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Method for industrially preparing triethyl gallium

A technology of triethyl gallium and methyl tetrahydrofuran, which is applied in the field of triethyl gallium preparation, can solve the problems of filling and transfer safety hazards, low reaction conversion efficiency, and high price of triethyl 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

[0003] There are many preparation methods for triethylgallium, but there are few methods that can be applied to industrialization. The common method is to use industrial triethylaluminum and gallium trichloride to carry out transalkylation reaction, but there are the following disadvantages: 1) reaction transformation 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 triethylaluminum 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 potential safety hazards, triethylaluminum 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 triethyl gallium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In a reactor filled with nitrogen, put 650g of gallium-magnesium alloy into it, add 2200g of anhydrous ether, and gradually add iodoethane (CH 3 CH 2 I) 2700g, by controlling ethyl iodide (CH 3 CH 2 The addition speed of 1) 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 1~50mmgH) to obtain triethylgallium and ether The complex was finally decomposed (the decomposed temperature is between 90 and 180° C.) to obtain 483 g of triethylgallium, with a yield of 75% (calculated as metal gallium).

Embodiment 2

[0017] In a reactor filled with nitrogen, put 650g of gallium-magnesium alloy into it, add 3000g of anhydrous ether, and gradually add iodoethane (CH 3 CH 2 I) 2700g, by controlling ethyl iodide (CH 3 CH 2 The addition speed of 1) 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 1~50mmgH) to obtain triethylgallium and ether The complex was finally decomposed (the temperature of decomposition was between 90°C and 180° C.) to obtain 457 g of triethylgallium, with a yield of 71% (calculated as metal gallium).

Embodiment 3

[0019] In a reactor filled with nitrogen, put 650g of gallium-magnesium alloy into it, add 2200g of anhydrous ether, and gradually add iodoethane (CH 3 CH 2 1) 2000g, by controlling ethyl iodide (CH 3 CH 2 The addition speed of 1) 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 1~50mmgH) to obtain triethylgallium and ether The complex is finally decomposed (the decomposed temperature is between 90 and 180° C.) to obtain 425 g of triethylgallium, with a yield of 66% (calculated as metal gallium).

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Abstract

The invention relates to a method for industrially preparing triethyl 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 triethyl gallium and ethers under the condition of reduced pressure; and finally decompounding the compound to obtain the triethyl 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

technical field [0001] The invention relates to a method for producing triethylgallium as a raw material in metalorganic chemical vapor deposition (MOCVD), in particular to a method for industrially preparing triethylgallium, and belongs to the technical field of triethylgallium preparation. Background technique [0002] Metal-organic compounds such as high-purity triethylgallium 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 triethylgallium is liquid at room temperature. When used in MOCVD, the source needs to be packaged in a steel cylinder, and then the temperature of the steel cylinder is control...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00
Inventor 孙祥祯潘兴华吕宝源孙明璐蔡岩馨陈化冰潘毅万欣
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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