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Method for preparing high-purity trimethylgallium at one step

A high-purity technology of trimethylgallium, which is applied in the field of one-step preparation of high-purity trimethylgallium, can solve problems affecting the purity of substances, and achieve the effects of convenient purification, cost saving, and increased boiling point

Active Publication Date: 2012-06-20
苏州普耀光电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] But because what adopted in the above-mentioned technical scheme is the ether of low molecular weight, because the ether of low molecular weight and product boiling point are closer, so can evaporate together with target product in the disassembly process, thereby influence its material purity

Method used

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  • Method for preparing high-purity trimethylgallium at one step
  • Method for preparing high-purity trimethylgallium at one step
  • Method for preparing high-purity trimethylgallium at one step

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 500g gallium-magnesium alloy Ga x Mg y and metallic magnesium Mg z Put it into the reaction kettle and protect it with inert gas. Wherein x=0.2, y=0.4, z=0.4, x+y+z=1, wherein x, y, z are molar ratios. Add 1200g of tetraethylene glycol dimethyl ether, and gradually add 1950g of methyl iodide dropwise under the condition of normal temperature stirring. After the reaction is completed, continue to reflux at a temperature of 60-100°C for 6h, distill off low boiling point substances, and then continue to raise the temperature to decompose The compounding temperature was controlled at 160-220°C to obtain 239g of high-purity trimethylgallium with a yield of 69% (calculated based on the mass of gallium metal).

[0025] The yield is calculated as follows:

[0026]

[0027] in:

[0028] m TMGa In order to obtain the quality of high-purity trimethylgallium,

[0029] m TMGa is the molecular weight of trimethylgallium,

[0030] m Ga is the molecular weight of gallium, ...

Embodiment 2

[0033] 500g gallium-magnesium alloy Ga x Mg y and metallic magnesium Mg z Put it into the reaction kettle and protect it with inert gas. Wherein x=0.25, y=0.5, z=0.25, x+y+z=1, wherein x, y, z are molar ratios. Add 1200g of tetraethylene glycol dimethyl ether, and gradually add 1950g of methyl iodide dropwise under the condition of normal temperature stirring. After the reaction is completed, continue to reflux at a temperature of 60-100°C for 6h, distill off low boiling point substances, and then continue to raise the temperature to decompose The mixing temperature was controlled at 160-220°C to obtain 324g of high-purity trimethylgallium with a yield of 80% (calculated based on the mass of gallium metal).

Embodiment 3

[0035] 500g gallium-magnesium alloy Ga x Mg y and metallic magnesium Mg z Put it into the reaction kettle and protect it with inert gas. Wherein x=0.3, y=0.4, z=0.3, x+y+z=1, wherein x, y, z are molar ratios. Add 1200g of tetraethylene glycol dimethyl ether, and gradually add 1950g of methyl iodide dropwise under the condition of normal temperature stirring. After the reaction is completed, continue to reflux at a temperature of 60-100°C for 6h, distill off low boiling point substances, and then continue to raise the temperature to decompose The compounding temperature was controlled at 160-220°C to obtain 333g of high-purity trimethylgallium with a yield of 73% (calculated based on the mass of gallium metal).

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Abstract

The invention belongs to the field of preparation of compounds including the III groups of elements in a periodic chart, and relates to a method for preparing high-purity trimethylgallium at one step, which includes the steps: under the protection of inert gas, utilizing polyethylene glycol dimethyl ether as dissolvent and utilizing gallium-magnesium alloy and magnesium metal as raw materials, adding methinehalide into a reaction system with stirring and controlling reaction speed by controlling dropping speed; after reaction is completed, distilling and removing low-boiling-point substance, and then releasing a complex of the polyethylene glycol dimethyl ether and the trimethylgallium so that the trimethylgallium is obtained. The method is simple in process and operation, stable in reaction conditions and convenient to control so as to be safer. Compared with a traditional industrialized method, the method has the advantages that raw materials are cheaper, reaction yield is high, safety is higher, unreacted raw materials are recyclable, production cost is greatly reduced, the raw materials contain no natural substance, safety factor is high in the reaction process, and the method is particularly suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation of compounds containing Group III elements of the periodic table, and relates to a method for preparing trimethylgallium. Background technique [0002] Metal-organic compounds such as high-purity trimethylgallium are widely used in the growth of indium gallium phosphide (InGaP), indium gallium arsenide nitrogen (InGaAsN), indium gallium arsenide (InGaAs) and other compound semiconductor thin film materials. It is the most important raw material for growing optoelectronic materials in the process of metal organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE), and it is also the most used raw material at present. [0003] In the prior art, there are many preparation methods of trimethylgallium, but few methods can be applied to industrialization. The common method is to use industrial trimethylaluminum and gallium trichloride to carry out transalkylation reaction. [0004] The Chinese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00
CPCY02P20/582
Inventor 茅嘉原王士峰李敏洪海燕
Owner 苏州普耀光电材料有限公司
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