A kind of method that adopts microreactor to prepare alkyl aluminoxane

An alkylaluminoxane and microreactor technology, which is applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, compounds containing elements of Group 3/13 of the periodic table, etc. The effect of reaction temperature and reaction process is safe and controllable

Active Publication Date: 2021-09-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problems of safety controllability and partial excessive hydrolysis in the existing preparation technology of alkyl aluminoxane, the present invention provides a continuous synthesis method of alkyl aluminoxane based on direct hydrolysis process and adopting micro-reactor technology, The method can realize effective microdispersion of water in an inert solvent, and effectively avoid the influence of potential solid by-products while realizing partial hydrolysis of alkylaluminum. The entire reaction process is efficient, safe and controllable. The microreactor includes a microdisperser And miniature continuous stirring reactor, described method comprises the steps:

Method used

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  • A kind of method that adopts microreactor to prepare alkyl aluminoxane
  • A kind of method that adopts microreactor to prepare alkyl aluminoxane
  • A kind of method that adopts microreactor to prepare alkyl aluminoxane

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Embodiment 1

[0034] Before starting the reaction, the microreactor system was vacuum-dried and replaced with nitrogen. Syringe pumps S1 and S2 transport toluene and distilled water at a flow rate of 8mL / min and 60μL / min respectively. After passing through the heat exchange section E1, the temperature of the stream drops to 5°C and enters the liquid-liquid microdisperser to realize the microdispersion of water in toluene. The dispersed particle size of water droplets is 10-100μm. Syringe pump S3 delivers the toluene solution of trimethylaluminum at a flow rate of 8mL / min, with a mass fraction of 5%, and controls the temperature of the stream to 0°C after passing through heat exchange section E2. The microdisperser M and micro continuous stirring reactor R1 were placed in an ice-water bath to control the temperature at 0°C. The dispersed emulsion of water and toluene is fed from the top of reactor R1, and reacts with the toluene solution of trimethylaluminum in the second stirred tank. The ...

Embodiment 2

[0038] In order to improve production capacity, the concentration of trimethylaluminum toluene solution was increased to 10wt%. When starting the reaction, the trimethylaluminum toluene solution and toluene stream were still delivered at 8mL / min, and distilled water was injected at 120μL / min. The molar ratio of aluminum was 0.7. Other reaction process, condition, device parameter are all the same as embodiment 1. The yield of methylaluminoxane at the end of the reaction was 69%.

Embodiment 3

[0040] 5wt% trimethylaluminum toluene solution was delivered to the reaction system at a flow rate of 8mL / min, distilled water was injected at 69μL / min, and dispersed with toluene stream, the flow rate was 8mL / min, and the molar ratio of water to trimethylaluminum was controlled as 0.8. Other reaction process, condition, device parameter are all the same as embodiment 1. At the end of the reaction, the yield of methylaluminoxane was 70.5%.

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Abstract

The invention discloses a method for preparing alkyl aluminoxane by using a microreactor. The continuous flow chemical reaction system includes a fluid delivery section, a microdisperser section, a microreactor section, and a collection and purification section. On the one hand, the dispersion size of water in the inert continuous phase is reduced through the microdisperser, the contact mode between the reactants is changed in the form of micro droplets, and it is fed into the continuous stirring reactor through multi-stage feeding to prevent excessive hydrolysis. Thereby reducing or avoiding the generation of solid by-products. On the other hand, the method uses a miniature continuous stirred reactor instead of a traditional microchannel reactor, reducing the risk of pipeline blockage. Aluminum alkyls and water react in a nearly equimolar ratio in a continuous stirred reactor to produce alkylaluminoxanes. The invention is simple and feasible, the reaction process is safe and controllable, the high-efficiency heat transfer and mass transfer characteristics ensure good heat removal and reaction performance, effectively reduce the excessive reaction and incomplete reaction, and the target product reaches a high yield and active.

Description

technical field [0001] The present invention relates to the preparation of alkyl aluminoxane, in particular to a method for continuously preparing alkyl aluminoxane through microreactor technology. Background technique [0002] Alkyl aluminoxane is an important cocatalyst in olefin polymerization catalysts, which assists metallocene catalysts or late transition metal catalysts to form catalytic active centers, and obtains homopolymerization and copolymerization materials with various special structures and properties. Alkyl aluminoxane is a low molecular weight oligomer obtained by partial hydrolysis of alkyl aluminum. This reaction is a fast and strong exothermic reaction. The reaction materials involved are flammable and explosive, and are extremely dangerous. The control and Synthesizers place extremely high demands. At present, the synthesis process of alkylaluminoxane is complex and the product is expensive. Therefore, the development of an efficient, safe and controll...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/06B01F13/00B01J4/00B01J19/00
CPCC07F5/068B01J19/0093B01J4/008B01F33/302
Inventor 张浩淼冯艺荣叶健王靖岱阳永荣黄正梁廖祖维蒋斌波孙婧元杨遥
Owner ZHEJIANG UNIV
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