Controllable preparation method of alkylaluminoxane

A technology of alkylaluminoxane and alkylaluminum, which is applied in the field of controllable preparation of alkylaluminoxane, can solve the problems of target product composition and performance influence, and achieves safe and controllable reaction process, flexible operation and simple method workable effect

Active Publication Date: 2022-06-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, from the perspective of improving the safety of the production process and the product yield, a key technical difficulty that still needs to be solved is how to achieve a high degree of water dispersion and prevent local overreaction due to uneven distribution of water concentration during the reaction process. Or the incomplete reaction will affect the composition and performance of the target product and other consequences

Method used

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  • Controllable preparation method of alkylaluminoxane
  • Controllable preparation method of alkylaluminoxane
  • Controllable preparation method of alkylaluminoxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A circular hole with a diameter of 1 cm was opened at the position where the side wall of the 250mL reaction kettle was level with the mechanical stirring paddle, and a stainless steel tube with a 45° upward inclination was connected with the kettle body. is 10 μm. The reaction kettle was equipped with a nitrogen inlet, a vent valve and a cooling jacket. Under nitrogen protection, 100 mL of trimethylaluminum toluene solution (10wt%) was added to the reaction kettle, and the temperature of the reaction kettle was controlled to be 0°C. A certain amount of distilled deionized water was put into the stainless steel tube to make [H 2 O] / [AlMe 3 ] The molar ratio is 0.7, the other end of the steel pipe is filled with nitrogen, and the pressure of nitrogen is adjusted to apply a driving force to the reaction water in the pipe, and the temperature of the reaction water in the stainless steel pipe is controlled to be 5 °C.

[0035] When starting the reaction, the trimethylalum...

Embodiment 2

[0038] The difference between this embodiment and Embodiment 1 is that the orifice is embedded in the sand core, and the diameter of the sand core is 2-4 μm.

[0039] Other reaction processes, conditions, and device parameters are the same as in Example 1. After the reaction was completed, the yield of methylaluminoxane was 65%.

Embodiment 3

[0041] Insert a stainless steel tube with an inner diameter of 1cm from the top of the 250mL reaction kettle. The end of the tube is close to the upper part of the stirring paddle, and a screen is fixed at the end of the tube as a support. A molecular sieve membrane is installed on the screen in the tube, with an average pore size of 0.5nm. The reaction kettle was equipped with a nitrogen inlet, a vent valve and a cooling jacket. Under nitrogen protection, 100 mL of trimethylaluminum toluene solution (10wt%) was added to the reaction kettle, and the temperature of the reaction kettle was controlled to be 5°C. A certain amount of distilled deionized water was put into the stainless steel tube to make [H 2 O] / [AlMe 3 ] The molar ratio is 0.7, the other end of the steel pipe is filled with nitrogen, and the driving force is applied to the reaction water in the pipe by adjusting the nitrogen pressure.

[0042] When starting the reaction, the trimethylaluminum solution was stirred...

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Abstract

The invention discloses a controllable preparation method of alkylaluminoxane, which comprises the following steps: step S1, finely dispersing the reaction water to below 10 microns through a dispersion release device; step S2, controlling the release of the dispersed reaction water process, input it into the reaction system to contact with the alkylaluminum solution to obtain the alkylaluminoxane solution. The method can realize sufficient dispersion of water in the reaction system, greatly reduces the possibility of excessive hydrolysis reaction, and the production process is safe and controllable.

Description

technical field [0001] The present invention relates to the preparation of polyolefin cocatalyst, in particular to a controllable preparation method of alkylaluminoxane. Background technique [0002] Alkyl aluminoxanes are an important class of cocatalysts for polyolefin catalysts. Among them, methylaluminoxane is the most important. It can be combined with metallocene catalysts or late transition metal catalysts to catalyze olefin polymerization or copolymerization to produce a series of high-end polyolefin materials with precisely adjustable microstructures and excellent properties. The development of the olefin industry plays a vital role. [0003] At present, the preparation methods of alkylaluminoxane mainly include two categories: hydrolysis method and non-hydrolysis method. [0004] The hydrolysis method is to generate alkylaluminoxane through the reaction of alkyl aluminum and water. According to the state of the reaction water, it can be divided into two categorie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/06C08F110/02C08F4/70
CPCC07F5/068C08F110/02C08F4/7042
Inventor 阳永荣叶健王靖岱蒋斌波孙婧元冯艺荣杨遥廖祖维黄正梁张浩淼
Owner ZHEJIANG UNIV
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