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Preparation method of trimethylaluminum

A technology of trimethylaluminum and methylaluminum chloride, applied in the field of metal organic chemistry, can solve problems such as difficulty, low reaction yield, multi-processing of by-products, etc., and achieves increased reaction rate, high product purity, and reaction yield. high effect

Active Publication Date: 2021-03-26
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The application provides a method for preparing trimethylaluminum to solve the problems of low reaction rate, low reaction yield, harsh experimental conditions, many by-products and difficult handling in the preparation of trimethylaluminum in the prior art

Method used

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Examples

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preparation example Construction

[0026] The embodiment of the present application provides a method for preparing trimethylaluminum, comprising the steps of: in the presence of a catalyst and a solvent, methylaluminum dichloride or sesquimethylaluminum chloride or dimethylaluminum chloride and metal M React with the system of methyl chloride to generate the chloride of trimethylaluminum and metal M; wherein, the catalyst is selected from metals or ions whose electrochemical sequence is arranged after metal aluminum; metal M is selected from alkali metals, alkaline earth metals or combinations thereof .

[0027] In the presence of catalyst and solvent, methylaluminum dichloride reacts with metal M and methyl chloride according to the following chemical reaction equation 1:

[0028] CH 3 AlCl 2 +M+CH 3 Cl→(CH 3 ) 3 Al+MCl x (1);

[0029] Wherein, when the metal M is an alkali metal, the value of x is 1, and when the metal M is an alkaline earth metal, the value of x is 2.

[0030] In the presence of a ...

Embodiment 1

[0081] Under a nitrogen atmosphere, add 11.3 g of commercially available methyl aluminum dichloride, 40 ml of n-hexadecane and 0.01 g of gold powder into a glass reactor, the weight ratio of gold powder to aluminum in methyl aluminum dichloride is 0.0037. Start stirring, keep the temperature in the glass reactor at 100°C, add molten metal sodium dropwise to the glass reactor (the heating temperature for melting metal sodium is 130°C), after adding 1g dropwise, start to feed in methyl chloride, continue Add molten metal sodium dropwise while maintaining ventilation, adjust the rate of methyl chloride through the gas flow meter equipped at the tail of the experimental device to ensure that no gas is discharged from the tail, keep the pressure in the glass reactor at 110-115 kPa, until 9.2 g of metal sodium is completely After the dropwise addition was completed, the stirring was continued for about 2.2 h until the methyl chloride was no longer absorbed, the aeration was stopped,...

Embodiment 2

[0084] Under a nitrogen atmosphere, 20.5 g of commercially available sesquimethylaluminum chloride, 40 ml of n-hexadecane and 0.1 g of silver powder were added to a glass reactor. The weight ratio was 0.019. Start stirring, keep the temperature in the glass reactor at 100°C, add molten sodium metal (the heating temperature for melting the sodium metal is 130°C) in batches into the glass reactor, add 4g and start to feed in methyl chloride, continue to drop Add molten metal sodium while maintaining ventilation, adjust the rate of methyl chloride through the gas flow meter at the tail of the experimental device to ensure that no gas is discharged from the tail, and keep the pressure in the glass reactor at 110-115 kPa until all 13.8 g of metal sodium drops After the addition was complete, the stirring was continued for about 3.1 h until the methyl chloride was no longer absorbed, the aeration was stopped, and the reaction system was lowered to room temperature.

[0085] Install...

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Abstract

The invention provides a preparation method of trimethylaluminum, which comprises the following steps: in the presence of a catalyst and a solvent, reacting methyl aluminum dichloride or sesquimethylaluminum chloride or dimethylaluminum chloride with a system of metal M and chloromethane to generate trimethylaluminum and a chloride of metal M; wherein the catalyst is selected from metal or ions thereof which are arranged behind metal aluminum in an electrochemical sequence; the metal M is selected from alkali metals, alkaline earth metals, or combinations thereof. The catalyst can significantly increase the reaction rate, so that the reaction can be carried out under very simple experimental conditions such as near normal pressure, the reaction yield and the product purity are higher, no by-product metal aluminum or unreacted alkali metal or alkaline earth metal is contained in the product, and the product is more convenient to treat.

Description

technical field [0001] The present application relates to the field of organometallic chemistry, in particular to a method for preparing trimethylaluminum. Background technique [0002] Trimethylaluminum is a very important chemical raw material. The applications of trimethylaluminum include: (1) In the field of organic catalysis, trimethylaluminum reacts with water to form highly active methylalumoxane, while methylaluminum Oxane is one of the most important cocatalysts in the metallocene catalytic system; (2) In the field of organic synthesis, trimethylaluminum and ethylene undergo oligomerization to form higher carbon alkylaluminum, which can be formed after oxidation and hydrolysis Straight-chain higher primary alcohols; trimethylaluminum can also be used to prepare other metal organic compounds, such as the reaction of trimethylaluminum and tin chloride to prepare methyltin; (3) in the field of polymer chemical industry, trimethyl The catalytic system formed by aluminu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06
CPCC07F5/062Y02P20/52C07F5/064B01J23/18B01J23/50B01J23/52B01J23/72B01J23/75B01J23/755
Inventor 杨敏杨雪孙祥祯
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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