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Method for industrially preparing trimethyl gallium

A technology of trimethyl gallium and methyl tetrahydrofuran, which is applied in the field of trimethyl gallium preparation, can solve the problems of filling and transfer safety hazards, low reaction conversion efficiency, and high price of trimethyl aluminum, and is suitable for large-scale industrialization. Production, easy to industrialize, easy to control effect

Active Publication Date: 2013-01-09
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are many preparation methods for trimethylgallium, but there are few methods that can be applied to industrialization. The common method is to use industrial trimethylaluminum and gallium trichloride to carry out the transalkylation reaction, but there are the following disadvantages: 1) reaction conversion The efficiency is not high, and a large number of by-products are produced; 2) the cost of raw materials is high, and as an industrialized preparation route, the price of trimethylaluminum is relatively high, while the price of gallium trichloride is more expensive, so the production cost is extremely high; 3) the raw materials are easy Combustible, there are safety hazards, trimethylaluminum is very sensitive to air and water vapor, it will spontaneously ignite when it encounters air, and explode when it encounters water.

Method used

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  • Method for industrially preparing trimethyl gallium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a reactor filled with nitrogen, put 580g of gallium-magnesium alloy into it, add 2100g of anhydrous ether, and gradually add methyl iodide (CH 3 I) 2050g, by controlling iodomethane (CH 3 1) The speed of addition controls the solvent reflux speed, after the reaction is completed, continue to keep reflux for 4 hours, then the solvent is steamed, and then under reduced pressure (vacuum degree is between 1~100mmgH) to obtain the mixture of trimethylgallium and ether The complex is finally decomposed (the decomposed temperature is between 70°C and 140° C.) to obtain 370 g of trimethylgallium, with a yield of 90% (calculated as metal gallium).

Embodiment 2

[0018] In a reactor filled with nitrogen, put 580g of gallium-magnesium alloy into it, add 1600g of anhydrous ether, and gradually add methyl iodide (CH 3 I) 2050g, by controlling iodomethane (CH 3 1) The speed of addition controls the solvent reflux speed, after the reaction is completed, continue to keep reflux for 4 hours, then the solvent is steamed, and then under reduced pressure (vacuum degree is between 1~100mmgH) to obtain the mixture of trimethylgallium and ether The complex was finally decomposed (the decomposed temperature was between 70 and 140° C.) to obtain 341 g of trimethylgallium, with a yield of 83% (calculated as metal gallium).

Embodiment 3

[0020] In a reactor filled with nitrogen, put 580g of gallium-magnesium alloy into it, add 2100g of anhydrous ether, and gradually add methyl iodide (CH 3 1) 1550g, by controlling iodomethane (CH 3 1) The speed of addition controls the solvent reflux speed, after the reaction is completed, continue to keep reflux for 4 hours, then the solvent is steamed, and then under reduced pressure (vacuum degree is between 1~100mmgH) to obtain the mixture of trimethylgallium and ether The complex was finally decomposed (the decomposed temperature was between 70°C and 140° C.) to obtain 325 g of trimethylgallium, with a yield of 79% (calculated as metal gallium).

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Abstract

The invention relates to a method for industrially preparing trimethyl gallium. The method is characterized by comprising the following steps: putting gallium-magnesium alloy materials into a reaction kettle filled with inert gases; adding alkyl halide step by step while stirring in the presence of ether solvents; controlling the return velocity of the solvents by controlling the dropwise adding velocity of alkyl halide; vaporizing the solvents after the reaction is finished; obtaining the compound of trimethyl gallium and ethers under the condition of reduced pressure; and finally decompounding the compound to obtain the trimethyl gallium. The process is simple and steady in reaction, easy to control, high in reaction yield and very safe in reaction process as the raw materials adopted in the reaction process do not contain materials liable to spontaneous combustion, thus being especially suitable for large-scale industrial production.

Description

[0001] Inventors (Sun Xiangzhen, Xu Xin, Pan Yi, Zhang Jinqi, Zhu Chunsheng, Chen Huabing, Ji Minkun, Sun Minglu) technical field [0002] The invention relates to a method for producing trimethylgallium as a raw material in metalorganic chemical vapor deposition (MOCVD), in particular to a method for industrially preparing trimethylgallium, and belongs to the technical field of trimethylgallium preparation. Background technique [0003] 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 (MOCVD) and chemical beam epitaxy (CBE), and are currently the most used raw materials. They are widely used in the growth of indium gallium Compound semiconductor thin film materials such as arsenic nitrogen (InGaAsN), indium gallium arsenic (InGaAs), indium gallium phosphide (InGaP), etc. Pure trimethylgallium is a liquid at room temperature. When us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00
Inventor 孙祥祯徐昕潘毅张进琪朱春生陈化冰吉敏坤孙明璐
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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