Preparation method of trimethylaluminium

A technology of trimethylaluminum and trimethylaluminum ether, which is applied in the field of high-purity metal organic compound preparation, can solve the problems of difficult recovery of reaction by-products, low yield of trimethylaluminum, etc., and simplifies processes, equipment, and reactions. Ease of process, improved yield and purity

Inactive Publication Date: 2015-12-23
JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing trimethylaluminum in order to overcome the defects of low trimethylaluminum yield and difficult recovery of reaction by-products in the prior art

Method used

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Examples

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preparation example Construction

[0014] The invention provides a kind of preparation method of trimethylaluminum, the method comprises:

[0015] (1) In the presence of an ether solvent and an inert atmosphere, the magnesium aluminum alloy is contacted with a haloalkane to obtain a trimethylaluminum ether complex;

[0016] (2) contacting the trimethylaluminum ether complex with high-boiling amines and / or phosphine compounds to obtain trimethylaluminum amine complexes and / or trimethylaluminum phosphine complexes;

[0017] (3) Decomposing the complex obtained in step (2).

[0018] According to the method of the present invention, wherein, in step (1), the haloalkane can be various haloalkane in the art, preferably methyl iodide and / or methyl bromide, more preferably methyl iodide, so as to further increase the yield of trimethylaluminum rate, and the reaction by-products are easier to recover.

[0019] According to the method of the present invention, wherein, in step (1), the ether solvent can be various conv...

Embodiment 1

[0038] This example is used to illustrate the preparation method of trimethylaluminum of the present invention.

[0039] (1) Add 570g of magnesium-aluminum alloy Al to the reactor filled with nitrogen gas x Mg y (x=0.53, y=0.47, x, y are mass fraction), 4000g2-methyltetrahydrofuran, in the 2-methyltetrahydrofuran containing magnesium aluminum alloy, slowly add 4260g methyl iodide dropwise under stirring condition (dropping speed is 3ml / min), control the reaction temperature to 40°C, and when the temperature of the reaction solution no longer rises, it means that the contact reaction has reached the end point (reaction time is 6h), and then continue to heat up to 90°C to distill 2-methyltetrahydrofuran, in 0.01MPa, 90°C to distill trimethylaluminum ether complexes;

[0040] (2) Transfer the trimethylaluminum ether complex obtained from the above distillation to a disassembly kettle containing 2623g of triphenylphosphine, react at 90°C for 2h, and then carry out the reaction s...

Embodiment 2

[0043] This example is used to illustrate the preparation method of trimethylaluminum of the present invention.

[0044] (1) Add 1000g of magnesium-aluminum alloy Al to a reactor filled with nitrogen gas x Mgy (x=0.59, y=0.41, x, y are mass fractions), 5000g2-methyltetrahydrofuran, slowly add 8520g methyl iodide dropwise in the 2-methyltetrahydrofuran containing magnesium aluminum alloy under stirring condition (dropping speed is 4ml / min), control the reaction temperature to be 50°C, and when the temperature of the reaction solution no longer rises, it means that the contact reaction has reached the end point (reaction time is 4h), and then continue to heat up to 90°C to distill 2-methyltetrahydrofuran. 0.005MPa, 90°C to distill trimethylaluminum ether complexes;

[0045] (2) Transfer the trimethylaluminum ether complex obtained from the above distillation to a disassembly kettle containing 5246g of triphenylphosphine, react at 100°C for 2h, and then carry out the reaction so...

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Abstract

The invention relates to a preparation method of trimethylaluminium. The method comprises steps as follows: (1) magnalium and haloalkane have a contact reaction in the presence of an ether solvent and in the inert atmosphere to produce a trimethylaluminium ether complex; (2) the trimethylaluminium ether complex and an amine and/or phosphine compound with the high boiling point have a contact reaction to produce a trimethylaluminium amine complex and/or a trimethylaluminium phosphine complex; (3) the complexes obtained in Step (2) are decomposed. With the adoption of the preparation method, the yield and the purity of the trimethylaluminium can be significantly increased, the yield of the trimethylaluminium can be higher than 80%, the purity can be 99.9999%, besides, a reaction kettle used in the method can be used as an evaporation kettle, the technology and equipment are simplified, the reaction process is easy to control, the prepared product can be separated from raw materials and byproducts more easily, the method is very applicable to industrial production, in addition, the byproducts can be used for synthesizing aluminum sulfate, and almost no waste is produced.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-purity metal-organic compounds, and in particular relates to a method for preparing trimethylaluminum. Background technique [0002] High-purity trimethylaluminum belongs to high-purity metal-organic compounds. It is a key supporting raw material for compound semiconductor thin film materials prepared by advanced metal-organic chemical vapor deposition (MOCVD) technology or atomic layer deposition thin film technology (ALD). It is widely used in LED equipment, new generation solar cells, phase change memory, semiconductor lasers, infrared detectors and supercomputers. [0003] At present, the preparation of trimethylaluminum has been studied to a certain extent, and the common methods are the reduction method of magnesium aluminum alloy, the synthesis method of alkyl aluminum and haloalkane, etc. The magnesium-aluminum alloy reduction method generally adopts the reaction of magnesium-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06
Inventor 陈飞彪廖维林谢贤清邱曾烨马玉峰吴伟
Owner JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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