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Preparation method of alkylaluminoxane 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: 2013-10-16
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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  • Preparation method of alkylaluminoxane solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under a nitrogen atmosphere, 100 milliliters of toluene was added to a 500 milliliter three-necked round-bottomed 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 120 milliliters of 3 mol / liter trimethylaluminum toluene solution and 24 ml 3 mol / liter triisobutylaluminum toluene solution were mixed at room temperature, added dropwise to the flask for 1 hour, the reaction temperature was maintained at -10°C, and then continued to stir for 2 hour; add 15 milliliters of 2 mol / liter of diethylaluminum chloride in toluene, add dropwise within half an hour, and continue to stir for 1 hour. The solid material was removed by filtration to give a clear solution of the alkylaluminoxane in toluene.

Embodiment 2

[0022] 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 150 milliliters of 3 mol / liter trimethylaluminum toluene solution and 30 ml 3 mol / liter triisobutylaluminum toluene solution were mixed at room temperature, added dropwise to the flask for 2 hours, the reaction temperature was maintained at -15°C, and then continued to stir for 3 hours , and then add 12.5 milliliters of 2 mol / liter of a toluene solution of diethylaluminum chloride, the addition is completed dropwise within half an hour, and the stirring is continued for 1 hour. The solid material was removed by filtration to give a clear solution of the alkylaluminoxane in toluene.

Embodiment 3

[0024] Under a nitrogen atmosphere, 100 milliliters of toluene was added into a 500 milliliter three-necked round-bottomed flask containing 21.7 grams of aluminum sulfate octadecahydrate (about 0.586 moles of water) and 0.75 grams (about 0.031 moles) of anhydrous lithium hydroxide, and then 150 Mix a milliliter 3 mol / liter trimethylaluminum toluene solution and 30 milliliter 3 mol / liter triisobutylaluminum toluene solution at room temperature, add dropwise to the flask for 2 hours, keep the reaction temperature at -20°C, and then continue to stir 2 hours; 15.0 ml of 2 mol / liter toluene solution of diethylaluminum chloride was added, the addition was completed 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 the alkylaluminoxane in toluene.

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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 cocatalyst alkyl aluminoxane solution. technical background [0002] Alkyl aluminoxane can be used as a cocatalyst for metallocene and late transition metal olefin polymerization, and methyl aluminoxane (MAO) is usually used as a cocatalyst for olefin polymerization in industry. Although methylaluminoxane has good catalytic activity, it is easy to produce gel (US4404344, US4665208, US4924018, US5087713, US5041585, US5003095, etc.) due to its poor solubility in solution, and the production cost is relatively high. limit its industrial application. [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 alkylalumoxanes or modified alkylalumoxanes prepared by these patented...

Claims

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Application Information

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Patent Type & Authority Patents(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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