Efficient purifying method of triethyl gallium

A purification method, the technology of triethylgallium, which is applied in the field of efficient purification of triethylgallium, can solve the problems of high viscosity, high risk, and difficult operation, and achieve the effect of improving the 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 triethylgallium, the existing technology will choose to give up part of triethylgallium and let it be taken out with low boiling point impurities. However, due to the characteristics of triethylgallium 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

[0021] 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.

[0022] 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.

[0023] For the crude product of triethylgallium with a purity of 99.0% (using diethyl ether as a solvent, using CH 3 CH 2 MgI and GaI 3 Prepared for raw material reaction) for purif...

Embodiment 2

[0030] 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.

[0031] 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.

[0032] For the crude product of triethylgallium with a purity of 99.0% (using diethyl ether as a solvent, using CH 3 CH 2 MgI and GaI 3 Prepared for raw material reaction) for purification.

[0033] Th...

Embodiment 3

[0038] 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.

[0039] 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.

[0040] For the crude product of triethylgallium with a purity of 99.0% (using diethyl ether as a solvent, using CH 3 CH 2 MgI and GaI 3 Prepared for raw material reaction) for purificatio...

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Abstract

The invention relates to an efficient purifying method of triethyl gallium, belonging to the technical field of compound purification. The purifying method comprises the following steps of firstly, filtering a crude product of triethyl gallium by using a first chromatographic column with a stationary phase as filler; and then, purifying the filtered crude product of triethyl gallium in a second chromatographic column with a stationary phase as surface grafted filler, wherein the surface grafted filler is filler of which the surface is grafted with tri-n-octylamine. 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 triethylgallium. Background technique [0002] High-purity triethylgallium is widely used in the growth of indium gallium phosphide, indium gallium arsenic nitrogen, indium gallium arsenic and other compound semiconductor thin film materials. It is an optoelectronic material grown in metal organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE) 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 (triethylgallium with insufficient purity will have a great impact on the performance of the chip and will also greatly damage the MOCVD equipment), high-purity triethylgallium is required The purity reaches 99.9999%, otherwise further purification is required. [0003] Chine...

Claims

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Application Information

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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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