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Method for industrially preparing trimethyl indium

A technology of trimethylindium and methyltetrahydrofuran, which is applied in the field of industrialized preparation of trimethylindium, can solve the problems of low reaction conversion efficiency, expensive indium trichloride, and high cost of raw materials, and is suitable for large-scale industrial production and reaction Simple and stable, high reaction yield effect

Active Publication Date: 2013-03-13
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation of trimethylindium generally adopts the transalkylation reaction of trimethylaluminum and indium trichloride, but there are the following disadvantages: 1) the reaction conversion efficiency is not high, and a large number of by-products are produced; 2) the cost of raw materials is high, and industrialization Although trimethylaluminum is cheap, indium trichloride is relatively expensive, especially in industrialized production, and the cost is extremely high; 3) raw materials are flammable, and there are potential safety hazards. Trimethylaluminum is very active and flammable, and the entire reaction must be protected by an inert gas There is a safety hazard

Method used

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  • Method for industrially preparing trimethyl indium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In a reactor filled with nitrogen, put 800g of indium-magnesium alloy into it, add 2150g of anhydrous ether, and gradually add methyl iodide (CH 3 I) 2420g, by controlling iodomethane (CH 3 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 1~70mmgH) to obtain trimethyl indium and ether The complex was finally decomposed (the decomposed temperature was between 80°C and 160° C.) to obtain 492 g of trimethylindium, with a yield of 87% (calculated as metal indium).

Embodiment 2

[0017] In a reactor filled with nitrogen, put 800 g of indium-magnesium alloy into it, add 1600 g of anhydrous ether, and gradually add methyl iodide (CH 3 I) 2420g, by controlling iodomethane (CH 3 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 1~70mmgH) to obtain trimethyl indium and ether The complex was finally decomposed (the decomposed temperature was between 80°C and 160° C.) to obtain 475 g of trimethylindium, with a yield of 84% (calculated as metal indium).

Embodiment 3

[0019] In a reactor filled with nitrogen, put 800g of indium-magnesium alloy into it, add 2150g of anhydrous ether, and gradually add methyl iodide (CH 3 I) 2050g, by controlling iodomethane (CH 3 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 1~70mmgH) to obtain trimethyl indium and ether The complex was finally decomposed (the decomposed temperature was between 80°C and 160° C.) to obtain 458 g of trimethylindium, with a yield of 81% (calculated as metal indium).

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Abstract

The invention relates to a method for industrially preparing trimethyl indium, The method is characterized by comprising the following steps: putting indium-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 indium and ethers under the condition of reduced pressure; and finally decompounding the compound to obtain the trimethyl indium. 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 the 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 trimethylindium as a raw material in metalorganic chemical vapor deposition (MOCVD), in particular to a method for industrially preparing trimethylindium, and belongs to the technical field of trimethylindium preparation. Background technique [0002] Metal-organic compounds such as high-purity trimethylindium are important raw materials for growing optoelectronic materials in the process of metal-organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE), and are widely used in the growth of indium phosphide, indium gallium arsenic nitrogen ( InGaAsN), indium gallium arsenide (InGaAs), indium gallium phosphide (InGaP) and other compound semiconductor thin film materials. Pure trimethyl indium is solid at room temperature. When used for MOCVD, the solid source needs to be packaged in a steel cylinder, and then the temperature of the steel cylinder is controlled to make its vapor pressure re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00
Inventor 孙祥祯陈化冰潘毅朱春生张进琪吉敏坤张溧
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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