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Method for preparing carbonyl fluoride from p-trichloromethylphenyl isocyanate

A technology of trichloromethylbenzene isocyanate and carbonyl fluoride, which can be used in the preparation of chlorides, chemical instruments and methods, preparation of amino-substituted functional groups, etc., can solve problems such as difficult reactions, and achieve good safety and high reaction yield. , the effect of mild reaction conditions

Active Publication Date: 2017-12-15
ZIBO FEIYUAN CHEM CO LTD
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Problems solved by technology

[0013] However, in the above reaction, it is difficult to carry out the reverse reaction, because it is relatively easy to remove hydrogen fluoride from the intermediate carbamoyl fluoride to obtain isocyanate, but it is relatively easy to generate the intermediate carbamoyl fluoride from the reaction of isocyanate and hydrogen fluoride. Difficult to respond

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  • Method for preparing carbonyl fluoride from p-trichloromethylphenyl isocyanate
  • Method for preparing carbonyl fluoride from p-trichloromethylphenyl isocyanate

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Embodiment Construction

[0038] The following will take p-trichloromethylphenylisocyanate as an example to further describe the present invention in detail, but the specific examples described below are only examples of the present invention and do not constitute any limitation to the present invention. All or part of the surface of the reaction device in the present invention is made of corrosion-resistant materials such as carbonyl fluoride, hydrogen fluoride, hydrogen chloride and hydrofluoric acid. The overall response is as follows:

[0039]

[0040] After the nitrogen leak test, vacuum the alloy autoclave, add 300Kg of p-trichloromethylbenzene isocyanate and 761Kg of anhydrous hydrogen fluoride under negative pressure, start stirring, control the temperature at 0°C, and react for 5 hours, then start to release the pressure slowly. to normal pressure.

[0041] The ice bath was removed, and the temperature of the oil bath was raised to 80° C., the pressure was controlled at 1.0 MPa, and the te...

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Abstract

The invention provides a method for preparing carbonyl fluoride from p-trichloromethylphenyl isocyanate. The method is a new one in which the carbonyl fluoride is safely and effectively obtained by reacting hydrogen fluoride and phenyl isocyanate; and the method can ensure that the reaction proceeds towards the direction of generating the carbonyl fluoride maximally. The method provided by the invention comprises the following steps: in the presence of the phenyl isocyanate and the excessive hydrogen fluoride, performing a first reaction on the hydrogen fluoride and the phenyl isocyanate at a low temperature; performing heating to perform a second reaction; collecting a p-trifluoromethyl aniline product; and performing cooling to collect the liquid hydrogen fluoride, introducing the uncondensed gas into a rectification tower, performing rectification, and performing separation to obtain hydrogen chloride and the carbonyl fluoride. The method provided by the invention can ensure high reaction yield, high product purity, mild reaction conditions and favorable safety; and on the basis of producing the carbonyl fluoride, the hydrogen fluoride, the hydrogen chloride and the p-trifluoromethyl aniline can be produced simultaneously, and no pollutant is discharged, thereby meeting environmental requirements.

Description

technical field [0001] The present invention provides a method for producing carbonyl fluoride, which is a new method capable of reacting hydrogen fluoride and p-trifluoromethylphenylisocyanate to safely and effectively obtain high-purity carbonyl fluoride. Background technique [0002] Carbonyl Fluoride (COF 2 ) has been used as a substitute for a gas with a high global warming coefficient, which has been used as a cleaning gas for CVD (Chemical Vapor Deposition) equipment used in the semiconductor industry, etc., and its demand is gradually expanding. [0003] Currently about COF 2 The synthesis methods mainly include: [0004] 1. Take CO and CO 2 the method of manufacture of the raw material; [0005] 2. A synthetic method using phosgene as a raw material; [0006] 3. A production method using trifluoromethane or chlorodifluoromethane as a raw material; [0007] 4. A synthetic method using tetrafluoroethylene and oxygen as raw materials. [0008] Method 1, due to C...

Claims

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Application Information

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IPC IPC(8): C01B32/00C01B7/03C01B7/07C07C209/22C07C211/52
CPCC01B7/035C01B7/0712C07C209/22C07C211/52
Inventor 邢茂源杨雪文李飞宗现刚
Owner ZIBO FEIYUAN CHEM CO LTD
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