Preparation method of high-purity trimethylindium

A technology of high-purity trimethylindium and trimethylindium, which is applied in the field of preparation of high-purity trimethylindium, can solve problems such as high viscosity, difficult operation, and high risk, and achieve simple operation and improved purification effect Effect

Active Publication Date: 2017-03-08
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] Disperse 100g of silica gel powder with a particle size of 1000 mesh in an aqueous hydrochloric acid solution with a concentration of 1mol / L, acidify at 80°C for 15h, cool to 40°C, add 5g of γ-aminopropyltriethoxysilane and continue stirring for 12h , Then add 10g of tri-n-octylamine, stir for 8h, and get grafted silica after filtration. Put the obtained grafted silica into a chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, then add n-hexane to wash, and the first chromatographic column can be obtained after washing. Put 100 g of silica gel powder with a particle diameter of 400 mesh into a chromatographic column (with an inner diameter of 10 mm), pressurize to ensure uniform filling, and the second chromatographic column can be obtained.

Embodiment 2

[0024] in CH 3 MgX and InX 3 (X is I or Br) as a raw material, with diethyl ether as a solvent, after the synthesis reaction, trimethylindium with a purity of 85.0% is obtained through crude extraction. The crude trimethylindium product was subjected to a purification operation including the following steps.

[0025] Step 2.1: Pour the trimethylindium into the second chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out.

[0026] Step 2.2: Pour all the solution collected in step 2.1 into the first chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out; then pour all the collected solution into the first chromatographic column , repeat the aforementioned operations of step 2 6 times;

[0027] Step 2.3: heat and decompose the first chromatographic column after the treatment in step 2.2. The heating temperature i...

Embodiment 3

[0030] CH 3 X (X is I or Br), indium and magnesium are used as raw materials, ether is used as a solvent, and trimethylindium with a purity of 85.0% is obtained through crude extraction after the synthesis reaction. The crude trimethylindium product was subjected to a purification operation including the following steps.

[0031] Step 2.1: Pour the trimethylindium into the second chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out.

[0032] Step 2.2: Pour all the solution collected in step 2.1 into the first chromatographic column prepared in Example 1, rely on gravity to flow down naturally, and collect the solution after the liquid flows out; then pour all the collected solution into the first chromatographic column , repeat the aforementioned operations of step 2 6 times;

[0033] Step 2.3: Heat and decompose the first chromatographic column after the treatment in step 2.2. The heating t...

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PUM

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Abstract

The invention relates to a preparation method of high-purity trimethyl indium, belonging to the technical field of preparing group III metallic compounds in the periodic table of elements. The preparation method disclosed by the invention comprises the following steps: (1) taking diethyl ether as a solvent to prepare a trimethyl indium crude product; (2) carrying out purification to the trimethyl indium crude product obtained in step (1), wherein the purification method comprises the step of adopting a first chromatographic column to carry out purification to the trimethyl indium crude product; and the stationary phase adopted by the first chromatographic column is grafted silica, and the grafted silica is silica of which the surface is grafted with tri-n-octylamine. The preparation method disclosed by the invention adopts the two steps of synthesis and separation and obtains the trimethyl indium of which the purity can reach 6N; above all, the purity method adopted is combined with the solid-liquid separation means, a certain coordination agent is loaded on the silica, not only is the operation simple, but also the purification effect is improved further.

Description

technical field [0001] The invention belongs to the technical field of preparation of group III metal compounds of the periodic table of elements, and more specifically, the invention relates to a preparation method of high-purity trimethyl indium. Background technique [0002] High-purity trimethyl indium is widely used in the growth of semiconductor thin film materials, and is an important raw material for growing optoelectronic materials in the process of metal organic chemical vapor deposition (MOCVD) and chemical beam epitaxy (CBE). 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00
CPCC07F5/00
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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