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Production method of ultra-high-purity triethylaluminium

A triethylaluminum, ultra-high technology, applied in the field of high-purity chemical preparation, can solve problems such as high impurity content, high silicon content, inability to remove all, and achieve high yield, less labor, and low process cost. Effect

Inactive Publication Date: 2019-12-03
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most of the commercially available triethylaluminum is used as a catalyst, which has high impurity content and cannot meet the purity requirements of the MOCVD process.
Due to the problem of the synthesis process, triethylaluminum contains a large amount of organic silicon with a wide boiling point range. After direct vacuum distillation, the content of silicon element in the residual impurity content is particularly high, which cannot be removed.
There are journal documents published, such as the report of "Research on High Purity Triethylaluminum and Triethylgallium", the triethylaluminum product also contains silicon impurities as high as 14ppm. With the development of the times and technology, this content does not Cannot meet the purity requirements of today's semiconductor materials

Method used

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  • Production method of ultra-high-purity triethylaluminium

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preparation example Construction

[0032] The preparation method of ultra-high-purity triethylaluminum of the present invention, concrete process step is:

[0033] 1) The raw material and the ligand form a stable solid-state complex, and the ligand is a compound containing phosphorus; in an anhydrous, oxygen-free and inert atmosphere glove box, take a ligand 1.2 times the amount of triethylaluminum and an appropriate amount of anhydrous n-hexane Put it into a round-bottomed flask, the ligand is insoluble in n-hexane to form a suspension; add the triethylaluminum raw material into the flask through a constant pressure funnel, stir and shake well, and let stand;

[0034] 2) Complex washing and filtering: outside the inert atmosphere glove box, configure a vacuum system with a cold trap. The cold trap is cooled by liquid nitrogen, and the absolute pressure of the vacuum is adjusted to 30±2KPa. slowly pour the solid complex formed by triethylaluminum and the ligand into the sand core funnel matching the suction fil...

Embodiment 1

[0040] In a 2000mL round-bottomed flask with a stirring rod, add 2.1mol of a ligand containing phosphorus, and then add 1000±50mL of dry n-hexane, stir to disperse the ligand evenly, and continue stirring.

[0041] Through a constant pressure funnel, drop 1.75mol of triethylaluminum raw material (containing 450ppm of silicon impurities) into the round bottom flask, triethylaluminum and the ligand form a solid complex, and release heat at the same time, the temperature of the kettle rises by about 10°C, and continue to stir to room temperature in the flask.

[0042] Place a clean sand core funnel on the suction filter bottle, configure a vacuum system with a cold trap outside the inert atmosphere glove box, cool the cold trap with liquid nitrogen, adjust the vacuum degree to 30±2KPa (absolute pressure), and connect it to the glove box After connecting with the suction filter bottle to build a suction filtration device, pour the suspension in the 2000mL bottle into a sand core f...

Embodiment 2

[0053] On the basis of Example 1, one n-hexane washing was reduced.

[0054] On the same device, put in the same raw materials, pour the suspension in the 2000mL bottle into a sand core funnel, perform intermittent vacuum filtration, and the filtered n-hexane falls into the suction filter bottle.

[0055] After the first suction filtration, cut off the vacuum, pour about 250±10mL of clean n-hexane into the sand core funnel to wash the solid left after suction filtration, and then suction filtration again.

[0056] Transfer away the normal hexane in the suction filter bottle, and continue to suck the solid in the sand core funnel for 30-40 minutes to make it dry.

[0057] The solids in the fritted funnel were transferred to a 2000 mL round bottom flask and weighed.

[0058] A crude product of triethylaluminum was obtained.

[0059] Put several batches of crude products into the kettle, and purify triethylaluminum by means of vacuum rectification under the vacuum degree of 0-0...

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Abstract

The invention relates to a production method of ultra-high-purity triethylaluminium. The production method of the ultra-high-purity triethylaluminium comprises the following steps: subjecting a triethylaluminium raw material and a phosphorus-containing compound ligand to complexation to form a stable solid complex; washing and filtering the complex: arranging a vacuum system with a cold trap outside an inert atmosphere glove box, adjusting a vacuum degree (absolute pressure) to be 30+ / -2 KPa, connecting the vacuum system with a suction filtration bottle after being connected with the interiorof the glove box, slowly pouring the solid complex into a sand core funnel matched with the suction filtration bottle, and performing suction filtration to obtain normal hexane; soaking the solid complex in the sand core funnel by adopting anhydrous normal hexane, and conducting suction filtration and drying on the complex; conducting decomplexation on the complex to obtain a crude product: transferring a dry solid ligand into a round-bottom flask, by adopting a vacuum heating method, receiving fractions at a temperature of 150 DEG C or below as low-boiling-point impurities, receiving fractions at a temperature from 150 DEG C to 190 DEG C as a crude product, and cooling a jacketed receiving bottle interlayer with normal hexane at a temperature of -50 DEG C; and conducting rectification inan anaerobic anhydrous inert atmosphere, and collecting middle fractions to obtain a product with a content of 99.9995%.

Description

technical field [0001] The invention relates to a precursor used in the semiconductor industry, in particular to a preparation method of ultra-high-purity triethylaluminum, and belongs to the technical field of high-purity chemical preparation. Background technique [0002] Triethylaluminum is a metal organic compound. It is a colorless liquid at normal temperature and pressure. It is chemically active. It can spontaneously ignite in air and explode when it meets water. In the petrochemical industry, triethylaluminum is one of the components of Ziegler-Natta catalysts, and is often used in low-pressure polymerization of ethylene, propylene polymerization and isoprene polymerization. In addition, triethylaluminum is also a key material for the production of rocket fuel and solar organic silicon raw materials; it is also widely used in plastic additives, anti-vibration agents, and fungicides. Its pure product can be used in metal organic chemical vapor deposition (MOCVD) proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06
CPCC07F5/062
Inventor 徐耀中万欣刘宇董礼刘子伟常华
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL
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