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Preparation method of ultra-high-purity carbon tetrachloride

A pure carbon tetrachloride and carbon tetrachloride technology, applied in the disproportionation separation/purification of halogenated hydrocarbons, organic chemistry, etc., can solve the problems of unsatisfactory requirements and cumbersome operation, and achieve low cost, simple operation, and less labor Effect

Active Publication Date: 2020-08-11
JIANGSU NATA OPTO ELECTRONICS MATERIAL
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] Patent Publication Nos. CN2379461Y, CN204111620U, CN102417434A, CN106040206A disclose the purification method of carbon tetrachloride, which can make the purity up to 99.9%. Requirements for pure carbon tetrachloride

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  • Preparation method of ultra-high-purity carbon tetrachloride
  • Preparation method of ultra-high-purity carbon tetrachloride

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Embodiment

[0038] There are many manufacturers of carbon tetrachloride, and the processes used are different, resulting in different content of impurities. Using GC detection, through comparison, screen AR-grade carbon tetrachloride from different manufacturers, and select products with less organic impurities and high effective content of carbon tetrachloride as raw materials. After GC detection, the effective content of carbon tetrachloride in the raw material is 96.82%, and there are about 14 kinds of organic impurities, accounting for 3.18%.

[0039] Get 5L carbon tetrachloride and pack in the round bottom flask, with 0.15% (calculated by the weight of carbon tetrachloride) AR grade P 2 o 5 Add it to the carbon tetrachloride raw material, seal it and shake it evenly, transfer it to an anhydrous and oxygen-free inert gas glove box, and let it stand for 1 day. Detected by a Mettler-Toledo moisture meter, the next step is to proceed after the moisture in the raw material is completely...

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Abstract

The invention discloses a preparation method of ultra pure carbon tetrachloride. The preparation method comprises following steps: raw materials are subjected to water removing treatment, and rectification so as to remove most organic and inorganic impurities; adsorption with molecular sieve and active carbon is carried out so as to remove trace organic impurities via adsorption; filtering is carried out so as to remove the molecular sieve and active carbon and obtain a filtrate containing no organic impurity; and at last distillation is carried out so as to remove inorganic impurities and obtain ultra pure carbon tetrachloride. It is confirmed by GC detection that the preparation method is capable of removing organic impurities in carbon tetrachloride; it is confirmed by ICP-OES all element detection that inorganic impurity content is less than 1ppm. The purity of carbon tetrachloride obtained via the preparation method is as high as 99.9999%, and is capable of satisfying raw material application requirements in the semiconductor industry. The preparation method is relatively low in cost; operation is simple; labor intensity is low; and the preparation method is suitable for industrialized large scale production.

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 carbon tetrachloride, and belongs to the technical field of high-purity chemical preparation. Background technique [0002] Carbon tetrachloride is a colorless, toxic, volatile liquid with a slightly sweet smell of chloroform. Mainly used in organic synthesis, drug extractant, insecticide, refrigerant, identification reagent of some metals and nonmetals. [0003] The methods for producing carbon tetrachloride usually include: methane hot chlorine substitution method, carbon disulfide chlorination method, phosgene catalytic method, high-pressure chlorine solution method, methane oxychlorination method, methanol hydrochlorination method, etc., among which the methane hot chlorine substitution method and carbon disulfide method are most commonly used. [0004] The carbon tetrachloride reagent sold on the market has an effec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/38C07C19/041
CPCC07C17/38C07C19/041
Inventor 徐耀中万欣刘宇董礼许从应林俊元潘兴华常华
Owner JIANGSU NATA OPTO ELECTRONICS MATERIAL