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Preparation method of aluminium methide oxyalkane

A technology of methylaluminoxane and alkylaluminum, which is applied in the field of preparation of metallocene cocatalyst-methylaluminoxane, can solve problems such as complex process flow, achieve the effect of simplifying post-processing and solving safety problems

Inactive Publication Date: 2005-03-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its main disadvantage is that since the trimethylaluminum solution is gradually added to the suspension of crystal hydrate, most of the initially added trimethylaluminum is converted into Al(OH) by the relatively excess water in the system 3 , only when the concentration of free water in the system is reduced to a certain extent, Al(OH) 3 side effects are reduced to a minor level
Therefore, the technological process of this method is still quite complicated

Method used

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  • Preparation method of aluminium methide oxyalkane
  • Preparation method of aluminium methide oxyalkane

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Experimental program
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Effect test

Embodiment 1

[0020] After the reaction bottle is fully vacuum-nitrogen replaced, add 50ml2mol.L -1 Triethylaluminum (TEA) decane solution, start stirring, add 2gBiCl under inert protection 3 , slowly warming up to 120°C. After the methyl bromide gas is passed through distilled water at 30°C, the methyl bromide entrained with water vapor is passed into the reaction flask. When the number of moles of methyl bromide gas reaches 0.4 mol in total, stop feeding methyl bromide, and continue stirring until no gas is produced, then stop the reaction. The solid was filtered off, and the solvent was removed under reduced pressure to obtain 3.1 g of white methylaluminoxane solid. Calculated based on the moles of triethylaluminum fed, the yield of the target product, methylaluminoxane, is 53.5%.

[0021] 1.7 g of the above methylalumoxane with 0.05 g Cp 2 ZrCl 2 , At 60°C and 0.8Mpa, ethylene was polymerized for 1 hour to obtain 584 grams of polyethylene.

Embodiment 2

[0023] After the reaction bottle is fully vacuum-nitrogen replaced, add 50ml2mol.L -1 Triethylaluminum (TEA) decane solution, start stirring, add 2gBiCl under inert protection 3 , slowly warming up to 120°C. After the methyl bromide gas is passed through distilled water at 50°C, the methyl bromide entrained with water vapor is passed into the reaction flask. When the number of moles of methyl bromide gas reaches 0.45 mol in total, stop feeding methyl bromide, and continue stirring until no gas is generated, then stop the reaction. The solid was filtered off, and the solvent was removed under reduced pressure to obtain 3.5 g of white methylaluminoxane solid. Calculated based on the moles of triethylaluminum fed, the yield of the target product, methylaluminoxane, is 60.3%.

[0024] 1.7 g of the above methylalumoxane with 0.05 g Cp 2 ZrCl 2 , At 60°C and 0.8Mpa, ethylene was polymerized for 1 hour to obtain 651 grams of polyethylene.

Embodiment 3

[0026] After the reaction bottle is fully vacuum-nitrogen replaced, add 50ml2mol.L -1 Triethylaluminum (TEA) toluene solution, start stirring, add 2gBiCl under inert protection 3 , slowly warming up to 100°C. After the methyl bromide gas is passed through distilled water at 50°C, the methyl bromide entrained with water vapor is passed into the reaction flask. When the number of moles of methyl bromide gas reaches 0.5 mol in total, stop feeding methyl bromide, and continue stirring until no gas is generated, then stop the reaction. The solid was filtered off, and the solvent was removed under reduced pressure to obtain 2.9 g of white methylaluminoxane solid. Calculated based on the moles of triethylaluminum fed, the yield of the target product methylaluminoxane is 50%.

[0027] 1.7 g of the above methylalumoxane with 0.05 g Cp 2 ZrCl 2 , At 60°C and 0.8Mpa, ethylene was polymerized for 1 hour to obtain 604 grams of polyethylene.

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Abstract

A methyl aluminoxyane as the metallocene cocatalyst for polymerizing olefin is prepared through reaction between bromomethane carrying water vapor and high-grade alkylaluminium.

Description

technical field [0001] The invention relates to a preparation method of alkyl aluminoxane, in particular to a preparation method of metallocene cocatalyst-methyl aluminoxane. Background technique [0002] There are many synthesis methods of methylaluminoxane used as metallocene cocatalyst, which are basically summarized into two categories: direct water process and indirect water process. The yield of direct water process target product is higher, but the risk of production process is bigger, meanwhile, in order to solve the risk of production process, often need to design various special equipments, make the construction investment of industrial plant increase greatly (US4924018 , US4772736, US4937363, US4908463, US5087713, US5041585). [0003] The indirect water process generally uses the reaction of crystalline hydrate and trimethylaluminum. The synthesis methods reported in the existing literature are all the synthesis methods in which the crystalline hydrate and the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06
Inventor 韦少义朱博超吴江魏红朱雅杰张长军郝萍
Owner PETROCHINA CO LTD
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