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The method for recovering iodine and gallium in the preparation of trimethylgallium raffinate from methyl iodide

A technology for recovering iodine from trimethylgallium raffinate, which is applied in the field of raffinate recovery, can solve problems such as high cost, and achieve the effects of low cost, high recovery rate and environmental friendliness.

Inactive Publication Date: 2016-08-17
李矗
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The alloy method generally uses gallium-magnesium alloy and methyl iodide to react. Since methyl iodide is relatively expensive, recovery of iodine and gallium from the raffinate after the reaction is of great significance for cost reduction and comprehensive harmless treatment, but there is no patent report so far. The method for recovering iodine and gallium in the preparation of trimethylgallium raffinate from methyl iodide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 160ml of ethanol to 200ml of the trimethylgallium raffinate prepared from methyl iodide, and stir the reaction until no paste becomes completely liquid; add 8ml of hydrochloric acid to the above solution to adjust the pH to 13; Filtrate, obtain filtrate and The mixed residue of magnesium hydroxide and ferric hydroxide, wash the filter residue with water until neutral, mix the washing water and filtrate; collect the precipitated gallium from the mixed solution of washing water filtrate, collect the washing water and filtrate, add appropriate amount of sulfuric acid to adjust PH=3.5 to precipitate gallium , 0.11g of gallium hydroxide was obtained, and the recovery rate of gallium was 93.4%.

Embodiment 2

[0024] Add 500ml of ethanol to 500ml of the trimethylgallium raffinate prepared from methyl iodide, and stir the reaction until no paste becomes completely liquid; add 20ml of hydrochloric acid to the above solution, adjust the pH to 13; filter , to obtain the mixed residue of the filtrate and magnesium hydroxide and iron hydroxide, wash the filter residue with water to neutrality, mix the washing water and the filtrate; collect the gallium sinking from the washing water filtrate mixture, collect the washing water and the filtrate, add an appropriate amount of sulfuric acid to adjust the pH =4 precipitates gallium, obtains gallium hydroxide 0.34g, and the recovery rate of gallium is 90%.

Embodiment 3

[0026] Add 270ml of ethanol to 300ml of the trimethylgallium raffinate prepared from methyl iodide, and stir the reaction until no paste becomes completely liquid; add 13ml of hydrochloric acid to the above solution, adjust the pH to 13; filter to obtain the mixed residue of the filtrate and magnesium hydroxide and iron hydroxide, wash the filter residue with water to neutrality, mix the washing water and the filtrate; collect the gallium sinking from the washing water filtrate mixture, collect the washing water and the filtrate, and add an appropriate amount of Sulfuric acid adjusts pH=3.5 to precipitate gallium to obtain 0.3 g of gallium hydroxide, and the recovery rate of gallium is 91.8%.

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PUM

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Abstract

The invention relates to a method for recovering iodine and gallium from raffinate produced in preparation of trimethyl gallium from iodomethane. The method is characterized by comprising the following six steps for recovery: alcoholysis; acidolysis; reduction and sublimation for recovery of iodine; neutralization and sedimentation of raffinate; filtering; and collection of mixed liquor of washing water and filtrate and precipitation of gallium. The method provided by the invention has the advantages of easiness, practicality, high recovery rates of iodine and gallium, small investment, low cost, easy operation and friendliness to the environment.

Description

technical field [0001] The invention relates to the recovery of the raffinate after the reaction of metal organic coordination compounds, in particular to a method for recovering iodine and gallium from the raffinate of trimethylgallium prepared from methyl iodide. Background technique [0002] 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 (MO CVD) and chemical beam epitaxy (CBE), and are currently the most used raw materials. They are widely used in the growth of indium Gallium arsenide nitrogen (InGaAsN), indium gallium arsenide (InGaAs), indium gallium phosphide (InGaP) and other compound semiconductor thin film materials. There are many preparation methods for trimethylgallium, and the common methods are aluminum alkyl method and alloy method. The alloy method generally uses gallium-magnesium alloy and methyl iodide to react....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/14C01G15/00
Inventor 李永锋莫荣
Owner 李矗