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CN1070181A - Method for preparing n-decane from liquid wax - Google Patents

Method for preparing n-decane from liquid wax Download PDF

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Publication number
CN1070181A
CN1070181A CN 92111179 CN92111179A CN1070181A CN 1070181 A CN1070181 A CN 1070181A CN 92111179 CN92111179 CN 92111179 CN 92111179 A CN92111179 A CN 92111179A CN 1070181 A CN1070181 A CN 1070181A
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China
Prior art keywords
decane
tower
wax
temperature
liquid wax
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Granted
Application number
CN 92111179
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Chinese (zh)
Other versions
CN1027888C (en
Inventor
金彰礼
李勋成
刘昆元
高惠芳
胡爱宝
涂仁强
范建西
雷英春
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PETROLEUM REFINERY YANSHAN PETROCHEMICALS CORP BEIJING
BEIJING COLLEGE OF CHEMICAL TECHNOLOGY
Original Assignee
PETROLEUM REFINERY YANSHAN PETROCHEMICALS CORP BEIJING
BEIJING COLLEGE OF CHEMICAL TECHNOLOGY
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Application filed by PETROLEUM REFINERY YANSHAN PETROCHEMICALS CORP BEIJING, BEIJING COLLEGE OF CHEMICAL TECHNOLOGY filed Critical PETROLEUM REFINERY YANSHAN PETROCHEMICALS CORP BEIJING
Priority to CN 92111179 priority Critical patent/CN1027888C/en
Publication of CN1070181A publication Critical patent/CN1070181A/en
Application granted granted Critical
Publication of CN1027888C publication Critical patent/CN1027888C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

本发明由液蜡制备正癸烷的方法是以C8~C15 正构烷烃为主组成的液蜡为原料,经过脱重蜡、脱轻 蜡、正癸烷精馏和吸附工序,得到正癸烷产品,还能得 到铝箔轧制油和皂化液蜡。当液蜡中含量C10正构 烷烃≥2wt%,C9、C10、C11中的异构烷烃<2wt%、芳 烃<1wt%,烯烃<1.5wt%、硫化物<30ppm时,可 以得到纯度为98.6wt%以上的正癸烷产品。该方法 生产流程简单,操作容易、生产成本低。

The method for preparing n-decane from liquid wax in the present invention uses liquid wax mainly composed of C 8 ~ C 15 normal alkanes as raw material, and undergoes heavy wax removal, light wax removal, n-decane rectification and adsorption processes to obtain n-decane Decane products, aluminum foil rolling oil and saponified liquid wax can also be obtained. When the content of C 10 normal paraffins in liquid wax is ≥ 2wt%, isoparaffins in C 9 , C 10 , and C 11 are < 2wt%, aromatics < 1wt%, olefins < 1.5wt%, and sulfides < 30ppm, you can get A n-decane product with a purity of more than 98.6 wt%. The method has the advantages of simple production process, easy operation and low production cost.

Description

The method for preparing n-decane by liquid wax
The present invention relates to the preparation method of n-decane, particularly is the preparation method of raw material with liquid wax.
N-decane requires the purity height as the solvent of polypropylene catalyst.Useful alpha-methyl styrene method of hydrotreating makes, owing to be to adopt pressurization catalytic reaction to produce, therefore investment is big, the cost height, and the product component complexity that this method obtains is difficult to separate, so the quality of n-decane product also is difficult for guaranteeing.
The method that the purpose of this invention is to provide the higher n-decane product of a kind of purity of cheapness.
The method for preparing n-decane that the present invention proposes, raw material adopts liquid wax, and it is that a kind of normal paraffin that contains is main, mainly by C 8~C 15The hydrocarbon mixture that normal paraffin is formed, generally it contains C 10Normal paraffin (3~5) wt%.Raw material is through taking off heavy wax, taking off light wax, n-decane rectifying and absorption process and obtain the n-decane product.Can also obtain simultaneously aluminum foil rolling oil and saponification liquor wax product.
In taking off heavy wax operation, the tower top temperature of taking off heavy wax tower is that 200~210 ℃ of tower still temperature are 240~245 ℃, theoretical plate number 15-25, take off in the light wax operation, the tower top temperature of taking off light wax tower is 160~170 ℃, tower still temperature is 210~220 ℃, theoretical plate number 28-40, in the n-decane rectification working process, the rectifying tower tower top temperature is 170~180 ℃, tower still temperature is 185.2~185.5 ℃, theoretical plate number 35-50, take off heavy wax, the equipment that takes off light wax, n-decane rectification working process is packing tower or tray column, (0.1-0.15MPa) operation under normal pressure.The service temperature of adsorption tanks is 150~190 ℃, and pressure is 0.3~0.5MPa, and air speed is 0.5~1NM 3/ M 3Sorbent material.The used sorbent material of adsorption tanks is molecular sieve, silica gel or carclazyte.Contain C in the raw material 10The high more separation acquisition n-decane product that helps more of normal paraffin amount.
Of the present invention with C 6~C 15Normal paraffin is in master's the liquid wax, wherein C 10Normal paraffin also can obtain highly purified n-decane product in the time of can be less than 2wt%, considers economically rationally and can guarantee the quality of this product, makes its purity more than 98.6wt%, requires C in the raw material 10Normal paraffin 〉=2wt%, C 9, C 10, C 11In isoparaffin<2wt%, aromatic hydrocarbons<1wt%, alkene<1000wt%, sulfide<30ppm.The service temperature of each operation is regulated in the said temperature scope according to the component of raw material and the change of component of Ge Ta charging.
Because the raw material that the present invention adopts is the product in the petroleum refining process, raw material sources are abundant.Main rectifying and the adsorptive separation technology process of adopting, therefore little than the method investment of hydrogenation reaction, Production Flow Chart is simple, processing ease, production cost is low, and obtains the higher n-decane product of purity easily.
Accompanying drawing is a general flow chart of the present invention.
As shown in drawings, heavy wax tower 2 is taken off in liquid wax 1 adding that raw material forms as mentioned above, and tower reactor material 4 is C12~C 15Cut, tower reactor material 4 obtain low-sulfur, low fragrant aluminum foil rolling oil 14 after sending into adsorption tanks 11 desulfurization, decolouring, and cat head material material 3 behind condenser 17 is sent into and taken off light wax tower 5, and tower reactor material 7 is mainly C11~C 13Cut, tower reactor material 7 are sent into adsorption tanks 12 and obtain saponification liquor wax 15 after the decolouring desulfurization, and the cat head material that takes off light wax tower 5 is mainly C8 to C10Cut, the material 6 behind condenser 18 enters n-decane rectifying column 8, and cat head material 9 is mainly C8、C 9Cut can be made fuel oil, and tower reactor material 10 obtains n-decane product 16 behind the deolefination in the adsorption tanks 13.
The n-decane product that adopts the inventive method to produce, through applying unit analytical test result: density 0.730, bromine number 0.03 gram bromine/100 grams, residue 0.002%, moisture content 80ppm, boiling range: 172.5 ℃ of initial boiling points, do 174.6 ℃, n-decane purity 98.61wt% meets Yanshan Petrochemical Co.'s company standard. Its cost only has 1/2 of imported product price.
Embodiment 1:
As shown in table 1, raw material is C 8~C 15Normal paraffin is main liquid wax, and wherein: n-decane is 1.95wt%.C 9, C 10, C 11In isoparaffin<2wt%, alkene<1.5wt%, aromatic hydrocarbons<1wt%, sulfide<30ppm.Obtain product n-decane (purity is 98.62wt%), aluminum foil rolling oil and saponification liquor wax.
Embodiment 2:
As shown in table 2, raw material is C 8~C 15Normal paraffin is main liquid wax, and wherein: n-decane is 5.0wt%.Obtain product n-decane (purity 98.63wt%), aluminum foil rolling oil and saponification liquor wax.
Embodiment 3:
As shown in table 3, raw material is C 8~C 15Normal paraffin is main liquid wax, and wherein: n-decane is 9.6wt%, obtains product n-decane (purity is 98.99wt%), aluminum foil rolling oil and saponification liquor wax.
Table 1.
One, takes off heavy wax tower Two, take off light wax tower Three, n-decane rectifying tower
The thing stream number 1 3 4 6 7 9 10
The logistics title Charging Cat head The tower still Cat head The tower still Cat head The tower still
Temperature (℃) 180 63.2 244.1 51.9 217.5 50.5 185.2
Pressure (MPa) 0.120 0.100 0.126 0.100 0.125 0.100 0.125
Weight fraction C8+C9 0.0030 0.0049 0 0.1332 0 0.9945 0.0120
C10 0.0200 0.0324 0 0.8651 0.0009 0.0055 0.9862
C11 0.2550 0.4121 0.0010 0.0017 0.4277 0 0.0018
≥C12 0.7220 0.5506 0.9990 0 0.5714 0 0
Reflux ratio 1.0 25.89 7.54
Stage number 18 35 45
Table 2.
One, takes off heavy wax tower Two, take off light wax tower Three, n-decane rectifying tower
The thing stream number 1 3 4 6 7 9 10
The logistics title Charging Cat head The tower still Cat head The tower still Cat head The tower still
Temperature (℃) 180 80.3 243.5 53.3 217.3 50.5 185.2
Pressure (MPa) 0.120 0.100 0.126 0.100 0.125 0.100 0.125
Weight fraction C8+C9 0.0050 0.0080 0 0.0884 0 0.9945 0.0125
C10 0.0520 0.0831 0 0.9105 0.0009 0.0055 0.9863
C11 0.2500 0.3988 0.0010 0.0011 0.4083 0 0.0012
≥C12 0.6930 0.5101 0.9990 0 0.5608 0 0
Reflux ratio 1.0 14.04 11.63
Stage number 16 33 40
Table 3.
One, takes off heavy wax tower Two, take off light wax tower Three, n-decane rectifying tower
The thing stream number 1 3 4 6 7 9 10
The logistics title Charging Cat head The tower still Cat head The tower still Cat head The tower still
Temperature (℃) 180 77.2 243.3 54.3 216.8 50.5 185.3
Pressure (MPa) 0.120 0.100 0.126 0.100 0.125 0.100 0.125
Weight fraction C8+C9 0.0060 0.0090 0 0.0579 0 0.9945 0.0090
C10 0.0980 0.1464 0 0.9410 0.0009 0.0055 0.9899
C11 0.2610 0.3895 0.0010 0.0011 0.4607 0 0.0011
≥C12 0.6350 0.4551 0.9990 0 0.5384 0 0
Reflux ratio 1.0 9.219 18.19
Stage number 20 30 32

Claims (3)

1、一种制备正癸烷的方法,其特征在于原料用液蜡,经过脱重蜡、脱轻蜡、正癸烷精馏和吸附工序制得:1. A method for preparing n-decane, characterized in that liquid wax is used as a raw material, which is obtained through heavy wax removal, light wax removal, n-decane rectification and adsorption processes: (1)液蜡是一种含正构烷烃为主的。主要由C8~C15正构烷烃组成的烃类混合物;(1) Liquid wax is a kind mainly containing normal alkanes. Hydrocarbon mixture mainly composed of C 8 ~C 15 normal alkanes; (2)脱重蜡工序:脱重蜡塔塔顶温度为200~210℃,塔釜温度为240~245℃,理论塔板数为15-25;(2) Heavy wax removal process: the temperature at the top of the heavy wax removal tower is 200-210°C, the temperature at the bottom of the tower is 240-245°C, and the number of theoretical plates is 15-25; (3)脱轻蜡工序:脱轻蜡塔塔顶温度为160~170℃,塔釜温度为210~220℃,理论塔板数为28-40;(3) Light wax removal process: the top temperature of the light wax removal tower is 160-170°C, the temperature of the bottom of the tower is 210-220°C, and the number of theoretical plates is 28-40; (4)正癸烷精馏工序:精馏塔塔顶温度为170~180℃,塔釜温度为185.2~185.5℃,理论塔板数为35-50;(4) N-decane rectification process: the temperature at the top of the rectification tower is 170-180°C, the temperature at the bottom of the tower is 185.2-185.5°C, and the number of theoretical plates is 35-50; (5)吸附工序:正癸烷精馏后的吸附罐的操作温度为150~190℃,压力为0.3~0.5MPa,空速为0.5~1NM3/M3吸附剂。(5) Adsorption process: the operating temperature of the adsorption tank after rectification of n-decane is 150-190° C., the pressure is 0.3-0.5 MPa, and the space velocity is 0.5-1 NM 3 /M 3 adsorbent. 2、根据权利要求1所述的方法,其特征在于液蜡中含量:C10正构烷烃≥2wt%,C9,C10,C11中的异构烷烃<2wt%,芳烃<1wt%,烯烃<1.5wt%,硫化物<30PPM。2. The method according to claim 1, characterized in that the content in liquid wax: C 10 normal paraffins ≥ 2wt%, C 9 , C 10 , C 11 isoparaffins < 2wt%, aromatics < 1wt%, Olefin <1.5wt%, sulfide <30PPM. 3、根据权利要求1所述的方法,其特征在于吸附工序的吸附剂为分子筛、硅胶或白土。3. The method according to claim 1, characterized in that the adsorbent in the adsorption step is molecular sieve, silica gel or clay.
CN 92111179 1992-09-29 1992-09-29 Method for preparing n-decane from liquid wax Expired - Fee Related CN1027888C (en)

Priority Applications (1)

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CN 92111179 CN1027888C (en) 1992-09-29 1992-09-29 Method for preparing n-decane from liquid wax

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Application Number Priority Date Filing Date Title
CN 92111179 CN1027888C (en) 1992-09-29 1992-09-29 Method for preparing n-decane from liquid wax

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CN1027888C CN1027888C (en) 1995-03-15

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101732883B (en) * 2010-01-21 2012-05-30 天津天大天海化工新技术有限公司 Adsorptive rectification tower for decoloring aromatic solvent oil and process method thereof
CN109553505A (en) * 2017-09-27 2019-04-02 中国石油天然气股份有限公司 Method for producing n-decane, n-dodecane and n-tetradecane from polyethylene wax by-product light wax oil
CN109628141A (en) * 2019-01-29 2019-04-16 中科合成油技术有限公司 A method of by F- T synthesis hydrofined oil separating monomer n-alkane

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101732883B (en) * 2010-01-21 2012-05-30 天津天大天海化工新技术有限公司 Adsorptive rectification tower for decoloring aromatic solvent oil and process method thereof
CN109553505A (en) * 2017-09-27 2019-04-02 中国石油天然气股份有限公司 Method for producing n-decane, n-dodecane and n-tetradecane from polyethylene wax by-product light wax oil
CN109553505B (en) * 2017-09-27 2021-09-28 中国石油天然气股份有限公司 Method for producing n-decanone, n-dodecane and n-tetradecane from polyethylene wax byproduct light wax oil
CN109628141A (en) * 2019-01-29 2019-04-16 中科合成油技术有限公司 A method of by F- T synthesis hydrofined oil separating monomer n-alkane

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