Trimethylaluminium preparation method

A technology of trimethyl aluminum and aluminum-magnesium alloy powder, which is applied in chemical instruments and methods, organic chemistry, compounds containing elements of Group 3/13 of the periodic table, etc., can solve the problem of low reaction conversion efficiency, high raw material cost, Inflammable raw materials and other problems, to achieve the effect of being suitable for large-scale industrial production, safe reaction process, and cheap materials

Inactive Publication Date: 2015-07-15
HENAN CHENGMING PHOTOELECTRIC NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are many preparation methods for trimethylaluminum, but few methods can be applied to industrialization. The common method is to use industrial triethylaluminum and haloalkane for transalkylation reaction, but there are the following disadvantages: 1) The reaction conversion efficiency is not high , a large number of by-products are produced; 2) The cost of raw materials is high. As an industrialized preparation route, the price of triethylaluminum is relatively high, and the production cost is extremely high; 3) The raw material is flammable and has potential safety hazards. Triethylaluminum is very harmful to air and water vapor. Sensitive, spontaneous combustion in air, explosion in water, potential safety hazards in filling, transfer, reaction and other processes during use

Method used

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Effect test

Embodiment 1

[0017] A method for preparing trimethylaluminum, comprising the following steps: under nitrogen protection, adding aluminum-magnesium alloy powder and ethers to a reaction kettle, the molar ratio of the ethers to aluminum in the aluminum-magnesium alloy powder is 6:1, Add the alkyl halide dropwise under stirring conditions, and keep the ethers reflux during the addition of the alkyl halides; after the addition of the alkyl halides, continue to maintain the reflux of the ethers for 4.5 hours, then adjust the temperature of the reactor to 80 ° C and keep it for 2.5 hours, and the ether Then adjust the temperature of the reaction kettle to 65°C and keep it, and steam the complex of trimethylaluminum and ethers under a vacuum of 50mmHg; transfer the complex of trimethylaluminum and ethers to the solution In the preparation kettle, then add tri-n-octylamine, the molar ratio of tri-n-octylamine to aluminum in the aluminum-magnesium alloy powder is 1.2:1, heat and reflux under stirri...

Embodiment 2

[0020] A method for preparing trimethylaluminum, comprising the following steps: under nitrogen protection, adding aluminum-magnesium alloy powder and ethers to a reaction kettle, the molar ratio of the ethers to aluminum in the aluminum-magnesium alloy powder is 4:1, Add the alkyl halides dropwise under stirring conditions, and keep the ethers reflux during the addition of the alkyl halides; after the addition of the alkyl halides, continue to keep the ethers under reflux for 5 hours, then adjust the temperature of the reactor to 45°C and keep it for 4 hours, and the ether Then adjust the temperature of the reaction kettle to 45°C and keep it, and steam the complex of trimethylaluminum and ethers under a vacuum of 1mmHg; transfer the complex of trimethylaluminum and ethers to the solution Add tri-n-octylamine to the mixing tank, the molar ratio of tri-n-octylamine to aluminum in the aluminum-magnesium alloy powder is 1:1, heat and reflux under stirring conditions, and keep for...

Embodiment 3

[0023] A method for preparing trimethylaluminum, comprising the following steps: under nitrogen protection, adding aluminum-magnesium alloy powder and ethers to a reaction kettle, the molar ratio of the ethers to aluminum in the aluminum-magnesium alloy powder is 8:1, Add the alkyl halides dropwise under stirring conditions, and keep the ethers reflux during the addition of the alkyl halides; after the addition of the alkyl halides, continue to keep the ethers under reflux for 4 hours, then adjust the temperature of the reactor to 100°C and keep it for 1 hour, and the ether Then adjust the temperature of the reaction kettle to 70°C and keep it, and steam the complex of trimethylaluminum and ethers under a vacuum of 100mmHg; transfer the complex of trimethylaluminum and ethers to the solution Add tri-n-octylamine to the mixing tank, the molar ratio of tri-n-octylamine to aluminum in the aluminum-magnesium alloy powder is 1.3:1, heat and reflux under stirring conditions, and keep...

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Abstract

A trimethylaluminium preparation method includes the steps of adding aluminium-magnesium alloy powder and ethers into a reactor under the protection of inert gas, dropwise adding alkyl halide under the stirring condition, keeping ether backflow in the dropwise alkyl halide adding process, continuing to keep the ether backflow for 4 hours to 5 hours after alkyl halide is dropwise added, regulating the temperature of the reactor to 45 DEG C to 100 DEG C, keeping the temperature for 1 hour to 4 hours, evaporating the ethers, regulating the temperature of the reactor to 45 DEG C to 70 DEG C, keeping the temperature, evaporating the coordination compound of trimethylaluminium and the ethers under the vacuum condition, moving the coordination compound of the trimethylaluminium and the ethers to a deolation kettle, adding tri-n-octylamine, conducting heating and backflow under the stirring condition, keeping for 2 hours to 3 hours, regulating the temperature of the deolation kettle to 85 DEG C to 89 DEG C again, keeping the temperature for 8 hours to 10 hours under the vacuum degree of 1 mmHg to 50 mmHg, evaporating the ethers, raising the temperature of the deolation kettle to 90 DEG C to 160 DEG C, keeping the temperature for 30 hours to 35 hours under the vacuum condition, and evaporating the trimethylaluminium.

Description

technical field [0001] The invention belongs to the technical field of organometallic compound synthesis, and in particular relates to a method for preparing trimethylaluminum. Background technique [0002] Metal-organic compounds such as high-purity trimethylaluminum are the most important raw materials for growing optoelectronic materials in the process of metal-organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE), and are currently the most used raw materials. They are widely used in compound semiconductor thin films Material. Pure trimethylaluminum is liquid at room temperature. When it is used for MOCVD, it needs to be packaged in a steel cylinder, and then the temperature of the steel cylinder is controlled to make its vapor pressure reach a certain value. Trimethylaluminum in the gas phase under the gas-solid equilibrium state is brought into the MOCVD or CBE growth system. [0003] There are many preparation methods for trimethylaluminum, but f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06
CPCC07F5/062
Inventor 宁红锋
Owner HENAN CHENGMING PHOTOELECTRIC NEW MATERIAL CO LTD
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