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WO2015060399A1 - Composition de graisse - Google Patents

Composition de graisse Download PDF

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Publication number
WO2015060399A1
WO2015060399A1 PCT/JP2014/078250 JP2014078250W WO2015060399A1 WO 2015060399 A1 WO2015060399 A1 WO 2015060399A1 JP 2014078250 W JP2014078250 W JP 2014078250W WO 2015060399 A1 WO2015060399 A1 WO 2015060399A1
Authority
WO
WIPO (PCT)
Prior art keywords
base oil
mass
oil
grease composition
catalyst
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2014/078250
Other languages
English (en)
Japanese (ja)
Inventor
泰葉 徳毛
坂本　清美
黒澤　修
健太郎 山口
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eneos Corp
Original Assignee
JX Nippon Oil and Energy Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JX Nippon Oil and Energy Corp filed Critical JX Nippon Oil and Energy Corp
Priority to JP2015543913A priority Critical patent/JP6682270B2/ja
Publication of WO2015060399A1 publication Critical patent/WO2015060399A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/02—Mixtures of base-materials and thickeners
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions used as base material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • C10M2215/065—Phenyl-Naphthyl amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy

Definitions

  • the present invention relates to a grease composition.
  • Grease is a lubricant made by dispersing a solid lipophilic solid thickener in base oil to make it semi-solid. Therefore, it is possible to make the lubrication system simple, and it is mainly used for lubrication of machine elements such as rolling bearings, plain bearings, ball screws, linear motion guides, gears, etc. for industrial machinery and transportation machinery systems. Widely used.
  • Rolling bearings in particular, include ball bearings and roller bearings, and are widely used in machine tool spindles, railway vehicle vehicles, engine accessories such as automobile alternators, constant velocity joints, wheels, and the like.
  • Patent Document 1 In recent years, energy saving is required, and reduction of energy loss of various mechanical systems has become an urgent issue.
  • the problem to be solved by the present invention is to provide a grease composition that has a low bearing rotation resistance, in particular, can greatly reduce the torque during rotation of the bearing, and can satisfy an excellent bearing fatigue life. is there.
  • the inventor of the present invention uses a base oil having specific properties for grease, thereby significantly reducing the torque during rotation of the bearing while maintaining the bearing fatigue life. Found that you can.
  • the present inventor first paid attention to the oil film forming ability of the bearing and the viscosity change of the lubricating base oil accompanying the temperature change, and by forming a sufficient oil film between the bearing rolling element and the bearing ring, the direct contact between them.
  • the base oil has a specific property, in particular, contains a large amount of paraffin components (ndM ring analysis), which is a component having a high viscosity index. I found out.
  • the present inventor has found that the urea adduct value is effective as an index of the content of paraffin that causes a torque increase at the start of the bearing at a low temperature. Further, by using a lubricant base oil whose urea adduct value,% C P ,% C A and viscosity index satisfy specific conditions, the low torque of the bearing from the normal temperature to the high temperature range while suppressing a rapid increase in starting torque at low temperature. It was found that the torque loss of mechanical elements such as bearings can be reduced.
  • This invention is made
  • [4] Use of the grease composition according to any one of [1] to [3] for a machine element.
  • [5] Use for a machine element according to [5], wherein the machine element is a bearing.
  • [6] A method for reducing torque of a machine element, wherein the machine element is lubricated with the grease composition according to any one of [1] to [3].
  • the grease composition of the present invention exhibits a special effect that the torque required for rotation of the bearing can be reduced while maintaining the bearing fatigue life.
  • the urea adduct value of the lubricating base oil is 4% by mass or less, preferably 3.5% by mass or less from the viewpoint of suppressing an increase in viscosity at a low temperature range and suppressing an increase in torque at the start of the bearing at a low temperature. More preferably, it is 3 mass% or less, More preferably, it is 2.5 mass% or less.
  • the urea adduct value of the lubricant base oil may be 0% by mass, but a lubricant base oil having a higher viscosity index can be obtained while sufficiently suppressing an increase in torque at the start of the bearing at a low temperature. It is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and particularly preferably 0.8% by mass or more from the viewpoint of ease of dewaxing conditions and excellent economic efficiency.
  • the urea adduct value as used in the present invention is measured by the following method. 100 g of weighed sample oil (lubricating base oil) is placed in a round bottom flask, 200 g of urea, 360 ml of toluene and 40 ml of methanol are added and stirred at room temperature for 6 hours. As a result, white granular crystals are produced as urea adducts in the reaction solution. The reaction solution is filtered through a 1 micron filter to collect the produced white granular crystals, and the obtained crystals are washed 6 times with 50 ml of toluene.
  • the recovered white crystals are put in a flask, 300 ml of pure water and 300 ml of toluene are added, and the mixture is stirred at 80 ° C. for 1 hour.
  • the aqueous phase is separated and removed with a separatory funnel, and the toluene phase is washed three times with 300 ml of pure water.
  • a desiccant sodium sulfate
  • the ratio (mass percentage) of the urea adduct thus obtained to the sample oil is defined as the urea adduct value.
  • the normal paraffin in the case where the normal paraffin remains in the lubricating base oil, as well as the components that cause a torque increase at the start of the bearing at a low temperature among isoparaffins. Can be collected accurately and reliably, it is excellent as an index of the content ratio of normal paraffin and the specific isoparaffin.
  • the inventors of the present invention have analyzed by using GC and NMR that the main component of the urea adduct is a normal paraffin and an isoparaffin urea adduct having 6 or more carbon atoms from the end of the main chain to the branch position. Confirm that there is.
  • the% C p of the lubricating base oil is 70 or more, preferably 70 to 99, more preferably 72 to 97. If% Cp is less than 70, the viscosity index is low, and the torque reduction effect is insufficient. From the viewpoint of availability and cost,% C p is preferably 99 or less.
  • % C A of the lubricating base oil from the viewpoint of high viscosity index of, 2 or less, preferably 0.7 or less, more preferably 0.6 or less.
  • % C P and% C A are the percentages of the number of paraffin carbons to the total number of carbons determined by a method (ndM ring analysis) based on ASTM D 3238-85, respectively. It means the percentage of the total number of aromatic carbons. That is, the preferable ranges of% C P and% C A described above are based on values obtained by the above method.
  • the viscosity index of the lubricating base oil in the present embodiment is 105 or more, preferably 110 to 200, more preferably 120 to 180.
  • the viscosity index is less than 105, the effect of suppressing the decrease in viscosity due to heat generation is insufficient, and when it exceeds 200, the flow resistance increases due to the small decrease in viscosity at high temperature, and the torque cannot be reduced.
  • the kinematic viscosity at 100 ° C. of the lubricating base oil in the present embodiment is preferably 2.0 to 22 mm 2 / s, more preferably 2.2 to 20 mm 2 / s, and further preferably 2.4 to 15 mm 2. / S, particularly preferably 3.0 to 8.0 mm 2 / s.
  • the lubricating base oil may volatilize due to high-temperature heating during grease production.
  • it is intended to obtain a lubricating base oil having a kinematic viscosity at 100 ° C. exceeding 22.0 mm 2 / s the yield is lowered, and the decomposition rate is increased even when heavy wax is used as a raw material. Tend to be difficult.
  • the kinematic viscosity at 40 ° C. of the lubricating base oil in this embodiment is preferably 5.0 to 200 mm 2 / s, more preferably 8.0 to 150 mm 2 / s, and even more preferably 10 to 100 mm 2 / s. It is.
  • a raw material oil containing normal paraffin can be used.
  • the raw material oil may be either mineral oil or synthetic oil, or may be a mixture of two or more of these.
  • the content of normal paraffin in the raw material oil is preferably 50% by mass or more, more preferably 70% by mass or more, still more preferably 80% by mass or more, more preferably 90% by mass, based on the total amount of the raw material oil. Especially preferably, it is 95 mass% or more, Most preferably, it is 97 mass% or more.
  • the raw material oil used in the present invention is preferably a wax-containing raw material that boils in the lubricating oil range defined in ASTM D86 or ASTM D2887.
  • the wax content of the raw material oil is preferably 50% by mass or more and 100% by mass or less based on the total amount of the raw material oil.
  • the wax content of the raw material can be measured by an analytical technique such as nuclear magnetic resonance spectroscopy (ASTM D5292), correlated ring analysis (ndM) method (ASTM D3238), solvent method (ASTM D3235).
  • wax-containing raw material examples include oils derived from solvent refining methods such as raffinate, partially solvent dewaxed oil, dewaxed oil, distillate, reduced pressure gas oil, coker gas oil, slack wax, foots oil, and Fisher- Examples include Tropsch wax, and among these, slack wax and Fischer-Tropsch wax are preferable.
  • Slack wax is typically derived from hydrocarbon raw materials by solvent or propane dewaxing. Slack wax may contain residual oil, which can be removed by deoiling. Foots oil corresponds to deoiled slack wax.
  • Fischer-Tropsch wax is produced by a so-called Fischer-Tropsch synthesis method.
  • a commercial product may be used as a raw material oil containing normal paraffin.
  • specific examples include Paraflint 80 (hydrogenated Fischer-Tropsch wax) and shell MDS waxy raffinate (Shell MDS Waxy Raffinate) (hydrogenated and partially isomerized middle distillate synthetic waxy raffinate). It is done.
  • the raw material oil derived from solvent extraction is obtained by sending a high-boiling petroleum fraction from atmospheric distillation to a vacuum distillation apparatus and extracting the distillation fraction from this apparatus with solvent.
  • the residue from the vacuum distillation may be denitrified.
  • aromatic components are dissolved in the extraction phase while leaving more paraffinic components in the raffinate phase. Naphthene is partitioned into the extraction phase and the raffinate phase.
  • phenol, furfural, N-methylpyrrolidone and the like are preferably used as phenol, furfural, N-methylpyrrolidone and the like are preferably used.
  • a bottom fraction obtained from a fuel oil hydrocracking apparatus may be used as a raw material by using a fuel oil hydrocracking apparatus having higher hydrogenation resolution.
  • the raw material oil is subjected to a process of hydrocracking / hydroisomerization so that the urea adduct value of the material to be treated is 4% by mass or less and the viscosity index is 100 or more.
  • a lubricating base oil can be obtained.
  • the hydrocracking / hydroisomerization step is not particularly limited as long as the urea adduct value and the viscosity index of the obtained workpiece satisfy the above conditions.
  • the preferred hydrocracking / hydroisomerization step in the present invention is: A first step of hydrotreating a raw oil containing normal paraffin using a hydrotreating catalyst; A second step of hydrodewaxing the object to be treated obtained in the first step using a hydrodewaxing catalyst; The to-be-processed object obtained by a 2nd process is equipped with the 3rd process of hydrotreating using a hydrotreating catalyst.
  • a hydrotreating step is provided before the hydrodewaxing step for the purpose of desulfurization / denitrogenation for the prevention of poisoning of the hydrodewaxing catalyst.
  • a part of the normal paraffin in the feedstock for example, about 10% by weight, preferably 1 to 10% by mass
  • desulfurization / denitrogenation is possible in the first step, but the purpose is different from that of the conventional hydrotreatment.
  • Providing such a first step is preferable for ensuring that the urea adduct value of the article to be processed (lubricant base oil) obtained after the third step is 4% by mass or less.
  • Examples of the hydrogenation catalyst used in the first step include a catalyst containing a Group 6 metal, a Group 8 to 10 metal, and a mixture thereof.
  • Preferred metals include nickel, tungsten, molybdenum, cobalt, and mixtures thereof.
  • the hydrogenation catalyst can be used in a form in which these metals are supported on a refractory metal oxide support, and the metal is usually present as an oxide or sulfide on the support. When a metal mixture is used, the metal may be present as a bulk metal catalyst in which the amount of metal is 30% by mass or more based on the total amount of the catalyst.
  • the metal oxide support examples include oxides such as silica, alumina, silica-alumina, and titania, and among these, alumina is preferable. Preferred alumina is ⁇ -type or ⁇ -type porous alumina.
  • the amount of the metal supported is preferably in the range of 0.5 to 35% by mass based on the total amount of the catalyst. Further, when a mixture of Group 9-10 metal and Group 6 metal is used, either Group 9 or Group 10 metal is present in an amount of 0.5-5% by weight, based on the total amount of catalyst, The Group 6 metal is preferably present in an amount of 5 to 30% by mass. Metal loading may be measured by atomic absorption spectroscopy, inductively coupled plasma emission spectroscopy, or other methods specified by ASTM for individual metals.
  • the acidity of the metal oxide support can be controlled by adding additives, controlling the properties of the metal oxide support (for example, controlling the amount of silica incorporated in the silica-alumina support), and the like.
  • additives include halogens, especially fluorine, phosphorus, boron, yttria, alkali metals, alkaline earth metals, rare earth oxides, and magnesia.
  • Cocatalysts such as halogen generally increase the acidity of the metal oxide support, but weakly basic additives such as yttria or magnesia tend to weaken the acidity of such support.
  • the treatment temperature is preferably 150 to 450 ° C., more preferably 200 to 400 ° C.
  • the hydrogen partial pressure is preferably 1400 to 20000 kPa, more preferably 2800 to 14000 kPa
  • the liquid space velocity (LHSV) is preferably 0.1 ⁇ 10 hr -1, more preferably 0.1 ⁇ 5 hr -1
  • a hydrogen / oil ratio is preferably 50 ⁇ 1780m 3 / m 3, more preferably 89 ⁇ 890m 3 / M 3 .
  • said conditions are an example and the hydrotreating conditions in the 1st process for the urea adduct value and viscosity index of the to-be-processed object obtained after a 3rd process satisfy
  • fill the said conditions respectively are a raw material, a catalyst, an apparatus, etc. It is preferable to select appropriately according to the difference.
  • the object to be processed after the hydrogenation treatment in the first step may be used as it is in the second step, but the object to be processed is stripped or distilled to generate gas from the object to be processed (liquid product). It is preferable to provide a step of separating and removing the object between the first step and the second step. Thereby, the nitrogen content and sulfur content contained in the workpiece can be reduced to a level that does not affect the long-term use of the hydrodewaxing catalyst in the second step.
  • the object of separation and removal by stripping or the like is mainly gaseous foreign matters such as hydrogen sulfide and ammonia, and stripping can be performed by ordinary means such as a flash drum and a fractionator.
  • the conditions of the hydrogenation treatment in the first step are mild, there is a possibility that the remaining polycyclic aromatics may pass through depending on the raw materials used. It may be removed by purification.
  • the hydrodewaxing catalyst used in the second step may contain either crystalline or amorphous material.
  • the crystalline material include molecular sieves having a 10- or 12-membered ring passage mainly composed of aluminosilicate (zeolite) or silicoaluminophosphate (SAPO).
  • zeolite include ZSM-22, ZSM-23, ZSM-35, ZSM-48, ZSM-57, ferrierite, ITQ-13, MCM-68, MCM-71 and the like.
  • An example of an aluminophosphate is ECR-42.
  • molecular sieves include zeolite beta and MCM-68.
  • ZSM-48 it is preferable to use one or more selected from ZSM-48, ZSM-22, and ZSM-23, and ZSM-48 is particularly preferable.
  • a hydrodewaxing catalyst that has been subjected to a reduction treatment in advance may be subjected to hydrodewaxing.
  • examples of the amorphous material for the hydrodewaxing catalyst include alumina doped with a group 3 metal, fluorinated alumina, silica-alumina, fluorinated silica-alumina, silica-alumina and the like.
  • Preferred embodiments of the dewaxing catalyst include those equipped with a metal hydrogenation component that is difunctional, ie, at least one Group 6 metal, at least one Group 8-10 metal, or a mixture thereof.
  • Preferred metals are group 9-10 noble metals such as platinum, palladium or mixtures thereof.
  • the mounting amount of these metals is preferably 0.1 to 30% by mass based on the total amount of the catalyst. Examples of the catalyst preparation and the metal mounting method include an ion exchange method and an impregnation method using a decomposable metal salt.
  • binder material when using a molecular sieve, it may be combined with a binder material having heat resistance under hydrodewaxing conditions, or may be without a binder (self-bonding).
  • Binder materials include silica, alumina, silica-alumina, binary combinations of silica and other metal oxides such as titania, magnesia, tria, zirconia, silica-alumina-tria, silica-alumina-magnesia, etc.
  • Inorganic oxides such as a combination of three components of oxides such as
  • the amount of molecular sieve in the hydrodewaxing catalyst is preferably 10 to 100% by mass, more preferably 35 to 100% by mass, based on the total amount of the catalyst.
  • the hydrodewaxing catalyst is formed by a method such as spray drying or extrusion.
  • the hydrodewaxing catalyst can be used in a sulfided or non-sulfided form, and a sulfided form is preferred.
  • the temperature is preferably 250 to 400 ° C., more preferably 275 to 350 ° C.
  • the hydrogen partial pressure is preferably 791 to 20786 kPa, more preferably 1480 to 17339 kPa
  • the liquid space velocity is preferably is 0.1 ⁇ 10 hr -1, more preferably 0.1 ⁇ 5 hr -1
  • a hydrogen / oil ratio is preferably 45 ⁇ 1780m 3 / m 3, more preferably 89 ⁇ 890m 3 / m 3.
  • said conditions are an example and the hydrodewaxing conditions in the 2nd process for the urea adduct value and viscosity index of the to-be-processed object obtained after a 3rd process satisfy
  • fill the said conditions are a raw material, a catalyst, and an apparatus, respectively. It is preferable to select appropriately according to the difference.
  • the material to be treated that has been hydrodewaxed in the second step is subjected to hydrorefining in the third step.
  • Hydrorefining is a form of mild hydrotreating that aims to saturate olefins and residual aromatic compounds by hydrogenation in addition to removal of residual heteroatoms and hues.
  • the hydrorefining in the third step can be carried out in cascade with the dewaxing step.
  • the hydrorefining catalyst used in the third step is preferably a metal oxide carrier on which a Group 6 metal, a Group 8-10 metal, or a mixture thereof is supported.
  • Preferred metals include noble metals, especially platinum, palladium and mixtures thereof. If a mixture of metals is used, it may be present as a bulk metal catalyst where the amount of metal is 30% by weight or more based on the catalyst.
  • the metal content of the catalyst is preferably 20% by mass or less for non-noble metals and 1% by mass or less for noble metals.
  • the metal oxide support may be either amorphous or crystalline oxide. Specific examples include low acid oxides such as silica, alumina, silica-alumina or titania, with alumina being preferred. From the viewpoint of saturation of the aromatic compound, it is preferable to use a hydrorefining catalyst in which a metal having a relatively strong hydrogenation function is supported on a porous support.
  • M41S series catalysts are mesoporous materials with high silica content, and specifically include MCM-41, MCM-48 and MCM-50.
  • Such a hydrorefining catalyst has a pore diameter of 1.5 to 10 nm, and MCM-41 is particularly preferable.
  • MCM-41 is an inorganic porous non-layered phase having a hexagonal arrangement of uniformly sized pores.
  • the physical structure of MCM-41 is like a bundle of straws where the opening of the straw (cell diameter of the pores) is in the range of 1.5 to 10 nm.
  • MCM-48 has cubic symmetry and MCM-50 has a layered structure.
  • MCM-41 can be made with pore openings of different sizes in the mesoporous range.
  • the mesoporous material may have a metal hydrogenation component that is at least one of Group 8, 9 or 10 metal, and the metal hydrogenation component is preferably a noble metal, particularly a Group 10 noble metal, platinum Most preferred is palladium, or a mixture thereof.
  • the temperature is preferably 150 to 350 ° C., more preferably 180 to 250 ° C.
  • the total pressure is preferably 2859 to 20786 kPa
  • the liquid space velocity is preferably 0.1 to 5 hr ⁇ 1. More preferably, it is 0.5 to 3 hr ⁇ 1 and the hydrogen / oil ratio is preferably 44.5 to 1780 m 3 / m 3 .
  • said conditions are an example and the hydrogenation production
  • fill the said conditions respectively are the difference of a raw material or a processing apparatus. It is preferable to select appropriately according to.
  • Lubricating oil base oil is preferably 70 to 95% by mass, particularly preferably 75 to 90% by mass, based on the total amount of the grease composition. If the content of the lubricating base oil is outside the range of 70 to 95% by mass, it becomes difficult to easily prepare a grease composition having a desired consistency.
  • Thickeners include soap-type thickeners such as metal soaps and composite metal soaps, benton, silica gel, urea-type compounds (diurea compounds, urea / urethane compounds, urethane compounds, etc.) Any thickener can be used. From the viewpoint of heat resistance, it is desirable to contain at least one selected from urea compounds and urea / urethane compounds.
  • soap-based thickener examples include sodium soap, calcium soap, aluminum soap, lithium soap, calcium composite soap, aluminum composite soap, lithium composite soap and the like.
  • urea thickener examples include urea compounds such as diurea compounds, triurea compounds, tetraurea compounds, and polyurea compounds; urea / urethane compounds; urethane compounds such as diurethane compounds, or a mixture of two or more of these. Of these, diurea compounds are preferred.
  • diurea thickener examples include diurea compounds obtained by reaction of diisocyanate and amine.
  • diisocyanates examples include aliphatic diisocyanates, alicyclic diisocyanates, and aromatic diisocyanates.
  • diisocyanates examples include diisocyanates having a hydrocarbon group.
  • the hydrocarbon group may be saturated or unsaturated, and may be linear or branched.
  • the aliphatic diisocyanate includes octadecane diisocyanate, decane diisocyanate, hexane diisocyanate, the alicyclic diisocyanate includes cyclohexyl diisocyanate, dicyclohexylmethane diisocyanate, and the aromatic diisocyanate includes phenylene diisocyanate, tolylene diisocyanate, diphenyl diisocyanate. , Diphenylmethane diisocyanate and the like are preferable.
  • monoamines include aliphatic monoamines, alicyclic monoamines, and aromatic monoamines.
  • Examples of these monoamines include amines having a hydrocarbon group.
  • the hydrocarbon group may be saturated or unsaturated, and may be linear or branched.
  • alicyclic monoamines include octylamine, dodecylamine, hexadecylamine, stearylamine, oleylamine, alicyclic monoamines include cyclohexylamine, dicyclohexylamine, and aromatic monoamines such as aniline and p-toluidine. preferable.
  • Thickeners may be used alone or in combination of two or more.
  • the content of the thickener is only required to obtain a desired consistency.
  • it is preferably 2 to 30% by mass or 5 to 30% by mass, more preferably 5 to 20% by mass, based on the total amount of the grease composition. % Or 10 to 20% by mass.
  • the grease composition according to the present embodiment is generally used in lubricating oils and greases as necessary.
  • detergents, dispersants, antiwear agents, viscosity index improvers, and antioxidants An agent, extreme pressure agent, rust inhibitor, corrosion inhibitor and the like can be added as appropriate.
  • Components other than the above components are preferably 10% by mass or less, more preferably 5% by mass or less, based on the total amount of the grease composition.
  • the method for producing a grease composition according to this embodiment includes a step of obtaining a grease composition by mixing a lubricating base oil and a thickener.
  • a thickener prepared in advance may be mixed with a lubricating base oil, or a raw material for the thickener is blended with the lubricating base oil and reacted in the lubricating base oil.
  • You may obtain a thickener.
  • a urea-based thickener when used, it may be blended with the lubricating base oil in the form of a urea compound, but diisocyanate and amines are blended with the lubricating base oil and reacted during the preparation of the grease.
  • a system thickener may be used.
  • the bottom fraction obtained from the fuel oil hydrocracking apparatus was used as a raw material for the lubricant base oil, and hydrotreating was performed using a hydrotreating catalyst. At this time, the reaction temperature and the liquid space velocity were adjusted so that the decomposition rate of normal paraffin in the raw material oil was 10% by mass or less. Further, the hydrotreated dewaxing is carried out at a temperature range of 315 to 325 ° C. using a zeolite hydrodewaxing catalyst adjusted to a noble metal content of 0.1 to 5 mass%. And dewaxed oil was obtained. Further, this dewaxed oil was hydrorefined using a hydrorefining catalyst.
  • Base oil B The fraction separated by distillation under reduced pressure in the step of refining the solvent refined base oil was subjected to hydrogenation after solvent extraction with furfural and then dewaxed with a mixed solvent of methyl ethyl ketone and toluene.
  • the wax that was removed during solvent dewaxing and obtained as slack wax was used as a raw material for lubricating base oil, and hydrotreated using a hydrotreating catalyst. At this time, the reaction temperature and the liquid space velocity were adjusted so that the decomposition rate of normal paraffin in the raw material oil was 10% by mass or less. Further, the hydrotreated dewaxing is carried out at a temperature range of 315 to 325 ° C.
  • the base oil C was a lubricating base oil having the following properties, obtained by subjecting a distillate obtained by distilling an atmospheric distillation residue under reduced pressure to a solvent.
  • Urea adduct value 5% by mass % C P : 66 % C A : 5
  • Viscosity index 100
  • Thickener A As the thickener A, a lithium stearate compound obtained by reacting stearic acid (1 molar equivalent) with lithium hydroxide (1 molar equivalent) was used.
  • Thickener B As the thickener B, a diurea compound obtained by reacting diphenylmethane diisocyanate (1 molar equivalent) with cyclohexylamine (2 molar equivalent) was used.
  • Phenyl- ⁇ -naphthylamine was used as an amine antioxidant.
  • Example 1 to 4 Comparative Examples 1 to 4
  • grease compositions having the compositions shown in Table 1 were prepared.
  • base oil A, B, C or D was used as the lubricating base oil, and stearic acid was added to this lubricating base oil and dissolved by heating.
  • a solution obtained by dissolving lithium hydroxide in water by heating was added, and water was evaporated while heating and stirring.
  • a gel-like substance is produced when the base oil is added, so cool it with stirring, add the antioxidant, and then pass them through a roll mill.
  • the grease compositions of Examples 1 and 3 and Comparative Examples 1 and 3 were obtained.
  • base oil A, B, C or D was used as the lubricating base oil, and diphenylmethane diisocyanate was added to this lubricating base oil and dissolved by heating.
  • diphenylmethane diisocyanate was added to this lubricating base oil and dissolved by heating.
  • a substance obtained by dissolving cyclohexylamine in the same base oil is added, a gel-like substance is formed. Therefore, after adding an antioxidant, these are passed through a roll mill, and the greases of Examples 2, 4 and Comparative Examples 2, 4 A composition was obtained.
  • the grease composition of the present invention has an exceptional effect that the torque required for rotation of the bearing can be reduced while maintaining the bearing fatigue life. Therefore, the grease composition of the present invention can be suitably used for lubrication of machine elements such as rolling bearings, plain bearings, ball screws, linear motion guides, and gears, and is useful in industrial machines and transportation machine systems. .

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

Une composition de graisse selon la présente invention comprend: une huile à base d'huile lubrifiante présentant une fraction d'adduit d'urée inférieure ou égale à 4 % en masse, un %CP supérieur ou égal à 70, un %CA inférieur ou égale à 2 et un indice de viscosité supérieur ou égal à 105; et un agent épaississant.
PCT/JP2014/078250 2013-10-23 2014-10-23 Composition de graisse Ceased WO2015060399A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008274236A (ja) * 2007-03-30 2008-11-13 Nippon Oil Corp 潤滑油組成物
WO2009072524A1 (fr) * 2007-12-05 2009-06-11 Nippon Oil Corporation Composition d'huile lubrifiante
JP2009227941A (ja) * 2008-03-25 2009-10-08 Nippon Oil Corp 潤滑油基油及びその製造方法並びに潤滑油組成物
JP2009227942A (ja) * 2008-03-25 2009-10-08 Nippon Oil Corp 潤滑油基油及びその製造方法並びに潤滑油組成物
JP2010235851A (ja) * 2009-03-31 2010-10-21 Jx Nippon Oil & Energy Corp 潤滑油組成物

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5165921B2 (ja) * 2007-04-27 2013-03-21 Ｎｏｋクリューバー株式会社 グリース組成物

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008274236A (ja) * 2007-03-30 2008-11-13 Nippon Oil Corp 潤滑油組成物
WO2009072524A1 (fr) * 2007-12-05 2009-06-11 Nippon Oil Corporation Composition d'huile lubrifiante
JP2009227941A (ja) * 2008-03-25 2009-10-08 Nippon Oil Corp 潤滑油基油及びその製造方法並びに潤滑油組成物
JP2009227942A (ja) * 2008-03-25 2009-10-08 Nippon Oil Corp 潤滑油基油及びその製造方法並びに潤滑油組成物
JP2010235851A (ja) * 2009-03-31 2010-10-21 Jx Nippon Oil & Energy Corp 潤滑油組成物

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