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A kind of preparation method of alkyl aluminoxane solution

A technology of alkylaluminoxane and alkylaluminum is applied in the field of preparation of metallocene, late transition metal cocatalyst alkylaluminoxane solution, which can solve the problem of lack of thermodynamic stability, reduced cocatalyst activity, hindering commercial application, etc. problems, to achieve the effect of facilitating storage and transportation, reducing losses, and improving catalytic activity

Active Publication Date: 2011-12-21
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The alkylalumoxanes or modified alkylalumoxanes prepared by these patented methods have improved the solubility of alkylalumoxanes and reduced production costs to varying degrees, but at the same time some new problems have emerged , such as reduced co-catalyst activity or the need for considerable aluminum loading, lack of thermodynamic stability, etc.
Due to these drawbacks, their commercial applications are hindered

Method used

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  • A kind of preparation method of alkyl aluminoxane solution

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Embodiment 1

[0020] In a nitrogen atmosphere, 100 ml of toluene was added to a 500 ml three-neck round bottom flask containing 23.7 g of copper sulfate pentahydrate (about 0.474 moles of water) and 0.84 g (about 0.035 moles) of anhydrous lithium hydroxide, and then 120 ml of Mix 3 mol / L of trimethylaluminum toluene solution and 24 ml of 3 mol / L of triisobutylaluminum toluene solution at room temperature, add dropwise to the flask for 1 hour, keep the reaction temperature at -10°C, and continue to stir 2 Hours; add 15 ml of a 2 mol / L toluene solution of diethyl aluminum chloride, dropwise addition is completed within half an hour, and continue to stir for 1 hour. The solid matter was removed by filtration to obtain a clear alkylaluminoxane toluene solution.

Embodiment 2

[0022] Under a nitrogen atmosphere, 100 ml of toluene was added to a 500 ml three-necked round bottom flask containing 18.6 g of magnesium chloride hexahydrate (about 0.542 moles of water) and 0.50 g (about 0.021 moles) of anhydrous lithium hydroxide, and then 150 ml of 3 The mol / L trimethylaluminum toluene solution and 30 ml of 3 mol / L triisobutylaluminum toluene solution were mixed at room temperature, and added dropwise to the flask for 2 hours. The reaction temperature was kept at -15°C, and then the stirring was continued for 3 hours , And then add 12.5 ml of a 2 mol / L toluene solution of diethyl aluminum chloride, the addition is completed within half an hour, and the stirring is continued for 1 hour. The solid matter was removed by filtration to obtain a clear alkylaluminoxane toluene solution.

Embodiment 3

[0024] Under a nitrogen atmosphere, 100 ml of toluene was added to a 500 ml three-neck round bottom flask containing 21.7 g of aluminum sulfate octahydrate (about 0.586 moles of water) and 0.75 g (about 0.031 moles) of anhydrous lithium hydroxide, and then 150 Mix 3 ml of 3 mol / L trimethylaluminum toluene solution and 30 ml of 3 mol / L triisobutylaluminum toluene solution at room temperature, add dropwise to the flask for 2 hours, keep the reaction temperature at -20°C, and continue stirring 2 hours; 15.0 ml of a toluene solution of 2 mol / L diethyl aluminum chloride is added, the addition is completed within half an hour, and the stirring is continued for 1 hour. The solid matter was removed by filtration to obtain a clear alkylaluminoxane toluene solution.

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Abstract

The invention provides a preparation method of an alkylaluminoxane solution, comprising the following steps: (1) mixing crystalline hydrate and alkali metal or alkaline earth metal anhydrous hydroxide, adding an organic solvent and stirring; (2) adding two or more different alkyl aluminums into silted size formed in the step (1) to react at low temperature; and (3) adding halogenated alkyl aluminum and stirring, and filtering solid substances out after reaction to obtain the alkylaluminoxane solution. One of the alkyl aluminums is trimethyl aluminium, and the other alkyl aluminum is high-carbon alkyl aluminum which contains 2-10 carbon atoms and has relative low price. The method has low cost, the obtained product has good gel resistance, and the analysis promotion activity of the alkylaluminoxane solution can be maintained.

Description

Technical field [0001] The invention relates to a method for preparing a metallocene and late transition metal promoter alkylaluminoxane solution. technical background [0002] Alkyl aluminoxane can be used as a co-catalyst for the polymerization of metallocene and late transition metal olefins. In industry, methyl aluminoxane (MAO) is generally used as a co-catalyst for olefin polymerization. Although methylaluminoxane has better catalytic activity, it is easy to produce gel due to its poor solubility in solution (US4404344, US4665208, US4924018, US5087713, US5041585, US5003095, etc.), and the production cost is relatively high. Limits its application in industry. [0003] In order to improve the solubility of alkylaluminoxanes and reduce production costs, researchers have done a lot of work, such as US5324800, US4752597, US4980878, US5157008, US5041584, WO96102580, EP0277003, EP0277004, US6153157 and so on. The alkylaluminoxanes or modified alkylaluminoxanes prepared by these p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06C08F4/642C08F110/02
Inventor 王雄韦少义姚培洪朱博超徐人威吴江张鹏刘文霞任峰王海郝萍宫国平姜立刚张平生王丹丹韩晓昱
Owner PETROCHINA CO LTD
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