Method for preparing high-purity trifluoroiodomethane

A high-purity technology of trifluoroiodomethane, applied in the field of preparation of fluorine-containing organic compounds, can solve the problems such as the content of inorganic impurities is not clearly specified, and achieve the effects of stable and reliable preparation process, easy operation, and reasonable and simple process

Inactive Publication Date: 2018-10-19
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the patent does not clearly state the content of inorganic impurities in the final product, such as N 2 , O 2 、H 2 O, HF, CO 2 Wait

Method used

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  • Method for preparing high-purity trifluoroiodomethane
  • Method for preparing high-purity trifluoroiodomethane
  • Method for preparing high-purity trifluoroiodomethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The raw material trifluoroiodomethane enters the two-stage adsorption column at a flow rate of 140g / h under the condition of 10°C and 0MPa. The first-stage adsorption column is filled with silica gel adsorbent, and the second-stage adsorption column is filled with 3A molecular sieve adsorbent to remove most of the water. and some organic impurities;

[0033] After adsorption, it is introduced into the rectification tower, and intermittent rectification is carried out at -10-0°C. The venting flow rate at the top of the tower is 0.3L / min, and the venting time is 30min. The purity of the top product is detected to be above 99.99%, and the product is discharged into the gas storage tank , filled into cylinders with a diaphragm compressor.

Embodiment 2

[0035] The raw material trifluoroiodomethane enters the two-stage adsorption column at a flow rate of 200g / h under the condition of 20°C and 0.1MPa. The primary adsorption column is filled with activated alumina adsorbent, and the secondary adsorption column is filled with 5A molecular sieve adsorbent. Most of water and some organic impurities;

[0036] After adsorption, it is introduced into the rectification tower, and intermittent rectification is carried out at -15~-10°C. The venting flow rate at the top of the tower is 0.5L / min, and the venting time is 20min. The purity of the top product is detected to be above 99.99%, and the product is discharged into the gas storage In the tank, fill it into the steel cylinder with a diaphragm compressor.

Embodiment 3

[0038] The raw material trifluoroiodomethane enters the two-stage adsorption column at a flow rate of 70g / h under the conditions of -10°C and -0.05MPa. The primary adsorption column is filled with silica gel adsorbent, and the secondary adsorption column is filled with 10X molecular sieve adsorbent. Most of water and some organic impurities;

[0039] After adsorption, it is introduced into the rectification tower, and intermittent rectification is carried out at -21~-16°C. The venting flow rate at the top of the tower is 0.8L / min, and the venting time is 10min. The purity of the top product is detected to be above 99.99%, and the product is discharged into the gas storage In the tank, fill it into the steel cylinder with a diaphragm compressor.

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Abstract

The invention discloses a method for preparing high-purity trifluoroiodomethane. The method comprises the steps that: raw material trifluoroiodomethane passes through a two-stage adsorption column ata certain temperature and pressure and at a certain flow rate to remove most of the water and some organic impurities, then trifluoroiodomethane enters a rectification tower, batch rectification is conducted at low temperature, and tower top is emptied to remove impurities of halogenated alkanes, halogenated olefins, halogenated alkynes, nitrogen, oxygen, carbon dioxide, carbon monoxide and the like of C1 to C5, thereby obtaining the high-purity trifluoroiodomethane with a purity greater than 99.99%, wherein the H2O content is less than 30 ppmv, HF content is less than 1ppmw, and requirementsof the semiconductor etching and electrical insulation industries are met. The method is reasonable in process and simple in operation, and is an ideal technique for preparing the high-purity trifluoroiodomethane.

Description

technical field [0001] The invention belongs to the technical field of preparation of fluorine-containing organic compounds, and relates to a preparation method of high-purity trifluoroiodomethane. Background technique [0002] Trifluoroiodomethane is the most important product among perfluoroiodoalkanes, and has broad application prospects in fire extinguishing, refrigeration, organic synthesis, semiconductor etching, electrical insulation and other fields. [0003] The purity of general industrial trifluoroiodomethane is 95-99%, which contains a variety of inorganic and organic impurities. When trifluoroiodomethane is used as an electronic etching gas or used in the field of electrical insulation, the types of impurities it contains And quantity has decisive impact on downstream product performance, therefore need to control each impurity content in trifluoroiodomethane, improve product purity. [0004] There are few public reports on the purification method of trifluoroi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/389C07C17/383C07C19/16
CPCC07C17/383C07C17/389C07C19/16
Inventor 董利庆飞要郭占英贾晓卿
Owner 泉州宇极新材料科技有限公司
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