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Method for preparing anti-gelling methylaluminoxane solution

A technology of anti-gel methylalumoxane and gelatinous methylalumoxane, which is applied in the field of preparation of metallocene cocatalyst methylalumoxane solution, can solve the problems of reducing MAO content, poor fluidity of metallocene catalysts, and gelation. and other issues to achieve the effect of reducing the loss of MAO and facilitating storage and transportation

Active Publication Date: 2012-10-17
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although indirect hydration usually results in a clear MAO solution, the solution can still form a gel after 2-3 weeks of standing
[0004] The generation of gel in the MAO solution not only reduces the content of MAO in the solution, causing great economic losses, but also may lead to poor fluidity of the prepared metallocene catalyst, resulting in catalyst agglomeration
In addition, the production of gel is very unfavorable to the storage and transportation of MAO
Although US5157137 improved the post-treatment of the MAO prepared by the above reaction and improved its anti-gel performance, it did not consider improving the anti-gel performance of MAO from the reaction process of MAO

Method used

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  • Method for preparing anti-gelling methylaluminoxane solution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under a nitrogen atmosphere, 100 milliliters of toluene was added into a 500 milliliter three-necked round-bottomed flask containing 16.7 grams of aluminum sulfate octadecahydrate (about 0.451 moles of water) and 0.81 grams (about 0.034 moles) of anhydrous lithium hydroxide, and then 125 Milliliter 3 mol / liter of trimethylaluminum toluene solution was added dropwise to the flask in 1 hour, the reaction temperature was maintained at -20°C, and then continued to stir for 2 hours; The toluene solution was added dropwise within half an hour, and the stirring was continued for 1 hour. The solid material was removed by filtration to give a clear solution of MAO in toluene (designated 1A).

Embodiment 2

[0024] Under a nitrogen atmosphere, 100 milliliters of toluene was added to a 500 milliliter three-necked round bottom flask containing 23.7 grams of copper sulfate pentahydrate (about 0.474 moles of water) and 0.84 grams (about 0.035 moles) of anhydrous lithium hydroxide, and then 130 milliliters of Add 3 mol / liter of trimethylaluminum toluene solution dropwise to the flask for 1.5 hours, keep the reaction temperature at -10°C, and then continue to stir for 2 hours; add 23.5 ml of 2 mol / liter of diethylaluminum chloride in toluene The solution was added dropwise within half an hour, and stirring was continued for 1 hour. The solid material was removed by filtration to give a clear solution of MAO in toluene (designated 2A).

Embodiment 3

[0028] Under a nitrogen atmosphere, 100 milliliters of toluene was added into a 500 milliliter three-neck round bottom flask containing 18.6 grams of magnesium chloride hexahydrate (about 0.542 moles of water) and 0.50 grams (about 0.021 moles) of anhydrous lithium hydroxide, and then 164 milliliters of 3 mol / liter of trimethylaluminum toluene solution was added dropwise to the flask in 2 hours, the reaction temperature was maintained at -15°C, then continued to stir for 3 hours, and then 29.5 ml of 2 mol / liter of diethylaluminum chloride in toluene was added The solution was added dropwise within half an hour, and stirring was continued for 1 hour. The solid material was removed by filtration to give a clear solution of MAO in toluene (designated 3A).

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Abstract

The invention provides a method for preparing anti-gelling methylaluminoxane solution, which is characterized in that: trimethyl aluminum and crystalline hydrate are used as raw materials, alkali metal or alkaline earth metal anhydrous hydroxide and halogenated alkyl aluminum are added in the reaction process, and the obtained methylaluminoxane solution has good anti-gelling performance.

Description

technical field [0001] The invention relates to a method for preparing a metallocene cocatalyst methyl aluminoxane solution (MAO), in particular to a method for preparing an anti-gel methyl aluminoxane solution. technical background [0002] There are many synthesis methods of metallocene cocatalyst methylaluminoxane, which can be mainly divided into direct hydration method and indirect hydration method. The methylalumoxane organic solution prepared by the direct hydration method (US4924018, US5087713, US5041585, US5003095, etc.) often contains gel or small particles, and these small particles are also easy to gather to form a gel after standing still, even if the gel and small After particle filtration, the methylalumoxane solution gels again after two to three weeks. [0003] The indirect hydration method generally adopts the reaction of crystalline hydrate and trimethylaluminum. US4404344 prepares MAO by adding trimethylaluminum to a toluene solution of copper sulfate p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/06
Inventor 王雄韦少义朱博超王喆姜平张建纲宫国平张鹏任峰姜立刚郝萍王海张平生王丹丹刘文霞韩晓昱
Owner PETROCHINA CO LTD
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