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Preparation method of trimethyl gallium

A technology of trimethyl gallium and methyl magnesium chloride, applied in the field of preparation of trimethyl gallium, can solve the problem of high energy consumption, and achieve the effects of shortening the process flow, reducing the production cost and improving the utilization value

Active Publication Date: 2017-05-31
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the trimethylgallium synthesis process disclosed in CN 103145745 A is an alloy method, and the raw material used is metal gallium obtained by electrolysis, which needs to be prepared into a gallium-magnesium alloy before the subsequent reaction. The energy consumption of the preparation process is high

Method used

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Examples

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Comparison scheme
Effect test

preparation example Construction

[0010] The invention provides a method for preparing trimethylgallium, the method comprising: reacting gallium salt and methylmagnesium chloride in an organic solvent under the protection of an inert gas, and then separating trimethylgallium from the obtained reaction mixture .

[0011] In the method of the present invention, preferably, the reaction conditions include: the temperature is 20-250°C, more preferably 50-150°C; the pressure is 0.005-2MPa, more preferably 0.01-1MPa; the time is 1-20h, more preferably 5-15h; based on gallium and methyl respectively, the molar ratio of gallium salt to methylmagnesium chloride is 0.5-2:3, more preferably 0.8-1.5:3.

[0012] In the method of the present invention, the gallium salt is not particularly limited, and it can be various gallium salts commonly used in the art that can be dissolved in organic solvents. Preferably, the gallium salt is the intermediate salt before gallium metal electrolysis in the process of extracting aluminum ...

Embodiment 1

[0030] This example is used to illustrate the preparation method of trimethylgallium of the present invention.

[0031] (1) Preparation of anhydrous ether solution of gallium chloride: Na 2 O Ga 2 o 3 ·2CO 2 ·(2-5)H 2O is mixed with hydrochloric acid solution for acid dissolution treatment to obtain hydrochloric acid immersion solution, and the aforementioned hydrochloric acid immersion solution is filtered, and the filtrate is evaporated and concentrated to obtain a gallium salt concentrate, and then the gallium salt concentrate is immersed in a macroporous cation exchange resin The column carries out the adsorption of gallium, then with hydrochloric acid solution, the macroporous cationic resin post after the aforementioned adsorption is eluted to obtain the eluent containing gallium, then add anhydrous ether (anhydrous ether and eluent) in the eluent Liquid volume ratio is 1:1) for extraction and drying to obtain anhydrous ether solution of gallium chloride.

[0032] (...

Embodiment 2

[0037] This example is used to illustrate the preparation method of trimethylgallium of the present invention.

[0038] (1) Preparation of diphenyl ether solution of gallium sulfate: Na 2 O Ga 2 o 3 ·2CO 2 ·(2-5)H 2 O is mixed with sulfuric acid solution for acid dissolution treatment to obtain sulfuric acid immersion solution, and the aforementioned sulfuric acid immersion solution is filtered, and the filtrate is evaporated and concentrated to obtain a gallium salt concentrate, and then the gallium salt concentrate is immersed in a macroporous cation exchange resin The column carries out the adsorption of gallium, then with sulfuric acid solution, the macroporous cationic resin column after the aforementioned adsorption is eluted, obtains the eluent containing gallium, then adds diphenyl ether (diphenyl ether and elution Liquid volume ratio is 2:1) for extraction and drying to obtain diphenyl ether solution of gallium sulfate.

[0039] (2) Preparation of diphenyl ether ...

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Abstract

The invention relates to the field of organic compounds and discloses a preparation method of trimethyl gallium. The method comprises the following steps: enabling a gallium salt and methylmagnesium chloride to react in an organic solvent under the protection of an inert gas, and separating the trimethyl gallium from an obtained reaction mixture. The method shortens the process flow, the electrolytic process with higher energy consumption and the synthesis process of a gallium magnesium alloy are avoided, and the production cost of the trimethyl gallium is remarkably lowered.

Description

technical field [0001] The invention relates to the field of organic compounds, in particular to a method for preparing trimethylgallium. Background technique [0002] High-purity trimethylgallium (TMG) is currently one of the main MO source products (high-purity metal-organic compounds), and is widely used as the basis for preparing new semiconductor optoelectronic products such as LEDs by MOCVD (metal-organic chemical vapor deposition) and other processes. Prepare raw materials. [0003] At present, the global demand for TMG is about 100 tons per year, and with the explosive growth of the downstream LED industry in recent years, its demand will still increase rapidly at a rate of at least 20% per year. Due to the high technical complexity and strong industry barriers of the MO source industry dominated by TMG, only a few companies such as the United States and China have the ability to industrialize. The status quo of oligopoly also makes the industry maintain an overall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00
CPCC07F5/00
Inventor 赵兴雷李国涛
Owner CHNA ENERGY INVESTMENT CORP LTD
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