc -35-201100483 can be broken at a high yield. It is particularly useful in the industry because it has a property suitable for a lubricating base oil, a petroleum-based processing oil or a diluent oil or a substrate thereof, and can simultaneously produce a plurality of aromatic-containing base oils having different viscosities. a) It is better to have the following traits: • Flow point: It is preferably _5t or less, and it is better that the following is especially good _20. (: Above. • Glass transfer point: better _ 3 (rc below, better is less severe, especially good is -50 〇 C or less; preferably -6 (TC or more, more preferably 100 C or more, especially good _8 〇〇 c or more) Particularly good is n or more. • Aniline point: preferably 70 ° C or more, more preferably 90. (: Above, especially good is 105 ° C or more; better! 12 (rc or less. Viscosity index: preferably 90 or more, more preferably % or more; preferably 120 or less, more preferably ι〇5 or less The flash point is preferably 2 5 0 C or more, preferably 3 1 〇 ° c or less. • Base oil composition according to ASTM D 3238: %Cp is preferably 6〇~7〇, °/〇 The amount of CN is preferably from 20 to 30, and the %CA is preferably from 5 to 1%. • The content of benzo(a)pyrene: preferably less than or equal to ppm by mass. • Total content of specific aromatic compounds (PAH): It is preferably 10 ppm by mass or less. As the base oil (al), 300 N or more and less than 6 N, preferably 3 0 4 5 N N, an aromatic base oil, in addition to the above properties It is preferred to have the following properties. 147202.doc -36- 201100483 • Dynamic viscosity at 40 °C · preferably 60~120 mm2/s, more preferably 65~90〇11112/8, especially good 70~8〇1111112/8 . • 10% by GC distillation, preferably 400 to 460 ° C, more preferably 430 to 450 ° C ° • 90% by GC distillation: preferably 500 to 540 ° C The better is 510~530〇C. • Total aromatic component (ASTM D 2549): preferably 30% by mass or more, more preferably 30 to 50% by mass. /〇.

Further, the value of the GC distillation in the present specification is a value measured in accordance with ASTM D 2887. The aromatic-containing base oil of 600 to 1200 N, preferably 700 to 1,000 N, of the base oil (a2) preferably has the following properties in addition to the above properties. • Dynamic viscosity at 40 ° C: preferably 120 to 250 mm 2 / s, more preferably 1 50 to 200 mm 2 / s. • 10% point by GC distillation: preferably 450 to 520 ° C, more preferably 460 to 500 ° C. • 90% by GC distillation: preferably 540 to 600 ° C, more preferably 560 to 590 ° C. • Total aromatic component (ASTM D 2549): preferably 30% by mass or more, more preferably 35 to 60% by mass, particularly preferably 40 to 50% by mass. As the base oil (b), an aromatic-containing base oil as the second extract or its purified oil obtained by carrying out the above-described first and second solvent extraction steps can be used. Further, the base oil (b) may be a mixture of two or more kinds of the second extract obtained in the above manner or a purified oil thereof. 147202.doc -37- 201100483 Base oil (b) is preferably a dynamic viscosity of 40 ° C above 200 mm 2 / s and less than 500 mm 2 / s, the glass transfer point is _6 〇 ~ _ 4 〇. (: base oil (bl) and / or 40 ° C dynamic viscosity of 500 mm 2 / s, glass transfer point of _50 ~ _3 〇 ° c base oil (b2). As base oil (b 1)' In addition to the above traits, it is preferred to have the following properties: • 40 C dynamic viscosity: preferably 2 〇〇 mm 2 / s or more and less than 500 mm 2 / s, more preferably 400 mm 2 / s or less, especially Good is below 350 mm2/s. Particularly good is below 300 mm2/s. • Glass transfer point: preferably _6〇~-40. 〇, more preferably -55~-48. 匚. Flow point: preferably 0 to 30 ° C, more preferably 1 5 ° C or more, especially preferably 20 ° C or more. • Difference between the flow point and the glass transfer point (flow point - glass transfer point) Preferably, it is 60C or more, more preferably 65 ° C or more, particularly preferably 701: or more; preferably 100. (: The following, more preferably 80 ° C or less.) • Total aromatic component: 50% by mass or more, preferably 6% by mass or more, more preferably 70% by mass or more, particularly preferably 8% by mass or more; more preferably 90% by mass or less. As a base oil (b2) ), in addition to the above traits, It is good to have the following traits: • 40 C dynamic viscosity: preferably 5 〇〇 mm's or more, more preferably 800 mm / s or more 'especially better than 1 〇〇〇 mm's; better is 5 Below 000 mm / s, more preferably below 2 〇〇〇 mm 2 / s, especially preferably below 1 500 mm 2 / s. 147202.doc -38- 201100483 • Glass transfer point: better nc, better It is _45~- hunger. • Total aromatic content: 50 mass; f% iγ, better 7 〇 mass: W% is better quality. Λ below. 8Gft% or more; 15GGN In the case of the aromatic-containing base oil, the base oil (8) can be simultaneously obtained by using the pressure of the decompression base corresponding to the deuterium.

The dynamic viscosity is preferably 2/s or more, more preferably 25 feet/above, and it is better to measure below 2, and more preferably below 2 mm/s. i soil "·, (4) and base oil (8) can be divided by the steaming. At this time, the viscosity of the scallops as a raw material is not particularly limited. However, it is preferred to obtain the desired base oil (4) and the desired base oil (8) in the form of a joint product. Therefore, it is preferred to select a reduced steam (four) score which is consistent with the properties of the base oil (4) and the base oil (8). And the same - reduced pressure steam _ is divided into starting materials. For example, when a base oil containing 25 〇 N or more and less than _ N as a base oil (al) is obtained, a vacuum distillation fraction corresponding to the fraction is used. Further, it is preferred that the aromatic-containing base oil of 250 N or more and less than 6〇〇N as the base oil (al) is obtained by the above-described second and second solvent extraction steps, and is obtained as a base oil. The dynamic viscosity of 4 〇t of (bl) is 2 〇〇mm / s or more and less than 500 mm 2 / s, preferably 25 〇 to 35 〇 mm 2 / s, particularly preferably 250 〜 3 〇〇 mm 2 / s extract (containing aromatic base oil). Further, for example, when a lubricating base oil of 600 to 1200 N as the base oil (a2) is obtained, a vacuum distillation fraction corresponding to the fraction is used. And better than 147202.doc -39- 201100483, with the above mentioned! And the second solvent extraction step, to obtain the oil-containing base oil of _~1200 N of the oil U2) and obtain the dynamic viscosity of the base oil (10) as ·5 〇〇〇%, good car : _~2_匪%, especially preferably _~丨5〇〇_2/s extract (: aromatic base oil). In this method, in order to obtain the desired base oil (4) and base oil (b), it is preferred to carry out batch treatment. In the blending step, the base oil (4) and the base oil (b) obtained in the above manner were subjected to a specific ratio to prepare a rubber blended oil. For example, the base oil (b) is blended at a ratio of not more than 95% by mass based on the total amount of the rubber blending oil (the ratio of the base oil (a) is not included and the ratio is 5% by mass or more. A rubber blending oil of the base oil (a) and the base oil (b). Further, the rubber blending oil may be separately prepared from the base oil without performing the above blending step. However, an appropriate dynamic viscosity is obtained. The viewpoint of the rubber blending oil of 10~70 mm2/s, preferably 15~5〇mm2/s, more preferably 20~32 mm2/s), and obtaining the flow point and glass transfer The difference of the points is 5 (the rubber blending oil of TC or more), based on the rubber blending oil as a whole, the blending ratio of the base oil (a) is preferably 〇 〇 5 〇 mass %, more Preferably, it is 20 to 40% by mass. Further, from the same viewpoint, the blending ratio of the base oil (b) is preferably from 9 to 50% by mass, more preferably from 80 to 60% by mass. The difference between the obtained pour point and the glass transition point is 5 〇. (: Above, and the glass transition point is -50 C or less, the base oil (a) is preferably contained. Oil (a2) 'Base oil (b) Since the difference between the flow point and the glass transition point is, for example, particularly large at 60 C or more, it is preferred to contain the base oil (b 1). Further, 147202.doc -40- 201100483 Increasing the yield of the rubber blending oil having the above-mentioned appropriate dynamic viscosity, the base oil (b) preferably contains the base oil (bl) and the base oil (b2). From this point of view, the base oil (a) or base The ratio of the oil (a2), the base oil (bl), and the base oil (b2) is preferably 10 to 40% by mass, 5 to 35 mass%, and 85 to 25% by mass, more preferably. It is 20 to 30% by mass, 20 to 30% by mass, and 6 to 4% by mass. Further, the rubber blending oil of the present embodiment may be blended with the base oil as long as the effect of the present invention is not impaired. The substrate of the present invention is not limited to the above embodiments. The present invention is not limited to the above embodiments. However, the present invention is not limited to the following examples. (Example 1) The atmospheric pressure steam (four) slag of crude oil is placed using a conventional vacuum distillation (four). The oil is subjected to vacuum distillation, and the fuel equivalent fraction, the 15 〇N equivalent fraction of the ruthenium fraction, the 350 N equivalent score, and the __ 当 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分 分The 35 〇N equivalent fraction is treated. Specifically, the first solvent extraction step is carried out: a 35 〇N equivalent fraction is introduced into the second extraction column 30 having a bottom temperature lower than the temperature of the column top to make a polar solvent (furfural) Contacting with a 350 N equivalent fraction. By the second solvent extraction step, the 350 N equivalent fraction is taken as a mixture of the first raffinate and the polar solvent obtained from the top portion of the third crucible extraction column. And a mixture of the third extract and the polar solvent obtained from the bottom portion. Then, the polar solvent is recovered by the unillustrated fraction, and the remainder and the first extract are obtained from the above mixture. Then, a second solvent extraction step is carried out: the first raffinate is introduced into the second extraction column 40 having a bottom temperature lower than the temperature at the top of the column, and is brought into contact with a polar solvent (furfural). By the second solvent extraction step, the first raffinate is fractionated as a mixture of the second raffinate and the polar solvent obtained from the top portion, and the second extract and the polar solvent obtained from the bottom portion. a mixture. Then, the polar solvent is recovered by a fractionation column (not shown) to obtain a second extract and a second raffinate from the above mixture. The total aromatic content of the second raffinate measured in accordance with ASTM D 2549 is 30% by mass or more. Further, the density of the second extract at 15 ° C is 0.94 g/cm 3 or more, and the total aromatic component measured in accordance with ASTM D 2549 is 30% by mass or more. The production conditions and yields of the first solvent extraction step and the second solvent extraction step are shown in Table 1. [Table 1] Manufacturing step 1st solvent extraction step 2nd solvent extraction step Raw material vacuum distillation fraction (350 N) Left side first residue polar solvent furfural furfural solvent ratio 1.3 2.0 Tower top temperature °C 90 116 bottom temperature °C 60 85 Residue 1st raffinate 2nd raffinate yield (relative to raw material)% by volume 74 80 PAH8 total content mass ppm <10 <10 extract 1st extract 2nd extract yield (relative to the raw material) Volume % 26 20 PAH 8 kinds of total content mass ppm > 10 < 10 Yield of the useful component % by volume - 74 The above second residue was subjected to MEK (methyl ethy丨ketone, methyl ethyl ketone) The wax and the hydrogenation finishing treatment are purified so that the flow point 147202.doc •42-201100483 is -10 ° C or lower, and the aromatic-containing base oil (lubricating base oil) having a total aromatic content of 30% by mass or more is obtained. ). This was used as a base oil (A1). Further, the second extract was used as a base oil (B1) or (B3) component. The properties of the base oil (A1), the base oil (B1) and the base oil (B3) are shown in Table 2. Further, the second extract was not subjected to purification treatment. [Table 2]

Base oil (Al) base oil (Bl) base oil (B3) density (15 ° C) g / cm3 0.8827 0.9539 0.9578 flash point (COC) °c 272 263 258 dynamic viscosity (40 ° C) mm2 / s 74.34 236.8 274.8 Dynamic viscosity (l〇〇°C) mm2/s 9.227 14.81 14.81 Viscosity index 99 37 11 Aniline point °c 107 61.7 59 Nitrogen component mass% 0.004 0.040 0.040 Composition (ASTM D 3238) %CP 67.6 56.6 54.4 %CN 26.9 19.6 19.7 %Ca 5.6 23.8 25.9 Composition (ASTM D 2140) %CA - 22.9 24.2 Composition (ASTM D 2549) Saturated component mass % 65.5 15.4 15.4 Total aromatic component mass % 33.9 82.3 82.3 Benzo(a)pyrene mass ppm <1 <1 <1 PAH8 total content mass ppm <10 <10 <10 GC distillation 10% point °C 444 - - 90% point °C 518 - - Flow point °C -12.5 25 25 Glass transfer point °C (Imagine: <-60) -53.9 -52.4 Flow point - glass transition point °C (Imagine: > 47.5) 78.9 - Total content of benzo(a)pyrene and 8 specific aromatic compounds (PAH) The measurement was carried out in the manner described below. First, 1 g of each aromatic-containing base oil was dissolved in hexane by a 50 ml flask to prepare a 2% by mass sample solution. The sample solution was loaded on a 5 mass% aqueous silicone gel, and after washing with hexane, the target component was eluted with a 1% by volume acetone/hexane solution. After the eluate was concentrated, a sample to which an internal standard substance was added was prepared and identified and quantified by a usual gas 147202.doc -43 - 201100483 phase chromatography mass spectrometer (GC-MS). (Example 2) An atmospheric distillation residue of crude oil was subjected to vacuum distillation using a usual vacuum distillation apparatus to fractionate a fuel equivalent fraction, a fraction below 150 N equivalent fraction, a 350 N equivalent fraction, and a 900 N equivalent fraction. The same as in the first embodiment except that the 900 N equivalent fraction was introduced into the first extraction column 30 instead of the 3 50 N equivalent fraction, and the production conditions of the first and second solvent extraction steps were changed as shown in Table 3. In this manner, the first and second raffinates, and the first and second extracts are produced. Further, the manufacturing is carried out plural times under the same conditions to obtain a plurality of manufactured articles. The production conditions and yields of the first solvent extraction step and the second solvent extraction step are shown in Table 3. The second aromatic component in Example 2 was also 30% by mass or more based on the total aromatic component measured in accordance with ASTM D 2549. Further, the density of the second extract at 15 ° C is 0.94 g/cm 3 or more, and the total aromatic component measured according to ASTM D 2549 is 30% by mass or more. [Table 3] Manufacturing step 1st solvent extraction step 2nd solvent extraction step Raw material vacuum distillation fraction (900 N) Left side first residue polar solvent furfural furfural solvent ratio 1.2 2.1 Tower top temperature V 90 121 Tower bottom temperature V 60 90 raffinate 1st raffinate 2nd raffinate yield (relative to raw material) vol% 75 75 PAH 8 total content mass ppm <10 <10 extract 1st extract 2nd extract yield (relative In the raw material) Volume % 25 25 PAH 8 kinds of total content mass ppm > 10 < 10 Yield of the useful component % by volume - 75 147202.doc -44· 201100483 For the two kinds of second raffinate which are different in the manufacturing lot, Purification treatment by MEK dewaxing and hydrogenation finishing treatment to obtain a flow point of -10 ° C or lower to obtain two aromatic-containing base oils (lubricating base oils) having a total aromatic component content of 30% by mass or more. This was used as a base oil (A2) and a base oil (A3). Further, the second extract obtained in the second solvent extraction step is used as a base oil (B2) together with the second raffinate for producing the base oil (A2). Further, the second extract obtained in the second solvent extraction step is used as a base oil (B4) together with the second raffinate for producing the base oil (A3). The properties of the base oil (A2), the base oil (A3), the base oil (B2) and the base oil (B4) are shown in Table 4. [Table 4] Base oil (A2) Base oil (A3) Base oil (B2) Base oil (B4) Density (15 ° C) g/cm3 0.893 0.8936 0.9768 0.9774 Flash point (COC) V 282 298 296 280 Dynamic viscosity (40°C) mm2/s 164 170.7 1090 1185 Dynamic viscosity (l〇〇°C) mm2/s 15.48 15.76 33.77 34.09 Viscosity index 95 94 23 14 Aniline point °c 112.4 112 59.7 60 Nitrogen component mass% 0.007 0.009 0.080 0.090 Composition (ASTMD 3238) %CP 68.1 68.0 57.5 57.5 %CN 24.9 25.0 9.7 9.7 %Ca 7.0 7.0 32.8 32.8 Composition (ASTM D 2140) %CA - - 29.5 29.5 Composition (ASTM D 2549) Saturated component mass % 55.9 55.9 9.0 9.0 Total Aromatic component mass% 43.3 43.3 86.9 86.9 Benzo(a)pyrene mass ppm <1 <1 <1 <1 PAH8 total content mass ppm <10 <10 <10 <10 <10 GC Distillation 10 %°°C 481 481 - - 90%°°C 573 573 - - Flow point °C -15 -12.5 17.5 20 Glass transfer point °C -63 -63 -41.9 -42.7 Flow point - glass transfer point °C 48 - 59.4 - According to Table 1 and Table 3, in Examples 1 and 2, there is a second extraction for rubber blending 147202.doc -45- 201100483 oil or its substrate The total yield of the second extract and the second extract is based on the raw material oil of the second extraction tower, and is 74 to 75 vol% (the yield of the useful component) is so accurate that it can be produced in a high yield for use as a rubber blend. Lubricating base oil (including aromatic base oil) of oil or its substrate. The base oils (A1), (B3) and (B4) of Examples 1 and 2 are both total aromatic components and 'A2), (A3), (Bl), (B2) according to Tables 2 and 4. , for 30 quality 1% or more and smell, k army μ up. Guang,,| One person points are 250 C or more. That is, in the present embodiment, a plurality of aromatic-containing base oils having excellent properties and different viscosities can be produced by using a plurality of vacuum distillation fractions having different viscosities. Further, in the base oils (A1), (A2), (A3), (Bl), (B2), (B3) and (B4), carcinogenic benzo(a)pyrene or 8 specific aromatic compounds ( The total content of pAH) is sufficiently reduced. Further, the difference between the flow point of the base oil (B 1) and the base oil (B2) and the glass transition point is 50 ° C or more, and in particular, the difference between the base oil (B1) is above and below the specificity. That is, it is confirmed that although the flow point of any of the base oil (B1) and the base oil (B2) is high, the glass transition point is low. Further, in the base oil (B1), the base oil (B2), the base oil (B3) and the base oil (B4) of Examples 1 and 2, the aromatic hydrocarbon content was high in mass%, and had a moderate glass transition point. Tg, therefore, if blended in a rubber composition, tensile strength or abrasion resistance can be improved. (Example 3) The above base oils (Α1), (Α2), (βΐ) and (B2) were blended according to the ratio of #5, and the rubber of Example 3-:^3-4 was prepared. Oil. The properties of each rubber blended oil are shown in Table 5. 147202.doc -46- 201100483 [Table 5] Example 3-1 Example 3-2 Example 3-3 Example 3-4 Base oil (A1) - - 20 - Base oil (A2) 25 10 - 33 base Oil (B1) 25 40 - - Base oil (B2) 50 50 80 67 Density (15 ° C) g / cm J 0.9501 0.9596 0.9585 0.95 Flash point (COC) °C 272 276 276 294 Dynamic viscosity (40 ° C) mm2 /s 415.8 468.0 544.1 501.0 Dynamic viscosity (l〇〇°C) mm2/s 21.89 22.27 24.97 24.83 Aniline point °C 75.8 66.1 71.2 78.7 Nitrogen component mass% 0.05 0.05 0.06 0.06 Composition (ASTM D 3238) %CP 60.3 59.1 60.1 61.2 %CN 16.5 14.4 14.1 15.8 %CA 23.2 26.6 25.8 23.0 Composition (ASTM D 2549) Saturated component mass % 22.3 16.2 22.1 23.1 Total aromatic component mass % 74.9 80.7 73.5 73.9 Composition (ASTM D 2007) Saturated component mass % 25.3 - - - Total aromatic component mass % 68.9 - - - Polar compound mass % 5.8 - - - Benzo(a)pyrene mass ppm <1 <1 <1 <1 PAH8 total content mass ppm <10 <10 <10 <10 Flow point °C 15.0 20.0 -5.0 -2.5 Glass transfer point °c -51.0 -49.3 -50.5 -51.5 Flow point - glass Move Point ° C 66.0 69.3 45.5 49.0

As shown in Table 5, the rubber blending oils of Examples 3-1, 3-2, 3-3 and 3-4 are all harmful substances which have a high total aromatic component and a flash point and are carcinogenic. Both are fully reduced. Further, the difference between the flow point and the glass transition point is 45 ° C or more. In particular, the rubber blending oils of Examples 3-1 and 3-2 have the following specific shapes: the difference between the pour point and the glass transition point is 60 ° C or more, although the total aromaticity according to ASTM D 2549 or ASTM D 2007 The composition is 50% by mass or more, and the pour point is 15 ° C or higher, but the glass transition point is -45 ° C or lower. It is also clear that the rubber blending oils of Examples 3-1 to 3-4 are all in accordance with ASTM D 3238 (eight: 20 to 35, glass transfer point Tg is -55 to -30 ° C, 147202). .doc -47- 201100483 A petroleum-based processing oil having a dynamic viscosity (10 °C) of 20 to 50 mm2/s and substantially no specific aromatic compound (PAH), so as a manufacturing step in a diene rubber When the diluent oil used in the process or the processing oil used in the processing of the diene rubber is blended, the following excellent effects are also produced: the fuel consumption and the slip resistance can be simultaneously satisfied, and the heat aging resistance or the abrasion resistance can be improved. (Reference Example 1) The atmospheric distillation residue oil of crude oil is subjected to vacuum distillation using a usual vacuum distillation apparatus, and a fuel equivalent fraction, a fraction below 150 N equivalent fraction, a 25 0 N equivalent fraction, and The above fraction (500 N equivalent fraction). The solvent extraction step is carried out: the 500 N equivalent fraction is introduced into the extraction column whose bottom temperature is lower than the temperature of the column top, in order to increase the yield of the raffinate, The aromatic component of the obtained lubricating base oil is 30% by mass/◦ And the specific aromatic compound (PAH) is contacted with a polar solvent (furfural) under the condition that the content of the specific aromatic compound (PAH) is less than 10 mass ppm. By the solvent extraction step, the 500 N equivalent fraction is taken as the first extraction. The residue and the first extract are shown in Table 6. The production conditions and the yield of the solvent extraction step are shown in Table 6. [Table 6] Manufacturing Step Solvent Extraction Step Raw Material Vacuum Distillation Fraction (500 N) Polar Solvent Furfural Solvent Ratio 2 Tower Top Temperature °C 120 bottom temperature °C 72 raffinate first raffinate yield (relative to raw material) vol%% 60 PAH8 total content mass ppm <10 extract first extract yield (relative to raw material) vol%% 40 PAH8 total content mass ppm >18 useful component yield volume% 60 147202.doc -48- 201100483 The first raffinate thus obtained is subjected to purification treatment using MEK dewaxing and hydrogenation finishing treatment so that The flow point is -10 ° C or lower, thereby obtaining two kinds of aromatic-containing base oils (lubricating base oils) having different manufacturing batches and having a total aromatic content of 30% by mass or more, which is used as a base oil (E1). , base oil (E2). Again, The extract was used as the base oil (F). The properties of the base oil (E1), the base oil (E2) and the base oil (F) are shown in Table 7. [Table 7] Aromatic base oil-based oil (El) group Oil ¢ 2) Base oil (F) Density (15 ° C) Λ g / cm 0.8867 0.8867 1.01 Flash point (COC) °c 270 270 - Dynamic viscosity (40 ° C) mm2 / s 100.4 100.4 - Dynamic viscosity (l 〇〇°C) mm2/s 11.18 11.18 30.7 Viscosity index 96 96 - aniline point °c 109 109 39 Nitrogen component mass% 0.004 0.004 - Composition (ASTM D 3238) %CP 66.1 66.1 - %CN 27.1 27.1 - %CA 6.8 6.8 - Composition (ASTM D 2140) %CA - - - Composition (ASTM D 2549) Saturated component mass % 62.2 62.2 - Total aromatic component mass % 37.3 37.3 - Benzoquinone (a) Beneficial mass ppm <1 <1 < 2 PAH8 total content mass ppm <10 <10 >18 GC distillation 10% point °C 458 458 - 90% point °C 537 538 - Flow point °C -12.5 -12.5 As shown in Table 6, In the present reference example, the yield of the first raffinate based on the raw material introduced into the extraction column was 60% by volume, and the yield of the first extract was 40% by volume. Further, as shown in Table 7, the total content of the aromatic-containing base oil (F) as a carcinogenic specific aromatic compound (PAH) exceeds 10 mass 147202.doc -49 - 201100483 PPm. The aromatic-containing base oil (F) is not suitable for use as a rubber blending oil directly, and even when blended with other lubricating base oils, it is usually not possible to blend the blending ratio by 50% by mass or more. . (Reference Example 2) The deasphalted oil of the vacuum-saturated residue oil of the crude oil was distilled as the raffinate and the extract by the same solvent extraction step as in Reference Example 1. The extract had a dynamic viscosity of 95 at 100 ° C, a total aromatic content of 69% by mass according to ASTM D 2549, a pour point of 12.5 ° C, and a glass transition point of _29.7. (:, the difference between the flow point and the glass transfer point (flow point-glass transition point) is 42.2 ° C. The extract is blended with the base oil of the above reference example i (£1) in a mass ratio of 8 〇: 2 〇 The rubber blending oil was prepared in combination. The rubber blending oil had a flow point of 〇 ° C, a glass transition point of _44.5 r, and a difference between the flow point and the glass transition point of 44.5 〇 C. (Reference Example 3) The N equivalent fraction was introduced into the extraction column instead of the 500 1^ equivalent fraction, and a solvent extraction step was carried out in the same manner as in Reference Example i to obtain a raffinate and an extract. Then, the raffinate was dewaxed by using mek. And the purification treatment of the hydrogenation finishing treatment to make the pour point below the child, and obtain the aromatic-containing base oil as the base oil (9). The flash point of the base oil (8) is less than 25 rc. In this reference example, It is not possible to obtain only one aromatic-containing base oil (500 N base oil) with a flash point of 25 generations or more from the total amount of steamed cranes (250 N equivalent fraction). Industrial availability 147202.doc -50- 201100483 According to the present invention, it is possible to provide a high total aromatic content and a high flash a rubber blending oil having a point and a low-surface transfer point, and a specific polycyclic grouping t content is sufficiently reduced, and a method for preparing the rubber blending oil. Further, according to the present invention, steaming can be carried out under reduced pressure. Divided into raw materials: a stroke method and (4) extract residue and extract, providing high =, low glass transition point 'has a higher total material group m to reduce the amount of carcinogenic substances fully reduced aromatic base oil. Can provide high

, ... A method for producing an aromatic-containing base oil containing such an aromatic base oil. BRIEF DESCRIPTION OF THE DRAWINGS 糸 shows the step of the rubber form of the present invention. [Description of main components] 16 ' 34 . 36 38'44, 46 48 Preferred implementation of the method 30 30 50 60

First extraction tower Second extraction tower Dewaxing unit Hydrogen finishing unit. 147202.doc •51-

Claims (1)

201100483 VII. Patent application scope: 1. A rubber blending oil with a total aromatic content of 5% by mass or more according to ASTM D 2007 or ASTM D 2549, and a flash point of 25 (TC or more, flow point and glass transfer) The difference between the points is 45. (: Above; the content of benzo(a)pyrene is i mass ppm or less, and the total content of the specific aromatic compound of the following 1) to 8) is 1 〇 mass ppm or less: 1) Benzo(a)pyrene (BaP) © 2) Benzo(e)pyrene (BeP) 3) Benzo(4)pyrene (BaA) 4) Chopsticks (CHR) 5) Benzo(b)propadiene (BbFA) 6) Benzo(j)propadienyl ruthenium (BjFA) 7) Benzo(k)propadienyl ruthenium (BkFA) 8) Benzene (a, h) oxime (DBAhA). q. The rubber blending oil of claim 1, wherein the aromatic-containing base oil (a) and the aromatic-containing base oil (b) contain at least the aromatic-containing base oil (b) The aromatic-containing base oil (a) contains a raffinate or a purified oil obtained by separating a vacuum distillation fraction of the original atmospheric oil distillation residue oil by a solvent extraction step, and 4 (the dynamic viscosity of the TC is 60~6〇〇mm2/s, aniline point is 7〇°C or more, and 1〇% point by GC distillation is 4〇〇~5〇〇. (:, 90% point is 500~6〇〇. : according to ASTM D 3238i%CA 3~20, glass transition point is -30. (: The following; the aromatic-containing base oil (b) contains the above-mentioned 147202.doc 201100483 atmospheric distillation residue by solvent extraction step The extract obtained by separating the oil under vacuum distillation fraction or its purified oil, and 4 〇. (: The dynamic viscosity is 200 mm 2 /s or more, the aniline point is 90 ° C or less, 15. (The density is 0.94 g /cm3 or more, the total aromatic component according to ASTM D 2549 is 3% by mass or more, and the content of the aromatic-containing base oil (a) is 95% by mass or less, and the above-mentioned content The base oil of the fragrant base (b) is 5 mass% or more. 3. The rubber blending oil of claim 2, wherein the solvent extraction step has: a first solvent extraction step, wherein the temperature at the bottom of the column is 3〇~9〇t:, the temperature of the top of the tower is returned to the first extraction tower of the bottom temperature, and the decompressed steam strip is contacted with the polar solvent to obtain the first raffinate and the third extract; In the second solvent extraction step, in the second extraction column in which the column bottom temperature and the column top temperature are higher than the first extraction column by 10° CU, the first raffinate is brought into contact with the polar solvent to obtain the second a raffinate and a second extract; the aromatic-containing base oil (b) is the second extract or a purified oil thereof. 4. A method for producing a rubber blended oil having a blend-containing aromatic group a blending step of the oil (a) and the aromatic-containing base oil (b); the aromatic-containing base oil (a) contains a vacuum distillation fraction of the crude oil atmospheric distillation residue by a solvent extraction step And the residue or its purified oil, and the dynamic viscosity of 40 C is 60~600 mm2/s, and the aniline point is 7 (T Above C, the 1% point by GC distillation is 4〇〇~50CTC, 90% is 500~600°C, according to ASTM D 3238% (^3~2〇, glass transition point is -30°) C hereinafter: 147202.doc 201100483 The base oil of the above-mentioned Fangxiang group (b) contains an extract obtained by separating the vacuum distillation fraction of the above-mentioned atmospheric distillation residue oil by a solvent extraction step, or a purified oil thereof, and 40° C has a dynamic viscosity of 200 mm 2 /s or more, a thief or less, a density of hunger of 94 g/cm 3 or more, and a total aromatic content of 30 mass % or more according to astm D 2549; the above rubber blended oil according to ASTM D 20〇7 or ASTM 〇2549 The total aromatic content is 50 mass. /〇 above, the flash point is 25〇.匸 or more, the difference between the flow point and the glass transition point is 451 or more, the content of benzo (a) is 1 ppm by mass or less, and the total content of the specific aromatic compound of the following 1) to 8) is 10 ppm by mass or less. 'And the content of the aromatic-containing base oil (a) exceeds 0 and 95 mass. /. The content of the following aromatic-containing base oil (b) is 5% by mass or more and less than 1% by mass: 1) benzo(a)pyrene (BaP) 2) benzo(e)pyrene (BeP) 3 Benzo(a)pyrene (BaA) 4) Chopsticks (CHR) 5) Benzo(b)propadienyl (BbFA) 6) Benzo(j)propadienyl (BjFA) 7) Benzo (k) Propadiene conjugate (BkFA) 8) Dibenzo(a,h) oxime (DBAhA). A method for producing an aromatic-containing base oil, which comprises a first solvent extraction step and a second solvent extraction step, and a first solvent extraction step at a bottom temperature of 30 to 90. (:, in the first extraction column where the temperature of the column top is higher than the temperature of the bottom of the column, the vacuum distillation fraction of the atmospheric distillation residue of the crude oil is contacted with the solvent of the polarity 147202.doc 201100483, and the first raffinate and the first 1st extract; a second solvent extraction step of contacting the first raffinate with a polar solvent in a second extraction column having a column bottom temperature and a column top temperature higher than 1 (rc or higher) of the first extraction column; And obtaining a first extract having a second raffinate and a density of 0.94 g/cm 3 or more and a total aromatic component of 3% by mass or more; and the aromatic-containing base oil contains the second extract; At least a part of the second raffinate or the purified oil thereof, the total aromatic component is 30% by mass or more. 6. The method for producing an aromatic-containing base oil according to claim 5, wherein the base oil preparation step is After the second solvent extraction step, the second raffinate is subjected to a purification treatment including a dewaxing treatment to obtain the purified oil, and the aromatic-containing base oil contains the purified oil, and the pour point is _5 < t The following, the stupid amine point is 9 ° ° C A method for producing an aromatic-containing base oil according to claim 5, wherein the aromatic-containing base oil contains the second extract, and the flash point is at least 〇. At least a part; and the dynamic viscosity of 40 C is 2〇〇mm2/s or more, the flash point is 25〇°c or more, and the flow point is 30. (: The following 'aniline point is 9 (TC below, glass transition point is - 30 C or less 'and the difference between the above-mentioned flow point and the above-mentioned glass transition point is 5 〇 ° C or higher. 8. The method for producing an aromatic-containing base oil according to claim 5, wherein the benzene containing the base oil of the fragrant aromatic group And (a) the content of cerium is 1 mass ppm or less, and the total content of the specific aromatic compound of the following 1) to 8) is 1 〇 mass pprn to 147202.doc -4- 201100483: 1) benzo (a) ) Ba (BaP) 2) Benzo(e)pyrene (BeP) 3) Benzo(a)pyrene (BaA) 4) Chopsticks (CHR) 5) Benzo(b)propadiene (BbFA) 6) Benzo(1)propadienyl ruthenium (BjFA) Ο 9. 10. 7) Benzo(k)propadienyl (BkFA) 8) — Ben (a, h) onion (DBAhA). An aromatic-containing base oil obtained by the method of the present invention, which is a base product of the present invention. A rubber blending oil comprising the aromatic oil of claim 9. ❹ 147202.doc -5-