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Efficient purifying method of trimethylindium

A purification method and trimethyl indium technology are applied in the field of efficient purification of trimethyl indium, which can solve the problems of high viscosity, high risk, and difficulty in removal, and achieve the effects of improving purification effect and simple operation.

Active Publication Date: 2015-08-05
苏州普耀光电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the complexing agents are macromolecular high-boiling point liquids with high viscosity. Small-molecular low-boiling point impurities are easily wrapped in macromolecular high-boiling point complexing agents and are not easy to be eliminated. The purity generally only reaches 95.0-99.0 %
On the other hand, in order to ensure the purity of trimethylindium, the existing technology will choose to give up a part of trimethylindium and let it be taken out together with low-boiling impurities. However, due to the characteristics of trimethylindium itself, this part of the work The risk is greater, it is not easy to operate, and it is more difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 100 g of silica gel powder with a particle size of 5 μm into a chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and the first chromatographic column can be obtained.

[0023] Disperse 100g of amorphous silica gel with a particle size of 5μm in a reaction kettle filled with anhydrous toluene solution, then add 6g of γ-aminopropyltriethoxysilane dropwise at 60°C, and stir for 12~ 15h; then dropwise add a total of 12g of tri-n-octylamine, stir and react for 6h, then filter, wash and dry to obtain surface-grafted amorphous silica gel. Add the obtained surface-grafted amorphous silica gel into a second chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and obtain the second chromatographic column.

[0024] For the crude product of trimethylindium with a purity of 99.0% (with diethyl ether as solvent, CH 3 MgI and GaI 3 Prepared for raw material reaction) for purification.

[00...

Embodiment 2

[0032] Put 100 g of alumina with a particle size of 5 μm into a chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and the first chromatographic column can be obtained.

[0033] Disperse 100g of alumina with a particle size of 5μm in a reaction kettle filled with anhydrous toluene solution, then add 6g of γ-aminopropyltriethoxysilane dropwise at 80°C, and stir for 15h; then A total of 12 g of tri-n-octylamine was added dropwise, stirred and reacted for 6 hours, and then filtered, washed and dried to obtain surface-grafted alumina. Add the obtained surface-grafted alumina into a second chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and then obtain the second chromatographic column.

[0034] For the crude product of trimethylindium with a purity of 99.0% (with diethyl ether as solvent, CH 3 MgI and GaI 3 Prepared for raw material reaction) for purification.

[0035] The purification ...

Embodiment 3

[0041] Put 100 g of titanium dioxide with a particle size of 5 μm into a chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and the first chromatographic column can be obtained.

[0042] Disperse 100g of titanium dioxide with a particle size of 5μm in a reaction kettle filled with anhydrous toluene solution, then add 6g of γ-aminopropyltriethoxysilane dropwise at 80°C, and stir for 18h; then drop Add a total of 12 g of tri-n-octylamine, stir and react for 6 hours, and then filter, wash and dry to obtain surface-grafted titanium dioxide. Add the obtained surface-grafted titanium dioxide into a second chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and then obtain the second chromatographic column.

[0043] For the crude product of trimethylindium with a purity of 99.0% (with diethyl ether as solvent, CH 3 MgI and GaI 3 Prepared for raw material reaction) for purification.

[0044] Th...

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Abstract

The invention relates to an efficient purifying method of trimethylindium, belonging to the technical field of compound purification. The purifying method comprises the following steps of (1) pouring a crude product of trimethylindium into a first chromatographic column with a stationary phase as filler, naturally and downwards flowing the crude product of trimethylindium by virtue of gravity, and collecting a solution when all the liquid flows up; (2) pouring the collected solution into a second chromatographic column with a stationary phase as surface grafted filler, naturally and downwards flowing the solution by virtue of gravity, and collecting the solution when all the liquid flows up; then, pouring the collected solution into the second chromatographic column, and repeating the operation 2-5 times, wherein the surface grafted filler is filler of which the surface is grafted with tri-n-octylamine; and (3) heating and disassembling the second chromatographic column treated in the step (2), and collecting by vacuumizing at the bottom of the chromatographic column to obtain purified trimethylindium. The purifying method disclosed by the invention is combined with a solid-liquid separation means, and a specific coordination agent is loaded on the filler, so that not only is the method simple, but also the purifying effect is further improved.

Description

technical field [0001] The invention belongs to the technical field of compound purification, and more specifically, the invention relates to a high-efficiency purification method of trimethylindium. Background technique [0002] High-purity trimethyl indium is widely used in the growth of compound semiconductor thin film materials such as indium gallium phosphide, indium gallium arsenic nitrogen, and indium gallium arsenic. The most important and the most used raw material at present. In order to meet the high-purity and high-precision quality requirements of optoelectronic materials (trimethylindium with insufficient purity will have a great impact on the performance of the chip and will also cause great damage to MOCVD equipment), high-purity trimethylindium is required The purity reaches 99.9999%, otherwise further purification is required. [0003] Chinese invention patent application CN102020668A discloses a method for the industrial production of trimethyl indium. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00B01D15/20
CPCB01D15/206B01J2220/54C07F5/00G01N30/50
Inventor 顾宏伟茅嘉原李敏王士峰洪海燕
Owner 苏州普耀光电材料有限公司
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