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Fluorination method for end groups of perfluoropolyether acid

A technology of perfluoropolyether and acid end groups, which is applied in the field of fluorine chemical synthesis, can solve the problems of low fluorination conversion rate and low utilization rate of fluorinating agent gas, and achieves less by-products, safe and stable reaction, and realization of utilization rate. Effect

Active Publication Date: 2017-02-15
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD +1
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  • Abstract
  • Description
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Problems solved by technology

[0006] The purpose of the present invention is to overcome the shortcomings of batch synthesis in the prior art, low utilization rate of fluorinating agent gas, and low fluorination conversion rate, and provide a method for fluorinating perfluoropolyether

Method used

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  • Fluorination method for end groups of perfluoropolyether acid
  • Fluorination method for end groups of perfluoropolyether acid

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Embodiment 1

[0021] Fill the gas-liquid contact reaction tube with an inner diameter of 15 cm and a height of 200 cm with fillers passivated by fluorine gas with a particle size of 3 mm. The fillers in this example are carbon steel, and the temperature is controlled at 60 ° C to carry out the reaction of fluorinated perfluoropolyether acids , taking fluorine nitrogen gas with a fluorine gas content of 20% as the fluorinating agent. Hexafluorobenzene is used as a solvent, and a perfluoropolyether acid solution with a mass concentration of 50% and a weight average molecular weight of 8000 g / mol is used as a reaction solution. The fluorination experiment was carried out by controlling the mole of fluorine gas in fluorine nitrogen to be 20:1 of perfluoropolyether. Blow the fluorinating agent into the air inlet at the reaction bottom of the catalytic tube at a speed of 2L / min, and the product perfluoropolyether content collected in the product collection bottle at the lower end of the reaction ...

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Abstract

The invention belongs to the field of fluorine chemical synthesis and particularly relates to a fluorination method for end groups of perfluoropolyether acid. The perfluoropolyether acid and a fluorinating agent are taken as raw materials for synthesis in a gas-liquid contact reaction tube with fluorine gas passivated filler as a filling agent, and the filler adopts one or a mixture of carbon steel, stainless steel 304 and stainless steel 316. The perfluoropolyether acid or a solution thereof sprays downwards from the top of the gas-liquid contact reaction tube, a fluorinating agent gas makes sufficient contact with perfluoropolyether continuously from bottom to top through filler gaps in the gas-liquid contact reaction tube, maximized gas-liquid contact is realized, so that the utilization of the fluorinating agent is realized to the greatest extent, and fluorination of the perfluoropolyether is sufficient and complete. Besides, the perfluoropolyether is subjected to continuous fluorination, the problem of kettle-by-kettle fluorination in the prior art is solved, and the operation procedure is simplified. Few by-products are produced during fluorination of the perfluoropolyether, the operation is simple, continuous production can be realized, reactions are safe and stable, and the method is suitable for industrial mass production and application.

Description

technical field [0001] The invention belongs to the field of fluorine chemical synthesis, and in particular relates to a method for fluorinating end groups of perfluoropolyether acids. Background technique [0002] Perfluoropolyether and its grease are due to their excellent extreme high temperature resistance, wide operating temperature range, excellent oxidation resistance and chemical corrosion resistance, wide material compatibility, excellent electrical insulation properties, and excellent film-forming properties. , excellent load-carrying and lubricating properties, it is widely used in cutting-edge scientific fields such as military industry, aerospace and nuclear industry. [0003] No matter the preparation of perfluoropolyether acid by anionic polymerization of hexafluoropropylene oxide represented by DuPont, or the preparation of perfluoropolyether acid by photooxidation method represented by Solvay, the end groups of the generated perfluoropolyether acid are all d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/323C08G65/326C08G65/328
CPCC08G65/3236C08G65/326C08G65/328
Inventor 肖鑫贺光瑞赵兴华耿谦张志君
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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