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Preparation method of trimethylgallium

A technology of trimethylgallium and trimethylaluminum, applied in the field of preparation of high-purity metal-organic compounds, can solve the problems of difficult recovery of reaction by-products and low yield of trimethylgallium, simplify the process and equipment, and increase the yield Efficiency and purity, ease of reaction process

Active Publication Date: 2015-12-23
JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing trimethylgallium in order to overcome the defects of low trimethylgallium yield and difficult recovery of reaction by-products in the prior art

Method used

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preparation example Construction

[0013] The invention provides a method for preparing trimethylgallium, the method comprising:

[0014] (1) Under an inert atmosphere, iodine is contacted with molten gallium to obtain gallium triiodide;

[0015] (2) In the presence of an initiator and an inert atmosphere, contact reaction of trimethylaluminum with gallium triiodide

[0016] According to the method of the present invention, wherein, in step (1), preferably, the reaction conditions include: the temperature is 100-140° C., and the time is 20-50 minutes; more preferably, the temperature is 120-130° C., and the time is 30 minutes. -40min, so as to further increase the yield of trimethylgallium.

[0017] According to the method of the present invention, wherein, in step (1), the ratio of iodine element to gallium element can be a conventional ratio, preferably, the molar ratio of iodine element to gallium element is 1.5-5:1, more preferably 2 -4.5:1.

[0018] According to the method of the present invention, wher...

Embodiment 1

[0040] This example is used to illustrate the preparation method of trimethylgallium of the present invention.

[0041] (1) Add 2900g of gallium into a reaction kettle filled with nitrogen gas, heat it to 120°C, add 16840g of iodine powder in batches to the molten gallium under stirring conditions, the reaction ends after 30 minutes, and slowly drop into the reaction kettle after natural cooling Add 10440g of trimethylaluminum, add 50g of initiator methyl iodide, continue the reaction at 50°C for 24h, distill out the crude trimethylgallium at 60°C under normal pressure, rectify the crude trimethylgallium, and collect the fraction at the temperature The temperature is 55.8°C, the pressure is normal pressure, and 4480g of trimethylgallium finished product is obtained, the calculated yield of trimethylgallium is 94%, and the purity of trimethylgallium in the finished product is 99.9999%;

[0042] (2) Recycling 25512g of the remaining reaction solution obtained by distilling out t...

Embodiment 2

[0044] This example is used to illustrate the preparation method of trimethylgallium of the present invention.

[0045] (1) Add 2000g of gallium into a reaction kettle filled with nitrogen gas, heat it to 120°C, add 14500g of iodine powder in batches to the molten gallium under stirring conditions, the reaction ends after 30 minutes, and slowly drop into the reaction kettle after natural cooling Add 7200g of trimethylaluminum, add 25g of initiator methyl iodide, continue the reaction at 60°C for 26h, distill out the crude trimethylgallium at 60°C under normal pressure, rectify the crude trimethylgallium, and collect the fractions at the temperature The temperature is 55.8°C, the pressure is normal pressure, and 3122g of trimethylgallium finished product is obtained, the calculated yield of trimethylgallium is 95%, and the purity of trimethylgallium in the finished product is 99.9999%;

[0046] (2) Recycling 16000 g of the remaining reaction liquid obtained by distilling the cr...

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Abstract

The invention relates to a preparation method of trimethylgallium. The method comprises steps as follows: (1) iodine and molten gallium have a contact reaction in the inert atmosphere, and gallium triiodide is obtained; (2) trimethylaluminium and the gallium triiodide have a contact reaction in the presence of an initiator and in the inert atmosphere. With the adoption of the preparation method, the yield and the purity of the trimethylgallium can be significantly increased, the yield of the trimethylgallium can be higher than 90%, the purity can be 99.9999%, besides, a reaction kettle used in the method can be used as an evaporation kettle, the technology and equipment are simplified, the reaction process is easy to control, the prepared product can be separated from raw materials and byproducts more easily, the method is very applicable to industrial production, in addition, the byproducts can be used for synthesizing aluminum sulfate, almost no waste is produced, use of a large amount of highly toxic products, namely, methyl iodide, can be avoided in the technology, and the method is very environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-purity metal-organic compounds, and in particular relates to a preparation method of trimethylgallium. Background technique [0002] High-purity trimethylgallium belongs to high-purity metal-organic compounds. It is the key supporting raw material for the preparation of compound semiconductor thin film materials by advanced metal-organic chemical vapor deposition (MOCVD) technology. It is widely used in LED equipment, new generation solar cells, phase change Memory, semiconductor lasers, infrared detectors and supercomputers and other fields. [0003] At present, the preparation of trimethylgallium has been studied to a certain extent, and the common methods are the alkylaluminum method and the alloy method. The alkylaluminum method uses trimethylaluminum and gallium trichloride to react, but the defect of preparing trimethylgallium in this method is that the yield is low, and the rea...

Claims

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Application Information

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IPC IPC(8): C07F5/00C01B7/14C01F7/74
Inventor 谢贤清廖维林邱曾烨陈飞彪马玉峰吴伟
Owner JIANGXI JIAYIN PHOTOELECTRIC MATERIAL
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