Trimethylaluminium preparation method

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...

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