Method for reducing content of polyethylene wax during ethylene oligomerization reaction

A polyethylene wax and ethylene oligomerization technology, applied in chemical instruments and methods, hydrocarbons, hydrocarbons, etc., can solve the problems of activity loss, activity reduction, light products, etc.

Inactive Publication Date: 2014-04-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the loss of activity is relatively large, and the effect of reducing polyethylene wax is general, and it is difficult to produce economic benefits
In addition, by changing the ligand structure, people have done a lot of exploration and research on catalysts coordinated by new ligands. However, the new catalytic system often leads to a significant decrease in activity or light products (the main products are low-carbon olefins such as C4). not ideal
[0006] In summary, as far as the prior art is concerned, there is no way to effectively reduce the problem of oligomerization catalyst by-product polyethylene wax

Method used

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  • Method for reducing content of polyethylene wax during ethylene oligomerization reaction
  • Method for reducing content of polyethylene wax during ethylene oligomerization reaction
  • Method for reducing content of polyethylene wax during ethylene oligomerization reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Under the protection of nitrogen, the pyridine bis-imine ligand L{2,6-bis-[(2-methyl-4-methoxyanilinoethyl)pyridine]} shown in formula a and chlorinated After iron is blended in a molar ratio of 1:1, a catalyst represented by formula a' is obtained. dubbed into 2×10 -6 mol / ml suspension of main catalyst in toluene. The cocatalyst methylaluminoxane (MAO) is a 10wt% toluene solution, and the concentration of the substance is about 1.5mol / L. The polyethylene wax inhibitor is tetraethyl silicate (TEOS).

[0051] The structural formula of 2,6-bis-[(2-methyl-4-methoxyanilinoethyl)pyridine]:

[0052]

[0053]A 250ml oligomerization reactor was heated to 90°C, and vacuum-baked for 2 hours, during which it was replaced three times with high-purity nitrogen and three times with polymer-grade ethylene. The temperature of the reactor was adjusted to a reaction temperature of 50° C. by circulating jacketed cooling water, and 50 ml of toluene was added as a reaction medium. S...

Embodiment 2

[0057] Add a certain amount of polyethylene wax inhibitor TEOS with a molar ratio of Si:Al=1.0, and other operations are the same as in Example 1.

[0058] After the gas-liquid-solid separation of the reaction product, the polyethylene wax was dried and weighed to obtain 0.39g; the liquid phase α-olefin product was analyzed by chromatography to obtain 3.11g; the content of polyethylene wax in the total product was 11.1wt.%. The activity of polyethylene wax is 0.39×10 6 g / mol Fe / h, α-olefin activity is 3.11×10 6 g / mol Fe / h.

Embodiment 3

[0060] Add a certain amount of polyethylene wax inhibitor TEOS with a molar ratio of Si:Al=3.0, and other operations are the same as in Example 1.

[0061] After the gas-liquid-solid separation of the reaction product, the polyethylene wax was dried and weighed to obtain 0.27g; the liquid-phase α-olefin product was analyzed by chromatography to obtain 3.41g; the content of polyethylene wax in the total product was 7.3wt.%. The activity of polyethylene wax is 0.27×10 6 g / mol Fe / h, α-olefin activity is 3.41×10 6 g / mol Fe / h.

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Abstract

The invention discloses a method for reducing the content of polyethylene wax during ethylene oligomerization reaction. The method comprises the steps as follows: adding a polyethylene wax inhibitor, a promoter and a primary catalyst into oligomerization reactor containing reaction medium, controlling the reaction temperature to be proper, introducing a vinyl monomer to reaction pressure, and performing oligomerization reaction. The polyethylene wax inhibitor is selected from one or more of ether, ketone, inner ester, a heterocyclic compound, an organic phosphine compound, a monocarboxylate or polycarboxylic compound and a silicon compound containing at least one Si-OR bond, wherein R adopts a hydroxy group. The method can effectively inhibit the generation of polyethylene wax, and meanwhile, obviously improve the yield of liquid phase alpha-olefin, thereby greatly reducing the content of the polyethylene wax during ethylene oligomerization reaction, and the method is beneficial to the safe and reliable operation of devices, so as to obtain high economic benefits.

Description

technical field [0001] The invention relates to the field of ethylene oligomerization to prepare higher α-olefins, in particular to a method for reducing the content of polyethylene wax by-product in the ethylene oligomerization reaction process. Background technique [0002] Linear alpha-olefins refer to C with double bonds at the ends of the molecule 4 The above linear olefins are very important petrochemical raw materials. Among them, C 4 ~C 24 The linear α-olefins have been widely used in the preparation of high-grade detergents, high-grade alcohols, high-grade lubricating oils, surfactants and oil additives and many other fields. Currently, nonselective oligomerization of ethylene is the preferred method to produce linear α-olefins, especially C 4 ~C 24 The most dominant and promising method for linear α-olefins. [0003] In 1998, Brookhart and Gibson respectively reported iron and cobalt catalysts with double imine pyridine as ligand. The catalytic activity of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C11/02C07C2/22C07C2/32
Inventor 蒋斌波叶健秦一超阳永荣王靖岱黄正梁廖祖维
Owner ZHEJIANG UNIV
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