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Method for preparing silica gel supported titanium-magnesium catalyst

A technology of catalyst and silica gel, which is applied in the field of preparation of high-activity silica gel-supported titanium-magnesium catalysts, which can solve the problems of increased specific surface area, reduced performance, and reduced pore size.

Active Publication Date: 2009-11-11
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if only the specific surface area of ​​silica gel is increased, although the activity of the catalyst is improved when it is used for olefin polymerization, due to the increase of the specific surface area of ​​silica gel, its pore size will inevitably decrease, and other performances will be significantly reduced, such as hydrogen adjustment. Sensitivity, copolymerization properties of ethylene and other α-olefins, etc., the relevant content has been disclosed in US Patent US3225023

Method used

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  • Method for preparing silica gel supported titanium-magnesium catalyst
  • Method for preparing silica gel supported titanium-magnesium catalyst
  • Method for preparing silica gel supported titanium-magnesium catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of catalyst components

[0019] (1) Weigh about 20g of spherical silica gel (produced by Grace Company in the United States, with an average particle size of 24μm and a specific surface area of ​​570m 2 / g), activated in a gas-phase fluidized bed activator at 600°C for 4 hours.

[0020] (2) In a reaction flask with a stirrer under nitrogen protection, add 100 mL of isopentane, 10 g of silica gel after thermal activation treatment in step (1) and 5.6 mL of AlEt with a concentration of 1 mmol / mL 3 Add the hexane solution, react at 20-30°C for half an hour, then slowly add 0.2mL dimethyldichlorosilane and 0.3mL tetrachlorofuran dropwise, and react for half an hour after the addition, then purge and dry it with high-purity nitrogen to become a fluid sexual powder.

[0021] (3) In another reaction flask with a stirrer, add 1.74g MgCl 2 and 0.64mL TiCl 4 and 174mL of tetrahydrofuran, heated and refluxed and stirred for 5 hours to obtain the catalyst mother liq...

Embodiment 2

[0028] Preparation of catalyst components

[0029] (1) Weigh about 20g of spherical silica gel (produced by Grace Company in the United States, with an average particle size of 24μm and a specific surface area of ​​570m 2 / g), activated at 600°C for 4 hours in a gas-phase fluidized bed activator.

[0030] (2) In a reaction flask with a stirrer under nitrogen protection, add 100 mL of isopentane, 10 g of silica gel after thermal activation treatment in step (1) and 5.6 mL of AlEt with a concentration of 1 mmol / mL 3 Add the hexane solution, react at 20-30°C for half an hour, then slowly add 0.2 mL of trimethylchlorosilane and 0.3 mL of tetrachlorofuran, blow and dry with high-purity nitrogen to form a fluid powder.

[0031] (3) In another reaction flask with a stirrer, add 1.74g MgCl 2 and 0.64mL TiCl 4 and 174mL of tetrahydrofuran, heated and refluxed and stirred for 5 hours to obtain the catalyst mother liquor.

[0032] (4) Mix the modified silica gel in step (2) with the ...

Embodiment 3

[0038] Preparation of catalyst components

[0039] (1) Weigh about 20g of spherical silica gel (produced by Grace Company in the United States, with an average particle size of 24μm and a specific surface area of ​​570m 2 / g), activated in a gas-phase fluidized bed activator at 600°C for 4 hours.

[0040] (2) In a reaction flask with a stirrer under nitrogen protection, add 100 mL of isopentane, 10 g of silica gel after thermal activation treatment in step (1) and 5.6 mL of AlEt with a concentration of 1 mmol / mL 3 Add the hexane solution, react at 20-30°C for half an hour, then slowly add 0.2mL methyltrichlorosilane and 0.3mL tetrachlorofuran dropwise, react for half an hour after the addition, and purge and dry with high-purity nitrogen to become fluid powder.

[0041] (3) In another reaction flask with a stirrer, add 1.74g MgCl 2 and 0.64mL TiCl 4 and 174mL of tetrahydrofuran, heated and refluxed and stirred for 5 hours to obtain the catalyst mother liquor.

[0042] (4)...

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Abstract

The invention relates to a method for preparing a silica gel supported titanium-magnesium catalyst, which is to treat a silica gel carrier by the steps of: placing silicon dioxide into a gas phase fluidized bed activator, taking high-purity nitrogen as carrier gas, increasing the temperature to between 200 and 800 DEG C, and performing temperature programmed dehydration for 4 to 10 hours; adding an alkane solvent into the dehydrated silicon dioxide, adding an alkyl metal compound, and evaporating the alkane solvent, wherein the weight ratio of Al to Si is equal to 0.05-0.1:1; adding the alkane solvent, at least one halogen-containing silane compound and at least one electron donor compound modifier containing halogen atoms into the silicon dioxide which is subjected to the surface treatment, and heating to evaporate the alkane solvent; and supporting a reaction product of a titanium compound, a magnesium compound and an electron donor on treated silica gel, and taking alkyl aluminum as a cocatalyst for ethylene polymerization on a gas phase fluidized bed. The method has the advantages of high polymerization activity, high bulk density of polymerization products, less fine powder and the like, and can produce high-quality polyethylene resins.

Description

technical field [0001] The invention relates to a preparation method of a highly active silica gel supported titanium-magnesium catalyst for ethylene polymerization or copolymerization. Background technique [0002] At present, the titanium-based Ziegler-Natta catalyst is the main catalyst for the production of polyolefins, and the linear low-density polyethylene film resin produced by this catalyst has good processability and mechanical properties. The catalysts used in the production of low-density polyethylene products by the gas phase polyethylene process are basically titanium / magnesium system Ziegler-Natta catalysts, such as the M-1 catalyst of the UCC company in the United States. The catalyst is a heterogeneous catalyst, which can improve the reactivity and other properties of the catalyst by loading the catalyst matrix and other additives, such as electron donors, on one or more inert, granular carriers. Microspherical silica gel (average particle size 10-100 μm) h...

Claims

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Application Information

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IPC IPC(8): C08F4/646C08F4/02C08F10/02
CPCY02P20/52
Inventor 姜涛吴林美邹恩广宁英男何书艳罗明检赵成才张丽郎笑梅张明辉李洪兴付义赵增辉高宇新张丽洋王立娟李红杨国兴刘君涛
Owner PETROCHINA CO LTD
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