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Olefin polymerization catalyst and preparation and application thereof

A technology for olefin polymerization and catalysts, applied in the field of catalysts, can solve problems such as difficult separation and poor shape of catalyst particles, and achieve the effects of simple preparation method, good particle shape, and less environmental pollution

Active Publication Date: 2010-11-10
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In patents CN 1532211A, CN 1140722A, and CN1552743, hexane is added once as a precipitation aid during catalyst preparation, which is conducive to the precipitation of the catalyst into particles, but the separation is difficult and the shape of the catalyst particles is not good

Method used

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  • Olefin polymerization catalyst and preparation and application thereof

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Experimental program
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Effect test

Embodiment 1

[0033] 1) Preparation of the main catalyst: In the reactor fully replaced by nitrogen, 2 g of magnesium dichloride, 3.5 ml of epichlorohydrin, 5.5 ml of tributyl phosphate, 75 ml of toluene, 15 ml of hexane, and 3.2 ml of ethanol were added successively, and the mixture was stirred. The temperature was raised to 70°C, after the solid was completely dissolved to form a homogeneous solution, the temperature was kept constant for 1h; then the temperature was lowered to -25°C, 58ml of titanium tetrachloride and 3.5ml of diethoxyisopropoxytert-butoxysilane were added dropwise, and the reaction was carried out for 1h. Then, the temperature was kept at -10 °C for 1 h, 0 °C for 1 h, and 20 °C for 1 h, 15 ml of hexane was added, the temperature was raised to a constant temperature of 60 °C, 10 ml of hexane was added, the reaction was carried out for 2 h, the stirring was stopped, the suspension was allowed to stand, and the layers were separated. The supernatant liquid was removed by su...

Embodiment 2

[0037] 1) Preparation of the main catalyst: In the reactor fully replaced by nitrogen, 5 g of magnesium dichloride, 7.5 ml of epichlorohydrin, 10.5 ml of tributyl phosphate, 150 ml of toluene, 10 ml of hexane, and 6.2 ml of ethanol were added successively, and the mixture was stirred. The temperature was raised to 60°C, after the solid was completely dissolved to form a homogeneous solution, the temperature was kept constant for 1 hour; then the temperature was lowered to -25°C, and 40ml of titanium tetrachloride was added dropwise. , add 10ml of hexane, react for 1h, heat up to a constant temperature of 70°C, 10ml of hexane, react for 2h, stop stirring, let the suspension stand, layer, remove the supernatant, wash twice with toluene and twice with hexane , blown dry with nitrogen to obtain the main catalyst component with good fluidity and narrow particle size distribution;

[0038] 2) Ethylene copolymerization: After the 0.5-liter stainless steel autoclave was fully replaced...

Embodiment 3

[0041] 1) Preparation of main catalyst: in the reactor fully replaced by nitrogen, add magnesium dichloride 5g, epichlorohydrin 5ml, tributyl phosphate 10.5ml, toluene 75ml, hexane 15ml successively, and heat up to 60 ℃ under stirring, After the solid was completely dissolved to form a homogeneous solution, the temperature was kept at a constant temperature for 1h; then the temperature was lowered to -25°C, 50ml of titanium tetrachloride was added dropwise, 5g of triethoxy-tert-butoxysilane was added after the dropwise addition, and after the reaction for 1h, the temperature was lowered to -10 ℃ constant temperature for 1h, 0℃ constant temperature for 1h, 0℃ constant temperature for 1h, add 15ml hexane, heat to 50 ℃ constant, add 20ml hexane, warm reaction for 2h, stop stirring, let the suspension stand, stratify, remove the supernatant , washed twice with toluene, twice with hexane, and dried with nitrogen to obtain the main catalyst component with good fluidity and narrow par...

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Abstract

The invention relates to an olefin polymerization catalyst and preparation and application thereof. A main catalyst consists of a carrier, a transition metal halide, an organic alcohol compound and an organosiloxane compound, wherein the molar ratio of the carrier to the transition metal halide to the organic alcohol compound to the organosiloxane compound is 1:(0.01-20):(0.1-6):(0.01-5); and the molar ratio of the transition metal halides in an assistant catalyst and the main catalyst is (30-500):1. In the preparation process, an assistant precipitation agent is added, wherein the assistant precipitation agent is alkane with the carbon atom number of 5 to 20 or cyclane with the carbon atom number of 5 to 20; and the mass ratio of the assistant precipitation agent to the carrier is (5-100):1. The olefin polymerization catalyst has the advantages of suitability for slurry process, gas-phase polymerization technology or combined polymerization technology, high catalyst activity, simple preparation method, low equipment requirement and less environmental pollution.

Description

technical field [0001] The present invention relates to a catalyst for ethylene polymerization or copolymerization and its preparation and application. Background technique [0002] Olefin polymerization catalysts are the core of polyolefin polymerization technology. From the perspective of the development of olefin polymerization catalysts, there are two main aspects: (1) the development of polyolefin resin catalysts that can prepare special or better performance, such as metallocene catalysts (2) For the production of general-purpose polyolefin resins, on the basis of further improving catalyst performance, simplify the catalyst preparation process, reduce catalyst costs, and develop environmentally friendly technologies to improve efficiency ,Increase competitiveness. Before the 1980s, the focus of polyethylene catalyst research was on the pursuit of catalyst efficiency. After nearly 30 years of hard work, the catalytic efficiency of polyethylene catalysts has been impro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F210/16C08F210/02C08F4/646C08F4/658C08F4/654C08F4/656
Inventor 义建军黄启谷李志飞卢晓英郑宏涛汪红丽陈商涛
Owner PETROCHINA CO LTD
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