Purification method and preparation method for carbonyl fluoride

A purification method and carbonyl fluoride technology, which are applied in the purification method and preparation field of carbonyl fluoride, can solve the problems of exposure, high toxicity, difficulty in purification and separation, etc., and achieve the effect of reducing the content

Active Publication Date: 2016-09-28
PERIC SPECIAL GASES CO LTD
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Problems solved by technology

[0005] 1) The method of using carbon monoxide or carbon dioxide to react with fluorinating agents such as fluorine gas and silver difluoride; this method is prone to explosion, and requires expensive corrosion-resistant materials, and the prepared carbonyl fluoride yield and purity are low
[0006] 2) Using phosgene COCl 2 A method of reacting with fluorinating agents such as hydrogen fluoride, antimony trifluoride, arsenic trifluoride, and sodium fluoride; the raw material phosgene used in this method is a highly toxic substance, and the purity of the prepared carbonyl fluoride is low
[0008] 4) The method of reaction between tetrafluoroethylene and oxygen is adopted; during the reaction process of this met

Method used

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  • Purification method and preparation method for carbonyl fluoride
  • Purification method and preparation method for carbonyl fluoride
  • Purification method and preparation method for carbonyl fluoride

Examples

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preparation example Construction

[0042] The present invention also provides a method for preparing carbonyl fluoride, comprising:

[0043] Using CO, CO 2 Any one or more of them react with fluorine-containing gas to prepare carbonyl fluoride; the fluorine-containing gas is ClF, ClF 3 and ClF 5 any one or more of

[0044] Or use COFCl to react with fluorine-containing gas to prepare carbonyl fluoride; the fluorine-containing gas is ClF, ClF 3 , ClF 5 and F 2 any one or more of them.

[0045] The present invention adopts CO, CO 2 And any one or more of COFCl, and ClF, ClF 3 , ClF 5 and F 2 Any one or more of them are raw materials, and the preparation of carbonyl fluoride gas has a higher yield and purity. At the same time, it has higher safety and economic benefits.

[0046] The present invention for the CO, CO 2 and COFCl are not particularly limited, and can be conventional CO, CO in the art 2 and COFCl.

[0047] The present invention is to described ClF, ClF 3 , ClF 5 and F 2 There is no sp...

Embodiment 1

[0061] 5 mol COF 2 The crude product gas is fed into a dry 5L stainless steel reactor device, and then fed into chlorine trifluoride for reaction, ClF 3 The molar ratio of carbonyl fluoride crude product gas is 1:1. The reaction temperature is 499°C, and the reaction pressure is 5MPa; the reaction product is derived from the gas outlet of the reactor device, passed into a cryogenic cold trap with a temperature of -110°C, and impurities are removed by freezing and vacuuming, and the purified product is collected. The gas is sent to the carbonyl fluoride refined gas storage tank, and the purified gas is detected.

[0062] Specifically, the purified gas was introduced into gas chromatography / mass spectrometer GC-MS (model GC-2014 of Shimadzu Corporation of Japan) and Fourier transform infrared spectroscopy FT-IR instrument (model Nicolet 6700) to analyze its composition. The collected gas was determined to be carbonyl fluoride by GC-MS and FT-IR, and the purity of the main comp...

Embodiment 2

[0066] The reaction temperature in the reactor is -99°C, and the reaction pressure is -0.09MPa. During the reaction, 2 grams of cesium fluoride CsF, ClF 3 The molar ratio to the carbonyl fluoride crude product gas is 1000:1 and the rest are the same as in Example 1.

[0067] The detection conditions of Example 1 are used to detect the purified gas, as can be seen: the purified gas is carbonyl fluoride with a purity of 99.95%; the impurity CO 2 Content-6 (volume ratio), COCl 2 Content-6 (volume ratio), CO content -6 (volume ratio), N 2 O content -6 (Volume ratio).

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Abstract

The invention provides a purification method for carbonyl fluoride. The purification method comprises the steps that purifying gas is used for reacting with impurities in gas of a crude carbonyl fluoride product to remove the impurities in the gas of the crude carbonyl fluoride product, wherein the purifying gas is any one or more of ClF, ClF3, ClF5 and F2. According to the purification method, the crude carbonyl fluoride reaction product is purified, any one or more of ClF, ClF3, ClF5 and F2 are adopted as the purifying gas to react with the crude carbonyl fluoride reaction product in a purification device, various impurities, especially CO2, CO, H2O, phosgene COCl2, N2O and the like, except carbonyl fluoride are removed, and the content of impurities is greatly reduced. In purified fine carbonyl fluoride gas, the purity of COF2 is larger than or equal to 99.95%, the content of CO2 is smaller than or equal to 150*10<-6> (the volume ratio), and the content of COCl2 is smaller than or equal to 150*10<-6> (the volume ratio).

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a purification method and preparation method of carbonyl fluoride. Background technique [0002] At present, in the field of semiconductor and liquid crystal manufacturing, perfluorocarbons are mostly used as etching gases and cleaning gases, but the above-mentioned gases usually have a large global warming potential (GWP, Global Warming Potential) value. In order to reduce the greenhouse effect, it is necessary to develop Alternative products with low GWP value. [0003] Carbonyl Fluoride (COF 2 ) is a semiconductor etching gas with a low GWP value, a semiconductor cleaning gas, and a fluorinating agent and an important intermediate in organic synthesis. [0004] At present, the production and preparation methods of carbonyl fluoride are generally divided into the following four types: [0005] 1) The method of reacting carbon monoxide or carbon dioxide with fluorin...

Claims

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Application Information

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IPC IPC(8): C01B31/00
CPCC01P2006/80
Inventor 蒋玉贵商洪涛孟祥军郑秋艳郗少杰李丹丹杨庆平
Owner PERIC SPECIAL GASES CO LTD
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