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Preparation method for perfluoroalkyl diacyl fluoride

A technology for crude products of perfluoroalkyl diacyl and alkyl diacyl fluoride, which is applied in the preparation of organic compounds, preparation of carboxylate, chemical instruments and methods, etc., can solve the problems of high price of antimony pentafluoride, and achieve suitable Large-scale production, simple preparation steps, and easy-to-obtain reagents

Inactive Publication Date: 2019-05-14
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0027] DuPont reported the use of antimony pentafluoride to convert perfluoropropionyl fluoride methyl ester to perfluoromalonyl fluoride. The raw material antimony pentafluoride is expensive and only suitable for laboratory research

Method used

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  • Preparation method for perfluoroalkyl diacyl fluoride
  • Preparation method for perfluoroalkyl diacyl fluoride
  • Preparation method for perfluoroalkyl diacyl fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The preparation steps of perfluoromalonyl fluoride are as follows:

[0046] (1) Add 300 milliliters of benzonitrile and 50 grams of potassium fluoride in a 1-liter reactor, and slowly drop in 40 grams of malonyl chloride, then react at 10°C and the reaction pressure is normal pressure, after 8 hours of reaction The reaction system was naturally returned to room temperature, and then separated to obtain 30 grams of crude malonyl fluoride;

[0047] (2) Add the crude malonyl chloride directly to an anhydrous hydrogen fluoride electrolyzer (Simon electrolyzer) for electrolysis, and use a low-temperature cold trap at -80°C to collect the gas generated by the electrolysis to obtain the crude perfluoromalonyl fluoride; , the temperature of electrolyte is 0~5 ℃, and electrode voltage is 5.5 volts, and the quality of malonyl chloride crude product is 5% of anhydrous hydrofluoric acid quality;

[0048] (3) Rectifying the crude perfluoromalonyl fluoride to obtain 16 grams of perf...

Embodiment 2

[0054] The preparation steps of perfluorosuccinyl fluoride are as follows:

[0055] (1) Add 300 milliliters of diethylene glycol dimethyl ether, 50 grams of Potassium Fluoride in a 1-liter reactor, then slowly drop in 61 grams of succinoyl chloride, then react at 10°C and the reaction pressure is normal pressure, After reacting for 12 hours, the reaction system was naturally returned to room temperature, and then separated to obtain the crude product of succinyl fluoride;

[0056] (2) Add the crude product of succinyl fluoride directly to an anhydrous hydrogen fluoride electrolytic cell for electrolysis, and use a low-temperature cold trap at -80°C to collect the gas generated by electrolysis to obtain the crude product of perfluorosuccinyl fluoride; wherein, the electrolyte The temperature is 0~5℃, the electrode voltage is 5 volts, and the quality of the crude product of succinyl chloride is 3% of the quality of anhydrous hydrofluoric acid;

[0057] (3) Rectifying the crude ...

Embodiment 3

[0063] The preparation steps of perfluoroglutaryl fluoride are as follows:

[0064] (1) Add 300 milliliters of tetrahydrofuran and 70 grams of cesium fluoride into a 1-liter reactor, then slowly drop in 24 grams of glutaryl chloride, then react at 20° C. and the reaction pressure is normal pressure, and make the reaction after 12 hours. The system naturally returned to room temperature, and then separated to obtain the crude product of glutaryl fluoride;

[0065] (2) Directly add the crude product of glutaryl fluoride to an anhydrous hydrogen fluoride electrolyzer for electrolysis, and use a low-temperature cold trap at -80°C to collect the gas generated by electrolysis to obtain the crude product of perfluoroglutaryl fluoride; wherein, the The temperature is 0-5°C, the electrode voltage is 5.3 volts, and the mass of glutaryl fluoride crude product is 8% of the mass of anhydrous hydrofluoric acid;

[0066] (3) Rectifying the crude perfluoroglutaryl fluoride to obtain 42 grams...

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Abstract

The invention relates to a preparation method for perfluoroalkyl diacyl fluoride, and belongs to the technical field of the fine fluorine chemical industry. The method comprises the following steps: using alkyl diacyl chloride as a raw material, firstly reacting with a fluridizer in a catalytic solvent and generating the alkyl diacyl chloride, and electrolyzing and fluorinating through an anhydrous hydrogen fluoride electrolyzer, to obtain the perfluoroalkyl diacyl fluoride, finally rectifying and purifying. A reagent used by the method is simple and easily obtained. A preparation process is simple and safe. Reaction time is short. The method is suitable for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of perfluoroalkyl bisacyl fluoride, which belongs to the technical field of fine fluorine chemical industry. Background technique [0002] Perfluoroalkyl bisacyl fluoride (general formula is FOC(CF 2 ) n COF) is an important compound for the synthesis of perfluorovinyl ether, bifunctional perfluoropolyether and bifunctional fluorine-containing polyurethane / polyamide monomers. Synthesizing high-performance functional fluorine-containing polymer materials from it is the current science of fluorine-containing materials. one of the research topics. Using perfluoroalkyl bisacyl fluoride as raw material can be used to prepare perfluorovinyl ether monomer Cytop and tetrafluoroethylene to copolymerize into amorphous optically transparent polymer, perfluorocarboxylic acid ion exchange resin, perfluoroether rubber, etc. . These polymers have unique chemical stability, corrosion resistance, flame retardancy, hydro...

Claims

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Application Information

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IPC IPC(8): C25B3/08C07C51/62C07C55/36C25B3/28
Inventor 耿谦刘智慧马毅斌李翔宇吕灵华曹红梅王振宇沙婷
Owner PERIC SPECIAL GASES CO LTD
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