Catalyst of ethylene trimerization, and application

A technology of ethylene trimerization and catalyst, applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, organic chemistry, etc., to achieve the effect of good selectivity, less polyethylene and high activity

Active Publication Date: 2006-12-06
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Catalyst of ethylene trimerization, and application
  • Catalyst of ethylene trimerization, and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1. Preparation of (diphenyl) phosphorus nitrogen (cyclopropyl) phosphorus (diphenyl) ligand

[0022] (1) Preparation of N, N-diisopropyl dichlorophosphoramide

[0023] in the N 2 Add dehydrated toluene (100mL) into a fully replaced stirred 250mL reactor, add PCl 3 (21.87mL, 0.25mol), and cooled to -20°C. Diisopropylamine (70 mL, 0.5 mol) was slowly added while stirring at room temperature, stirred for 3 hours, raised to room temperature and continued to react for 2 hours, then filtered and dried to obtain 38.1 g (0.19 mol, 74%) of the product.

[0024] (2) Preparation of phenylmagnesium bromide lattice reagent

[0025] in the N 2 Add dehydrated THF (100 mL) and magnesium powder (9.11 g, 0.375 mol) into a fully replaced stirred 250 mL reactor, cool down in an ice bath and slowly add bromobenzene (11.775 g, 0.075 mol) dropwise. After 2 hours, heat to reflux and continue the reaction for 2 hours to obtain the lattice reagent.

[0026] (3) Preparation of diphenyl phos...

Embodiment 2

[0035] 1. Preparation of (diphenyl) phosphorus nitrogen (cyclopentyl) phosphorus (diphenyl) ligand

[0036] (1) Preparation of N, N-diisopropyl dichlorophosphoramide

[0037] With embodiment 1.

[0038] (2) Preparation of phenylmagnesium bromide lattice reagent

[0039] With embodiment 1.

[0040] (3) Preparation of diphenyl phosphorus chloride

[0041] With embodiment 1.

[0042] (4) Preparation of (diphenyl) phosphorus nitrogen (cyclopentyl) phosphorus (diphenyl)

[0043] in the N 2 Add dehydrated dichloromethane (20mL), triethylamine (3.75mL), and diphenylphosphine chloride (1.326mL, 7.2mol) into a fully replaced stirred 100mL reactor, cool to 0°C, and slowly Add cyclopentylamine (0.415 mL, 3.5 mmol). After stirring for 30 minutes, the reaction was continued at room temperature for 12 hours. Filtration and drying gave the product (0.55 g, 32.68%).

[0044] 2. Preparation of catalyst

[0045] in the N 2 Add dehydrated cyclohexane (10mL), trimethylaluminum (10mL), ...

Embodiment 3

[0049] 1. Preparation of (diphenyl) phosphorus nitrogen (fluorenyl) phosphorus (diphenyl) ligand

[0050] (1) Preparation of N, N-diisopropyl dichlorophosphoramide

[0051] With embodiment 1.

[0052] (2) Preparation of phenylmagnesium bromide lattice reagent

[0053] With embodiment 1.

[0054] (3) Preparation of diphenyl phosphorus chloride

[0055] With embodiment 1.

[0056] (4) Preparation of (diphenyl) phosphorus nitrogen (fluorenyl) phosphorus (diphenyl)

[0057] in the N 2 Add dehydrated dichloromethane (20mL), triethylamine (3.75mL), and diphenylphosphine chloride (1.326mL, 7.2mol) into a fully replaced stirred 100mL reactor, cool to 0°C, and slowly Fluorenamine (0.652 g, 3.6 mmol) was added. After stirring for 30 minutes, the reaction was continued at room temperature for 12 hours. Filtration and drying gave the product (0.48g, 24.3%).

[0058] 2. Preparation of catalyst

[0059] in the N 2 Add dehydrated cyclohexane (10mL), tripropylaluminum (10mL), (diph...

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Abstract

A catalyst for the self-polymerization of the ethene with three molecule to selectively generate 1-hexene is prepared from the Cr compound, the ligand containing P and/or N, aluminum alkylide, and promoter in the mole ratio of 1: (0.5-100): (50-5000): (0.5-100).

Description

technical field [0001] The invention relates to an ethylene trimerization catalyst composed of a chromium compound a, a ligand b containing P and / or N, an alkyl aluminum c and an accelerator d for ethylene trimerization and its application. technical background [0002] As we all know, 1-hexene and other linear α-olefins are important chemical products and intermediates, and are widely used in polyethylene comonomers, plasticizer alcohols, flavors and fragrances, synthetic lubricants and oil additives and other fields. The use of 1-hexene as a comonomer can significantly improve the density of polyethylene and improve its mechanical properties such as tear resistance and tensile strength. When used as a plasticizer alcohol, it can improve the low-temperature flexibility, processability and outdoor weather resistance of polyethylene products, especially for the manufacture of cables and wires, auto parts or decorative parts. [0003] EP 0608447A1 reports a chromium-based cat...

Claims

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Application Information

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IPC IPC(8): B01J31/24B01J31/14B01J31/02C07C2/36C07C2/34
Inventor 张宝军姜涛李建忠邢立华宁英男孙淑坤匡洞庭张德顺李玉龙陈谦黄付玲衣学飞张尚勇陈洪侠李建功袁宗辉张岩张婧元赵晶莹王斯晗王桂芝王路海马建英
Owner PETROCHINA CO LTD
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