Method for preparation of carbonyl fluoride by cracking of perfluorinated compound and carbonyl fluoride

A technology of perfluorinated compounds and perfluoroacyl fluorides, applied in the fields of carbon compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as inability to fully utilize raw materials, achieve low product separation requirements, enhance utilization, and react Simple operation effect

Active Publication Date: 2019-04-12
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] Feed CF2=CFOCF2CF3 (50g / s, 98% purity) and oxygen at a molar ratio of 1:2 into a tube furnace preheated to 800°C for reaction. The reactor tube is 80cm long and has a nominal diameter of one inch. Reaction pressure 2bar. After the reaction gas was cooled by air, it was slowly passed into a certain amount of anhydrous methanol to ensure that all the gas and anhydrous methanol were fully contacted and reacted. After washing and drying the reaction mixture, it was processed by GC and found that More than 98% is dimethyl carbonate, and the remaining 2% is perfluoroacetyl fluoromethyl ester.

Embodiment 2

[0075] CF3CF2CF2OCF (CF3) CF2OCF (CF3) CF2OCF (CF3) COF (95% purity, the remaining 5% is CF3CF2CF2OCF (CF3) CF2OCF (CF3) COF) is sprayed into the tube furnace at a speed of 25g / s, and simultaneously fed with Oxygen with acyl fluoride molar ratio of 2.2:1 is reacted in a tube furnace preheated to 600°C. The tube length of the reaction furnace is 80 cm, and the nominal diameter is one inch. Injection is to atomize the liquid into the reactor for reaction. After the reaction gas was cooled by air, it was slowly passed into a certain amount of anhydrous methanol to ensure that all the gas and anhydrous methanol were fully contacted and reacted. After washing and drying the reaction mixture, it was processed by GC and found that More than 92% is dimethyl carbonate, 3% is perfluoroacetyl fluoride methyl ester, 3% is perfluoropropionyl fluoride methyl ester, and about 2% of the reaction product is perfluoromethacryloyl fluoride.

Embodiment 3

[0077] Pass perfluoroisobutylene and oxygen into a tube furnace preheated to 1000°C at a molar ratio of 1:2 for reaction. The tube length of the reaction furnace is 2m, and the nominal diameter is one inch. The feeding rate of perfluoroisobutylene is 120g / s, and the internal pressure of the tubular reactor is 1.1 bar. After the reaction gas was cooled by air, it was slowly passed into a certain amount of anhydrous methanol to ensure that all the gas and anhydrous methanol were fully contacted and reacted. After washing and drying the reaction mixture, it was processed by GC and found that More than 99% is dimethyl carbonate, and the remaining 1% is perfluoroacetyl fluoromethyl ester.

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PUM

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Abstract

Belonging to the field of fine fluorine chemical industry, the invention in particular relates to a method for preparation of carbonyl fluoride by cracking of a perfluorinated compound and carbonyl fluoride. The following compounds are adopted as the reactant for reaction with oxygen in the presence or absence of a catalyst to produce carbonyl fluoride. The compounds include: 1) perfluoroolefine;2) perfluoroacyl fluoride; and 3) perfluorocarbonyl fluoride. The method of cracking the perfluorinated compound into carbonyl fluoride can convert all the raw materials into carbonyl fluoride, the by-product is few, and the follow-up product separation requirement is low, at the same time toxic and harmful substances in the organofluorine compound can be converted into useful basic raw materials,thus greatly enhancing the utilization of carbon atoms and fluorine atoms, the reaction operation is simple, the safety is greatly improved, and 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 specifically relates to a method for preparing carbonyl fluoride by cracking perfluorinated compounds and the carbonyl fluoride. Background technique [0002] Carbonyl fluoride, as an etching gas and cleaning gas for chemical vapor deposition (CVD) chambers in the new generation of semiconductor industry manufacturing, 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 equipment investment and energy consumption in semiconductor industry manufacturing, and has broad development p...

Claims

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Application Information

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Patent Type & Authority Applications(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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