Preparation method of high-purity trimethyl aluminum

A technology of high-purity trimethylaluminum and trimethylaluminum, applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve problems such as high viscosity, difficult operation, and high difficulty problems, to achieve the effect of simple operation and improved purification effect

Active Publication Date: 2015-07-15
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 trimethylaluminum, the existing technology will choose to give up a part of trimethylaluminum and let it be taken out together with low-boiling impurities. However, due to the characteristics of trimethylaluminum 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

[0024] Disperse 100g of silica gel powder with a particle size of 400 mesh in an aqueous hydrochloric acid solution with a concentration of 0.1mol / L, stir at 60-70°C for 10-20h, cool to 40°C, add 5g of γ-aminopropyltriethoxysilane and continue stirring 10~20h, then add 10g of tri-n-octylamine, stir for 4~8h, filter to get grafted silica. 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

[0026] in CH 3 MgX and AlX 3 (X is I or Br) as a raw material, with diethyl ether as a solvent, after the synthesis reaction, trimethylaluminum with a purity of 99.0% is obtained through crude extraction. The crude trimethylaluminum was subjected to a purification operation including the following steps.

[0027] Step 2.1: Pour the trimethylaluminum 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.

[0028] 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 operation of step 2 3 times;

[0029] Step 2.3: Heat and decompose the first chromatographic column after the treatment in step 2.2, the heating temperature is 1...

Embodiment 3

[0032] CH 3 X (X is I or Br), aluminum and magnesium are used as raw materials, ether is used as a solvent, and trimethylaluminum with a purity of 99.0% is obtained through crude extraction after the synthesis reaction. The crude trimethylaluminum was subjected to a purification operation including the following steps.

[0033] Step 2.1: Pour the trimethylaluminum 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.

[0034] 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 operation of step 2 3 times;

[0035] Step 2.3: Heat and decompose the first chromatographic column after step 2.2. The heating temperature is 120°...

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Abstract

The invention relates to a preparation method of high-purity trimethyl aluminum, belonging to the technical field of preparation of compounds of Group 3 metals in the periodic table. The preparation method comprises the following steps: (1) preparing a trimethyl aluminum crude product by using aether as a solvent; and (2) purifying the trimethyl aluminum crude product obtained in the step (1), wherein a first chromatographic column is utilized to purify the trimethyl aluminum crude product and adopts grafted silicon dioxide as a stationary phase, and the grafted silicon dioxide is silicon dioxide with tri-n-octyl amine grafted on the surface. The preparation method adopts the two steps of synthesis and separation to obtain the trimethyl aluminum of which the purity can reach 6N. The purification method combines the solid-liquid separation means to load the specific complexant onto the silicon dioxide; and thus, the method is simple to operate and further enhances the purification effect.

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 method for preparing high-purity trimethylaluminum. Background technique [0002] High-purity trimethylaluminum 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 (trimethylaluminum 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 trimethylaluminum is required The purity reaches 99.9999%, otherwise further purification is required. [0003] Chinese invention patent application CN102020668A discloses a me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06
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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