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Preparation method of electronic grade hexafluoroethane

A hexafluoroethane, electronic-grade technology, applied in the field of preparation of fluorine-containing gas, can solve the problems of small contact area, unfavorable gas passage, influence on reaction efficiency, etc., and achieve the effect of high conversion rate and good effect

Active Publication Date: 2016-12-21
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The catalysts used in existing patents and literature technologies use metals or metal fluorides, and the contact area with organic gases is small, which is not conducive to the passage of gases and affects the efficiency of the reaction

Method used

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  • Preparation method of electronic grade hexafluoroethane
  • Preparation method of electronic grade hexafluoroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step (1): Preparation of Catalyst

[0024] 100Kg of antimony trioxide, 700Kg of water, 20Kg of hydrogen peroxide (mass percentage concentration 40), stirred at 30°C for 4 hours, filtered, and dried to obtain polyantimonic acid; then add 100Kg of activated clay and 2Kg of molecular sieve , stirred at 30°C for 4h, extruded and granulated after the reaction, dried at 300°C for 7h to obtain a catalyst carrier, and then added 2Kg of sodium metaaluminate and 0.3Kg of 1,2-dimethyl-3-hydroxyethylimidazole Tetrafluoroborate, 78Kg hydrogen fluoride pyridine complex, react at 43°C for 6h, and then dry at 150°C for 8h. Get a catalyst.

[0025] Step (2): Synthesis reaction

[0026] Hydrogen fluoride gas and chloropentafluoroethane gas enter the reactor equipped with this catalyst to react, the molar ratio of hydrogen fluoride gas to chloropentafluoroethane is 2:1, the reaction temperature is 400°C, and the space velocity is 3BV / h. Crude hexafluoroethane was obtained.

[0027] St...

Embodiment 2

[0030] Step (1): Preparation of Catalyst

[0031] Mix 100Kg of antimony trioxide, 500Kg of water, and 10Kg of hydrogen peroxide (concentration of 30% by mass), stir at 25°C for 2 hours, filter, and dry to obtain polyantimonic acid; then add 50Kg of activated clay and 1Kg of molecular sieve , stirred at 25°C for 2h, extruded and granulated after the reaction, dried at 200°C for 5h to obtain a catalyst carrier, and then added 1Kg of sodium metaaluminate and 0.1Kg of 1,2-dimethyl-3-hydroxyethylimidazole Tetrafluoroborate, 50Kg hydrogen fluoride pyridine complex, react at 25°C for 5h, and then dry at 100°C for 5h. Get a catalyst.

[0032] Step (2): Synthesis reaction

[0033] Hydrogen fluoride gas and chloropentafluoroethane gas enter the reactor equipped with this catalyst to react, the molar ratio of hydrogen fluoride gas to chloropentafluoroethane is 1:1, the reaction temperature is 400°C, and the space velocity is 1BV / h. Crude hexafluoroethane was obtained.

[0034] Step (...

Embodiment 3

[0037] Step (1): Preparation of Catalyst

[0038] 100Kg of antimony trioxide, 1000Kg of water, 30Kg of hydrogen peroxide (mass percentage concentration 50), stirred at 60°C for 5h, filtered, and dried to obtain polyantimonic acid; then add 200Kg of activated clay and 5Kg of molecular sieve , stirred at 60°C for 5h, extruded and granulated after the reaction was completed, dried at 500°C for 10h to obtain a catalyst carrier, then added 5Kg of sodium metaaluminate, 1Kg of 1,2-dimethyl-3-hydroxyethylimidazole tetra Fluoroborate, 150Kg hydrogen fluoride pyridine complex, react at 60°C for 10h, then dry at 200°C for 10h. Get a catalyst.

[0039] Step (2): Synthesis reaction

[0040] Hydrogen fluoride gas and chloropentafluoroethane gas enter the reactor equipped with this catalyst to react, the molar ratio of hydrogen fluoride gas to chloropentafluoroethane is 3:1, the reaction temperature is 500°C, and the space velocity is 5BV / h. Crude hexafluoroethane was obtained.

[0041] ...

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Abstract

The invention relates to a preparation method of electronic grade hexafluoroethane. The preparation method comprises the following steps: a hydrogen fluoride gas and a chloropentafluoroethane gas enter a reactor containing a novel catalyst, and undergo a reaction at 300-500 DEG C at an air speed of 1-5 BV / h to prepare crude hexafluoroethane, wherein a molar ratio of the hydrogen fluoride gas to the chloropentafluoroethane gas is 1-3:1; and the crude hexafluoroethane is rectified, the rectified hexafluoroethane enters an adsorption tower containing an adsorbent and is adsorbed to obtain the highly-pure hexafluoroethane product.

Description

technical field [0001] The invention relates to a method for preparing fluorine-containing gas, in particular to a method for preparing electronic-grade hexafluoroethane. Background technique [0002] In recent years, with the rapid development of the semiconductor industry, the requirements for the purity of electronic special gas are getting higher and higher, and hexafluoroethane has solved the problem of Conventional wet etching cannot meet the problem of high-precision thin-line etching of deep submicron integrated circuits of 0.18-0.25m, and can perfectly meet the requirements of such processes with small line widths. In various CVD processes based on SiH, hexafluoroethane is used as a cleaning gas. Compared with methane, it has the characteristics of low emission, high gas utilization rate, reaction chamber cleaning rate and equipment output rate. High-purity hexafluoroethane is a necessary medium for VLSI and plays an important role in the development of the semicon...

Claims

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Application Information

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IPC IPC(8): C07C19/08C07C17/10B01J31/26
CPCB01J31/26B01J2231/46C07C17/10C07C19/08
Inventor 陈刚张晓东周井森王宁李军陈立峰钱红东荀雨静郑九丽
Owner ZHEJIANG BRITECH CO LTD
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