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Method for preparing carbonyl fluoride by cracking perfluorinated compound and carbonyl fluoride

A technology of perfluorinated compounds and carbonyl fluoride, applied in the fields of carbon compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problem of inability to fully utilize raw materials, and achieve low product separation requirements, less by-products, and enhanced utilization. Effect

Active Publication Date: 2022-07-15
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the preparation of formyl fluoride, neither of these two methods can achieve full utilization of raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] CF2=CFOCF2CF3 (50g / s, 98% purity) and oxygen were introduced into a tube furnace preheated to 800°C in a molar ratio of 1:2 for reaction. The tube length of the reaction furnace was 80cm and the nominal diameter was one inch. The reaction pressure is 2 bar. The reacted gas is slowly introduced into a certain amount of anhydrous methanol after air cooling to ensure that all the gases and anhydrous methanol are fully contacted and reacted. After the reaction mixture is washed and dried, GC is carried out. More than 98% is dimethyl carbonate, and the remaining 2% is perfluoroacetyl fluoromethyl.

Embodiment 2

[0075] CF3CF2CF2OCF(CF3)CF2OCF(CF3)CF2OCF(CF3)COF (95% purity, the remaining 5% is CF3CF2CF2OCF(CF3)CF2OCF(CF3)COF) was injected into the tube furnace at a speed of 25g / s, and the Oxygen with a molar ratio of acyl fluoride compound of 2.2:1 was reacted in a tube furnace preheated to 600°C. The tube length of the reaction furnace was 80cm and the nominal diameter was one inch. Sparging is to atomize the liquid into the reactor for reaction. The reacted gas is slowly introduced into a certain amount of anhydrous methanol after air cooling to ensure that all the gases and anhydrous methanol are fully contacted and reacted. After the reaction mixture is washed and dried, GC is carried out. More than 92% is dimethyl carbonate, 3% is perfluoroacetyl fluoride methyl ester, 3% is perfluoropropionyl fluoride methyl ester, and there is about 2% perfluoromethacryloyl fluoride in the reaction product.

Embodiment 3

[0077] The perfluoroisobutene and oxygen in a molar ratio of 1:2 were introduced into a tubular furnace preheated to 1000°C for reaction. The length of the reaction furnace tube was 2m and the nominal diameter was one inch. Wherein the perfluoroisobutene feeding speed is 120g / s, and the pressure in the tubular reactor is 1.1bar. The reacted gas is slowly introduced into a certain amount of anhydrous methanol after air cooling to ensure that all the gases and anhydrous methanol are fully contacted and reacted. After the reaction mixture is washed and dried, GC is carried out. More than 99% is dimethyl carbonate, and the remaining 1% is perfluoroacetyl fluoromethyl.

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Abstract

The invention belongs to the field of fine fluorine chemical industry, and particularly relates to a method for preparing carbonyl fluoride by cracking a perfluorinated compound and carbonyl fluoride. The following compounds are used as reactants to react with oxygen in the presence or absence of catalysts to generate carbonyl fluoride; the compounds include: 1) perfluoroalkene; 2) perfluoroacyl fluoride; 3) perfluorocarbonyl fluoride. The method for cracking perfluorinated compounds into carbonyl fluoride can convert all raw materials into carbonyl fluoride, with few by-products, low requirements for separation of subsequent products, and at the same time, toxic and harmful substances in organic fluorine compounds can be converted into useful The basic raw material greatly enhances the utilization rate of carbon atoms and fluorine atoms, the reaction operation is simple, and the safety is greatly improved. At the same time, the method expands the preparation channels of carbonyl fluoride.

Description

technical field [0001] The invention belongs to the field of fine fluorine chemical industry, and particularly relates to a method for preparing carbonyl fluoride by cracking a perfluorinated compound and carbonyl fluoride. Background technique [0002] Carbonyl fluoride, as an etching gas and cleaning gas for chemical vapor deposition (CVD) chambers in the next-generation semiconductor industry, has a very low global warming potential (GWP) compared to traditional nitrogen trifluoride. At the same time, carbon Acyl fluoride has excellent cleaning performance, the cleaning effect is not inferior to perfluorocarbon and nitrogen trifluoride, and has a lower GWP value. Since carbonyl fluoride reacts with water and decomposes into carbon dioxide (C02), which can be rapidly decomposed in the atmosphere, the use of carbonyl fluoride can greatly reduce the equipment investment and energy consumption of semiconductor industry manufacturing, and has broad development potential. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/00
CPCC01B32/00
Inventor 肖鑫冀汝南于颖
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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