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Synthesis method of poly alpha-olefin

A synthesis method and olefin technology, applied in lubricating compositions, base materials, petroleum industry, etc., can solve problems such as poor low temperature performance

Active Publication Date: 2017-10-31
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for synthesizing a polyalpha-olefin lubricating oil base oil with excellent performance by two-step polymerization. The polyalpha-olefin with a highly regular molecular structure is obtained through the first step process, and then through the second step process Add BF with high branching characteristics 3 Polymerize the reaction product of the first step and the remaining monomers to obtain a molecular structure with a suitable degree of branching and a suitable molecular chain length, which not only ensures that the product has good viscosity-temperature characteristics, but also solves the problem of poor low-temperature performance of the product. Therefore, two-step polymerization steps can be used to obtain poly-α-olefin lubricating base oils with excellent comprehensive properties

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The above-mentioned two-step polymerization method is used to carry out the polymerization reaction. First, the reactor is purged three times with nitrogen to remove the air and traces of water in the polymerization reactor, and the first step of polymerization reaction is started: add 100 mL of solvent to the polymerization reactor in sequence. Cyclohexane, 3mL TiCl 4 , add Al(Et) according to the Al / Ti molar ratio of 0.5:1 3 , then add 100mL of the reaction monomer decene-1, start heating and stirring, control the reaction temperature at 50-80°C, stop stirring after 10 minutes of reaction, add 0.1mL of ethanol to terminate the polymerization reaction, when the temperature in the reactor drops to room temperature Carry out the second step of reaction: add 3mL of n-butanol to the reaction kettle, and introduce 0.2MPa BF 3 (about 1.0g), start stirring, the reaction temperature is 10°C, after 0.5h of reaction, stop stirring, empty the reactor, flush with nitrogen for rep...

Embodiment 2

[0032] Adopt the same polymerization method as Example 1: add 100mL solvent successively in the polymerization reactor, 5mlTiCl 4 , add Al(Et) according to the Al / Ti molar ratio of 1:1 3 , then add the reaction monomer decene-1100mL, start to heat up and stir, control the reaction temperature to 50-80°C, stop stirring after 20 minutes of reaction, add 0.1mL ethanol to terminate the polymerization reaction, and proceed when the temperature in the reactor drops to room temperature The second step reaction: add 5mL n-butanol to the reaction kettle, and feed 0.4MPa BF 3 (together 2.0g), start stirring, reaction temperature 60 ℃, after reacting for 1h, stop stirring, after the reaction finishes, carry out product aftertreatment and performance test by the method for embodiment 1. The 100°C viscosity of the obtained product is 47mm 2 / s, the viscosity index is 152, and the pour point is -45°C.

Embodiment 3

[0034] Using the same polymerization method as in Example 1: add 100mL solvent, 7mlTiCl to the polymerization reactor successively 4 , add Al(Et) according to the Al / Ti molar ratio of 2:1 3 , then add the reaction monomer decene-1100mL, start to heat up and stir, control the reaction temperature to 50-80°C, stop stirring after 30 minutes of reaction, add 0.1mL ethanol, terminate the polymerization reaction, and carry out the reaction when the temperature in the reactor drops to room temperature The second step reaction: add 7mL n-butanol to the reaction kettle, and feed 0.6MPa BF 3 (together 3.0g), start stirring, 20 ℃ of reaction temperature, after reacting 1h, stop stirring, the method for embodiment 1 is carried out product aftertreatment and performance test after reaction finishes. The obtained product has a kinematic viscosity of 47mm at 100°C 2 / s, the viscosity index is 152, and the pour point is -48°C.

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Abstract

The invention relates to a synthesis method of poly alpha-olefin. The synthesis method comprises the following steps: carrying out reaction on a C8-C12 olefin monomer for a certain time under the action of a Ziegler-Natta catalyst system; after the reaction is finished, adding a quenching agent, finishing reaction and stopping stirring, extracting heat by virtue of external circulation, lowering a system temperature to room temperature, then adding an initiating agent, introducing BF3, controlling a polymerization temperature, reacting for 0.5-3 hours, and then carrying out aftertreatment, so that a poly alpha-olefin oligomerization mixture is obtained.

Description

technical field [0001] The present invention relates to a method for the synthesis of polyalphaolefins. Background technique [0002] Poly-α-olefin lubricating base oil (PAO) is a type of base oil obtained by polymerization of α-olefins (branched or unbranched) under the action of a catalyst, and then hydrogenated. It is the most promising synthetic base oil. varieties. Compared with mineral base oils, it has high viscosity index, low pour point, good hydrolysis resistance and oxidation stability, wide liquid phase range, small evaporation loss, low pour point, high viscosity index, good thermal oxidation stability, etc. , can meet increasingly stringent OEM specifications, and meet contemporary stringent energy-saving and environmental protection requirements. At the same time, it has good blendability with mineral oil and can be used in fully synthetic or semi-synthetic oils. [0003] The excellent performance of PAO depends on the degree of polymerization, molecular st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/14C08F4/642C08F4/14C10M107/10C10N30/02
CPCC08F110/14C10M107/10C10M2205/003C10M2205/0285C08F4/6421C08F4/14C10N2020/02
Inventor 王秀绘王亚丽黄付玲褚洪岭王斯晗高飞王桂芝徐显明王力搏李瑞峰刘通曹媛媛白玉洁于部伟马克存蒋岩孙恩浩闫义斌朱丽娜韩雪梅韩云光陈谦曾群英孙淑坤
Owner PETROCHINA CO LTD
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