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Method for production of trimethyl gallium at high efficiency and low cost

A trimethylgallium, low-cost technology, applied in the field of metal-organic compound preparation, can solve the problems of high production cost, high cost of raw materials, high toxicity of methyl iodide, etc., achieve high use value and reduce manufacturing cost

Inactive Publication Date: 2013-10-02
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The alkylaluminum method uses industrial trimethylaluminum and gallium trichloride for alkylation exchange reaction, which has high cost of raw materials and a large number of by-products, so the production cost is high; the alloy method generally uses gallium-magnesium alloy and methyl iodide reaction , although its cost is lower than the alkylaluminum method, the methyl iodide used in the reaction is more expensive, its production cost is higher, and its methyl iodide is more toxic

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a reaction kettle filled with nitrogen, put 22Kg of gallium-magnesium alloy, add 200Kg of methyl tetrahydrofuran, heat to above 30°C under stirring conditions, add iodomethane (CH 3 I) 0.5Kg, the reaction is initiated, the reaction temperature will rise, and at this time, monochloromethane (CH 3 Cl) to maintain the reaction, the reaction rate is controlled by adjusting the rate of introducing monochloromethane, after the reaction is completed, continue to reflux for 4 hours, then distill the solvent, and obtain The complex of trimethylgallium and ether, the complex of trimethylgallium and ether is transferred to the disassembly kettle, and gradually added to 75Kg tri-n-butylamine under stirring conditions, after the dropwise addition is completed, turn on the heating to make it reflux and After maintaining reflux for 2 hours, distill off methyl tetrahydrofuran, then remove low-boiling impurities under reduced pressure (vacuum degree between 1 and 100mmHg), and then h...

Embodiment 2

[0022] In a reaction kettle filled with nitrogen, put 22Kg of gallium-magnesium alloy, add 160Kg of methyl tetrahydrofuran, heat to above 30°C under stirring conditions, add iodomethane (CH 3 I) 0.5Kg, the reaction is initiated, the reaction temperature will rise, and at this time, monochloromethane (CH 3 Cl) to maintain the reaction, the reaction rate is controlled by adjusting the rate of introducing monochloromethane, after the reaction is completed, continue to reflux for 4 hours, then distill the solvent, and obtain The complex of trimethylgallium and ether, the complex of trimethylgallium and ether is transferred to the solution kettle, gradually added to 75Kg tri-n-octylamine under stirring conditions, after the dropwise addition is completed, turn on the heating to make it reflux and After maintaining reflux for 2 hours, distill off methyl tetrahydrofuran, then remove low-boiling impurities under reduced pressure (vacuum degree between 1 and 100mmHg), and then heat up ...

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Abstract

The invention relates to a method for production of trimethyl gallium at high efficiency and low cost. The method includes: adding a gallium-magnesium alloy into a reaction kettle filled with an inert gas, in the presence of an ether solvent, conducting heating to 30-80DEG C under a stirring condition, adding an initiator, initiating a reaction, then introducing methane chloride continuously till the end of the reaction, controlling the reaction rate by controlling the introduction speed of the methane chloride, evaporating the solvent after the end of the reaction, carrying out distillation under a pressure reduction condition to obtain a complex of trimethyl gallium and ether, adding the complex into high boiling point organic amine N(R')3, conducting distillation to remove the ether solvent, then further removing ether and low boiling point impurities under a reduced pressure, finally performing decomplexation to obtain an oxygen-free trimethyl gallium crude product, and rectifying the trimethyl gallium crude product so as to obtain high purity trimethyl gallium. By employing the methane chloride gas and the gallium-magnesium alloy to react to prepare trimethyl gallium, the reaction conversion rate reaches over 85%. Due to the low price of methane chloride, the production cost of trimethyl gallium can be greatly reduced.

Description

technical field [0001] The invention relates to a method for preparing trimethylgallium, in particular to a method for producing trimethylgallium with high efficiency and low cost, and belongs to the technical field of metal organic compound preparation. Background technique [0002] Metal-organic compounds such as high-purity trimethylgallium are the most important raw materials for growing optoelectronic materials in the process of metal-organic chemical vapor deposition (MO CVD) and chemical beam epitaxy (CBE), and are currently the most used raw materials. They are widely used in the growth of indium Gallium arsenide nitrogen (InGaAsN), indium gallium arsenide (InGaAs), indium gallium phosphide (InGaP) and other compound semiconductor thin film materials. [0003] There are many preparation methods for trimethylgallium, and the common methods are aluminum alkyl method and alloy method. The alkylaluminum method uses industrial trimethylaluminum and gallium trichloride fo...

Claims

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Application Information

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IPC IPC(8): C07F5/00
Inventor 孙祥祯许从应张德来潘兴华
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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