Method for oligomerization of alpha-olefin based on microchannel reaction

A technology of microchannel reaction and microchannel reactor, which is applied in the synthesis field of fully synthetic lubricating base oil, can solve the problems of many by-products, low pentamer selectivity, long residence time, etc., and achieve improved efficiency and good solubility , the effect of cost reduction

Pending Publication Date: 2018-01-16
上海纳克润滑技术有限公司
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Problems solved by technology

[0009] In order to solve the above-mentioned technical problems, the present invention provides a method for α-olefin oligomerization based on microchannel reaction. First, organic acid is used to modify aluminum trichloride. On the one hand, the activity of its catalytic center is changed to make it suitable for Synthesis of low-viscosity PAO. On the other hand, the modified aluminum trichloride catalyst system has good solubility in halogenated hydrocarbons, which is suitable for microchannel reactions. There are many problems, such as the low selectivity of the three, four and five polymers of the ideal components of lubricating oil. The microchannel reactor has the natural advantages of high-efficiency mass transfer and heat exchange, and can precisely control the reaction temperature and residence time to realize α-olefin oligomers. Different percentages of polymers in

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  • Method for oligomerization of alpha-olefin based on microchannel reaction
  • Method for oligomerization of alpha-olefin based on microchannel reaction

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Effect test

Embodiment 1

[0039] Use organic acid to modify aluminum trichloride: mix acetic acid and aluminum trichloride at a molar ratio of 0.6:1, and use 1,2-dichloroethane as a solvent, react at room temperature for 30 minutes, and the state of the reaction system is no obvious Particles, homogeneously dispersed yellow-brown liquid, the mass concentration of aluminum trichloride is 0.25g / ml.

[0040] The microchannel reaction process used is as follows: figure 1 As shown, the entire device includes a catalytic system and an olefin feed preheating section, a strong mixing reaction section, and a water washing and quenching section. Among them, the reactor is made of ceramic material, the inner diameter of the smallest part of the channel is 0.8mm, and the spherical structure, the liquid holding volume of the strong mixing reaction section is 100ml, and the residence time of the reaction section can be calculated according to the flow rate and the liquid holding volume.

[0041] In the α-olefin pol...

Embodiment 2

[0044] The preparation of the homogeneous aluminum trichloride catalyst system and the microchannel reaction process used are as in Example 1.

[0045] 1-decene is used as the raw material, the reaction temperature is 80°C, the mass flow rate ratio of the feed metering pump of the catalytic system to the 1-decene feed pump is 1:21, and the residence time in the reaction section is 200s.

[0046] The product can be detected by gas chromatography after being neutralized and washed. At this time, the conversion rate of the product is 93%, and the selectivity of trimers, tetramers and pentamers, which are ideal components of lubricating base oil, is 92%.

Embodiment 3

[0048] The preparation of the homogeneous aluminum trichloride catalyst system and the microchannel reaction process used are as in Example 1. Except changing the molar ratio of acetic acid and aluminum trichloride to 1:1. After the modification reaction of aluminum trichloride with organic acid is completed, the catalytic system becomes a clear and transparent liquid.

[0049] 1-decene is used as the raw material, the reaction temperature is 80°C, the mass flow rate ratio of the feed metering pump of the catalytic system to the 1-decene feed pump is 1:15, and the residence time in the reaction section is 300s.

[0050] The product can be detected by gas chromatography after neutralization and washing. At this time, the conversion rate of the product is 76%, and the selectivity of trimers, tetramers and pentamers, which are ideal components of lubricating base oil, is 93%.

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Abstract

The invention provides a method for oligomerization of alpha-olefin based on a microchannel reaction. The method comprises that aluminum trichloride is modified through an organic acid in the presenceof a halogenated hydrocarbon as a solvent, wherein after the modification reaction of aluminum trichloride, the modified aluminum trichloride has good solubility and is uniformly dispersed in the halogenated hydrocarbon, and alpha-olefin as a starting raw material is preheated, is efficiently mixed and fast reacts in the presence of the uniform aluminum trichloride dispersed system as a catalystin a microchannel reactor, wherein the temperature in the reaction channel is 50-150 DEG C, pressure in the reaction channel is 0-20 MPa, staying time is 30-600s and a mass ratio of aluminum trichloride to alpha-olefin is 0.5-5%. In the product, trimer, tetramer and pentamer (lubricating base oil ideal component) selectivity is 95%. Through aluminum trichloride modification, organic dispersibilityis obtained. The method is suitable for a microchannel continuous reaction and has the advantages of high-efficiency mass transfer, stable temperature control and easy regulation and control of product selectivity.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fully synthetic lubricating base oils, and in particular relates to a method for α-olefin oligomerization based on microchannel reaction. Background technique [0002] Poly-α-olefin (Poly-alpha-olefin, PAO) is one of the important synthetic lubricating oils. As lubricating base oil, it accounts for 60-70% of the total synthetic lubricating oils. It has thermal stability, oxidation stability and shear Good stability, low freezing point, high viscosity index, etc. With the rapid development of the automobile industry, the demand for low-viscosity PAO is increasing day by day. As the main catalyst for low-viscosity PAO, boron trifluoride was reported by HamiitonLyleA and others as early as 1964 (US, 3149178[P].1964), Mobil ShubkinRL studied the mechanism and product structure of α-olefin oligomerization catalyzed by BF3 (.Ind.eng.chem.prod.res.dev..1980, 19(1):15-19), and since then the patents...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/22C07C11/02
Inventor 洪显忠宋上飞刘中文
Owner 上海纳克润滑技术有限公司
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