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Ethylene selective trimerization and tetramerization catalytic system and application thereof

A selectivity and ethylene technology, applied in catalytic reactions, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low overall selectivity of linear α-olefins and achieve by-products The effect of less polymer content, high total selectivity, and high catalytic activity

Pending Publication Date: 2022-03-11
浙江智英石化技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention aims to finely adjust the steric hindrance of the active center of the complex in the catalytic system, effectively control the stability of the active center of ethylene selective oligomerization, and make the chain growth reaction and product carbon number distribution controllable, thereby obtaining high catalytic activity, Catalyst system for ethylene selective oligomerization with high 1-hexene and 1-octene selectivity to address C in ethylene oligomerization 6 ~C 8 The problem of low overall selectivity for linear α-olefins

Method used

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  • Ethylene selective trimerization and tetramerization catalytic system and application thereof
  • Ethylene selective trimerization and tetramerization catalytic system and application thereof
  • Ethylene selective trimerization and tetramerization catalytic system and application thereof

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preparation example Construction

[0051] In one embodiment of the present invention, the preparation method of transition metal complex a may include the following steps:

[0052]

[0053] (1) Preparation of Ph 2 PR 1 NL

[0054] Take a certain amount of Ph 2 PR 1 NH, add a small amount of n-hexane and cool in the refrigerator for 10-20 minutes for later use. Take a certain amount of n-BuLi, add a small amount of n-hexane and put it in the refrigerator to cool for 10-15 minutes, then take out the above two medicines, slowly add n-BuLi to the above standby solution, let it rise to room temperature naturally, and stir for about 12 -24h, filter with sand core funnel, wash twice with n-hexane, and get white solid Ph after vacuum drying 2 PR 1 N Li ①.

[0055] (2) Preparation of clofosamine

[0056] Take a certain amount of N,N-dimethylethylenediamine, triethylamine and phosphorus trichloride and dissolve them in appropriate amount of dichloromethane respectively for later use; Chloromethane solution wa...

Embodiment 1

[0072] 1. Preparation of N-cyclopentyl-N-(diphenylphosphino)-N-2,5-dimethyl-2,4-diazaphosphine / Cr complex

[0073]

[0074] (1) Preparation of lithium cyclopentyl (diphenylphosphine) amide ①

[0075]

[0076] Put diphenylphosphine chloride (1.05g, 0.01mol), cyclopentylamine (0.79g, 0.01mol) and triethylamine (1.41g, 0.015mol) into bottles respectively, add appropriate amount of THF to dissolve and set aside. Under vigorous stirring, the THF solution of triethylamine and diphenylphosphorous chloride were successively added dropwise into the THF solution of cyclopentylamine, and allowed to react overnight. The mixture is filtered and the liquid product is vacuum-dried to obtain a white transparent oil as the intermediate N-cyclopentyl-1,1-diphenylphosphineamine.

[0077] Under vigorous stirring, n-butyl lithium (3.3 mL, 0.007 mol, -30°C) in n-hexane was added dropwise to intermediate b (1.94 g, 0.007 mol, -30°C) in n-hexane and reacted overnight. After the reaction, the ...

Embodiment 2

[0090] With embodiment 1. The difference is that R 2 , R 5 For ethyl. The results of catalyst activity, product formation and product selectivity are shown in Table 1.

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Abstract

The invention provides a catalytic system for selective trimerization and tetramerization of ethylene and application of the catalytic system, and belongs to the technical field of transition metal homogeneous catalysis. The catalytic system comprises: a transition metal complex a, wherein the transition metal complex a is an organic metal compound of IVB to VIII groups; a cocatalyst b, wherein the cocatalyst is an organic compound containing a group IIIA element; wherein the transition metal complex a has a structure as shown in a formula (I), R1, R2, R3, R4, R5, R6, R7, R8 and R9 can be the same or different and are independently selected from alkyl, aryl, acetylacetonyl, carbonyl, tetrahydrofuryl or halogen respectively, and R1, R2, R3, R4, R5, R6, R7, R8 and R9 can be the same or different and are independently selected from alkyl, aryl, acetylacetonyl, carbonyl, tetrahydrofuryl or halogen; m is transition metal, and the transition metal comprises chromium, molybdenum, tungsten, cobalt, titanium, tantalum, vanadium, zirconium, iron, nickel or palladium. The catalyst system provided by the invention is used for selective oligomerization of ethylene, and has the characteristics of high catalytic activity, high selectivity of 1-hexene and 1-octene, and few by-products.

Description

technical field [0001] The invention belongs to the technical field of transition metal homogeneous catalysis, and specifically relates to a catalytic system for preparing 1-hexene and 1-octene through selective trimerization and tetramerization of ethylene and an application thereof. Background technique [0002] In recent years, polymer synthetic materials have been continuously innovated, and the market demand for high-end high-performance synthetic materials has increased year by year. The application of advanced linear α-olefins such as 1-hexene, 1-octene and 1-decene in the fields of high-performance polyolefin materials, synthetic lubricating oil base oils and oil additives, and detergents continues to increase, and the demand continues to increase. 4.2% rate growth. Ethylene selective oligomerization is the main method to produce high-purity 1-hexene, 1-octene, 1-decene and 1-dodecene and other advanced linear α-olefins, especially ethylene selective trimerization t...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C11/02C07C11/107C07C2/32
CPCB01J31/1855B01J31/143C07C2/32B01J2531/0258B01J2531/62B01J2231/20B01J35/19C07C11/02C07C11/107
Inventor 薛宽荣
Owner 浙江智英石化技术有限公司
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