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A kind of preparation method of carbonyl fluoride

A technology for carbonyl fluoride and carbonyl fluoride products is applied in the field of preparation of carbonyl fluoride, which can solve the problems of difficult industrialized production, low electrolysis efficiency, uneconomical operation, etc., and achieves uniform concentration of reactants, long operation period, and equipment investment. less effect

Active Publication Date: 2020-10-30
ZHEJIANG JUSHENG FLUOROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest feature of this method is the use of a porous fluorinated resin-based bubble generator, through which CO is dispersed into tiny bubbles and blown into anhydrous hydrofluoric acid liquid, which determines whether the method is effective or not, the process It is more complicated and uses CO dangerous medium. In the electrolysis process, sodium fluoride, an electrolytic additive, is added to promote dissolution. The addition of sodium fluoride, an electrolytic additive, will cause rapid corrosion of the plate; and this method is gas phase feeding, The efficiency of electrolysis is relatively low, the actual operation is uneconomical, and it is difficult to industrialize production

Method used

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  • A kind of preparation method of carbonyl fluoride

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Effect test

Embodiment 1

[0034] (1) Add 15kg of methanol and 85kg of AHF into the electrolyte preparation tank respectively, stir at 5°C and 50rpm for 30min to obtain the electrolyte, and set aside;

[0035] (2) Put the electrolyte obtained in step (1) into the water removal tank for electrolytic dehydration. The initial current of electrolytic dehydration is 10A. After electrolytic dehydration starts, the current is increased at a rate of 10A / 2h. When the current reaches 60A When the electrolytic dehydration is finished, the electrolyte solution after dehydration is obtained for subsequent use;

[0036] (3) The dewatered electrolyte solution obtained in step (2) is continuously added to the electrolytic cell (the anode material is 6# nickel, and the cathode material is carbon steel), and the electrolytic fluorination reaction is carried out at a temperature of 19°C under normal pressure , the electrolysis voltage is controlled to be 6V, the working current is 70A, the gas phase product obtained by elec...

Embodiment 2

[0040] (1) Add 10kg of methanol and 90kg of AHF into the electrolyte preparation tank respectively, stir at 15°C and 80rpm for 5min to obtain the electrolyte, and set aside;

[0041] (2) Put the electrolyte obtained in step (1) into the water removal tank for electrolytic dehydration. The initial current of electrolytic dehydration is 10A. After electrolytic dehydration starts, the current is increased at a rate of 5A / 2h. When the current reaches 50A When the electrolytic dehydration is finished, the electrolyte solution after dehydration is obtained for subsequent use;

[0042] (3) The electrolyte obtained in step (2) after water removal is continuously added to the electrolytic cell (the anode material is 6# nickel, and the cathode material is carbon steel), and the electrolytic fluorination reaction is carried out at a temperature of 20 ° C and normal pressure , control the electrolysis voltage at 5V, working current 60A, the gas phase product obtained by electrolysis is co...

Embodiment 3

[0046] (1) Add 20kg of methanol and 80kg of AHF into the electrolyte preparation tank respectively, stir at 10°C and 70rpm for 10min to obtain the electrolyte, and set aside;

[0047] (2) Put the electrolyte obtained in step (1) into the water removal tank for electrolytic dehydration. The initial current of electrolytic dehydration is 8A. After electrolytic dehydration starts, the current is increased at a rate of 7A / 2h. When the current reaches 52A When the electrolytic dehydration is finished, the electrolyte solution after dehydration is obtained for subsequent use;

[0048] (3) The electrolyte obtained in step (2) after water removal is continuously added to the electrolytic cell (the anode material is 6# nickel, and the cathode material is carbon steel), and the electrolytic fluorination reaction is carried out at a temperature of 15°C under normal pressure , the electrolysis voltage is controlled at 7V, the working current is 30A, the gas phase product obtained by elect...

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Abstract

The invention discloses a carbonyl fluoride preparing method. The carbonyl fluoride preparing method comprises the following steps that firstly, by weight, methyl alcohol and anhydrous hydrogen fluoride are prepared into an electrolyte to be used later; secondly, the electrolyte is subjected to electrolysis water removal to be used later; and thirdly, the electrolyte obtained after water removal is continuously added into an electrolytic cell, the electrolysis fluorination reaction is conducted, a gas phase product obtained through electrolysis is subjected to condensation, and the carbonyl fluoride product is obtained. The carbonyl fluoride preparing method has the advantages that the technology is simple, cost is low, the current efficiency is high, the running period is long, and the product quality is stable.

Description

technical field [0001] The invention relates to the technical field of acid fluorides, in particular to a preparation method of carbonyl fluoride. Background technique [0002] Carbonyl fluoride is also known as carbonyl fluoride, fluorophosgene, molecular formula: CF 2 O, structural formula: F 2 C=O, molecular mass: 66.01, boiling point: -84.5°C, relative density at 20°C / 101.325kpa is 2.29, irritating, non-flammable, colorless and toxic gas at normal temperature and pressure, soluble in water and ethanol, Rapidly hydrolyzes with water to release HF and CO 2 , and generate smoke. COF 2 It can fluorinate carbonyl compounds, react with perfluoroalkenes in the presence of metal fluorides to generate perfluoroacyl fluorides, and react with alcohols and amines to generate esters and fluorocarbonic acid amides, respectively. COF 2 It can be decomposed into CF when heated above 300°C 4 and CO 2 . Dry COF 2 It has no corrosive effect on metals, but it is very corrosive whe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/24
CPCC25B1/245
Inventor 朱洪吉余考明陈伟峰叶智萍范稳李彬
Owner ZHEJIANG JUSHENG FLUOROCHEM