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Ethylene selective trimerization/tetramerization catalyst system as well as preparation method and application thereof

A catalyst and selective technology, applied in the direction of physical/chemical process catalysts, catalytic reactions, chemical instruments and methods, etc., can solve the problems of complex process routes and huge investment in equipment, and achieve simple synthesis, high catalytic activity, and temperature resistance Good results

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

If one wants to obtain high-purity 1-hexene and 1-octene, it needs to be separated by multi-column rectification. The process route is complicated and the investment in equipment is huge.

Method used

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  • Ethylene selective trimerization/tetramerization catalyst system as well as preparation method and application thereof
  • Ethylene selective trimerization/tetramerization catalyst system as well as preparation method and application thereof
  • Ethylene selective trimerization/tetramerization catalyst system as well as preparation method and application thereof

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preparation example Construction

[0051] In one embodiment of the present invention, the preparation method of ligand a is a conventional preparation method, which may specifically include the following steps:

[0052] ① Preparation of monophosphine amine intermediate: Dissolve a certain amount of substituted amine compound in n-hexane and cool to a certain temperature; slowly add a certain amount of n-butyllithium n-hexane solution into the above solution, and naturally rise to room temperature, Stir overnight, filter and wash with an appropriate amount of n-hexane, and drain the filter cake to obtain the lithium salt of the amine compound; disperse the lithium salt of the above-mentioned amine compound in an appropriate amount of n-hexane, cool to a certain temperature, and dissolve a certain amount of disubstituted chlorine The n-hexane solution of phosphorus compound was slowly added dropwise to the above lithium salt, naturally raised to room temperature, stirred overnight, after the volatile components we...

Embodiment 1

[0067] 1. Preparation of ligand N,N'-dicyclopentyl-N,N'-bis(diphenylphosphine)-1-phenylborondiamine (C 40 h 43 BN 2 P 2 )

[0068] ① Preparation of monophosphine amine intermediate:

[0069] in N 2 In an atmospheric glove box, dissolve dehydrated cyclopentylamine (3.40g, 3.2mL, 0.040mol) in dehydrated n-hexane (100mL), cool to -78°C, and dissolve n-butyl Lithium n-hexane solution (17.1mL, 0.041mol, 2.4mol / L) was slowly added dropwise to the above solution, continued to stir overnight after the dropwise addition, after filtering, washed the filter cake twice with 20mL n-hexane, and drained to obtain lithium cyclopentylamide Salt 3.55g (0.039mol, 97.5%).

[0070] The cyclopentylamine lithium salt intermediate product obtained above was dispersed in n-hexane (100mL), cooled to -35°C, diphenylphosphorus chloride (8.60g, 0.039mol) was dissolved in 20mL of n-hexane, and slowly added dropwise to In the above solution, naturally rise to room temperature, stir overnight, vacuu...

Embodiment 2

[0079] 1. Preparation of N,N'-bis(diphenylphosphine)-N,N'-diisopropyl-1-phenylborondiamine (C 36 h 39 BN 2 P 2 )

[0080] ① Preparation of monophosphine amine intermediate:

[0081] in N 2 In a glove box under the atmosphere, dissolve dehydrated isopropylamine (2.36g, 3.42mL, 0.040mol) in dehydrated n-hexane (100mL), cool to -78°C, and add n-butyllithium while stirring n-Hexane solution (17.1mL, 0.041mol, 2.4mol / L) was slowly added dropwise to the above solution, continued to stir overnight after the dropwise addition was completed, washed the filter cake twice with 20mL n-hexane after filtration, and drained to obtain the lithium salt of isopropylamine 2.41 g (0.037 mol, 93.4%).

[0082] Disperse the intermediate product of lithium salt of isopropylamine obtained above in n-hexane (100mL), cool to -35°C, dissolve diphenylphosphorus chloride (8.16g, 0.037mol) in 20mL of n-hexane, slowly add dropwise to the above The solution was naturally raised to room temperature, s...

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Abstract

The invention provides an ethylene trimerization and tetramerization catalyst system as well as a preparation method and application thereof, and belongs to the field of olefin selective trimerization or tetramerization catalysis. The catalyst system is characterized by comprising: a ligand a; a transition metal compound b; the transition metal compound b is a compound containing IIIB-VIIB group or VIII group transition metal; an activator c; the activating agent c is an organic compound containing IIIA group elements; the ligand a at least contains one group as shown in a formula (I), and R1, R2, R3, R4, R5, R6 and R7 can be the same or different and are respectively and independently selected from alkyl and derivatives thereof, aryl and derivatives thereof, halogen and heteroatom-containing substituents. The catalyst system provided by the invention has the advantages of high catalytic activity, high selectivity of target products 1-hexene and 1-octene, less 1-butene and 1-C10 < + >, less by-product oligomer, and the mass percentage gt of C6-C8 linear alpha-olefin in the product; 90%. And the catalyst has good temperature resistance, and the operation temperature of the reaction device can reach 90 DEG C.

Description

technical field [0001] The invention belongs to the field of olefin selective trimerization or tetramerization catalysis, and relates to an ethylene trimerization and tetramerization catalyst system and its preparation method and application. Background technique [0002] As an important class of organic chemical raw materials and intermediates, linear α-olefins can be widely used in the production of high-performance polyethylene, surfactants, synthetic lubricants, and oil additives. In recent years, their market demand has been increasing rapidly. trend. C 4 -C 8 Linear α-olefins can be used as comonomers to copolymerize with ethylene to produce high-performance linear low-density polyethylene, high-density polyethylene and polyolefin elastomers. In particular, high-purity 1-hexene and 1-octene can significantly improve the abrasion resistance, environmental stress cracking resistance and mechanical properties of linear low-density polyethylene and high-density polyethy...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C11/02C07C11/107C07C2/32
CPCB01J31/188B01J31/143C07C2/32B01J2531/0258B01J2531/62B01J2231/20B01J35/19C07C11/02C07C11/107
Inventor 薛宽荣黄德超张飞张舒婷薛玉洁梁金奎
Owner 浙江智英石化技术有限公司
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