Full-fluorine octyl sulfuryl fluoride production technology

A technology of perfluorooctanesulfonyl fluoride and fluorooctanesulfonyl fluoride, which is applied in the field of perfluorooctanesulfonyl sulfonyl fluoride production technology, can solve the problem that there is no public report on the chemical synthesis production method and process of perfluorooctanesulfonyl fluoride, The continuous electrolysis time and life of the plate are shortened, and the equipment utilization rate is low, and the continuous electrolysis time is extended, the equipment utilization rate is improved, and the production efficiency is improved.

Inactive Publication Date: 2009-05-13
湖北恒新化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect of the original electrolysis process is that the efficiency of single tank is low and the utilization rate of equipment is low
Moreover, when the solubility of organic matter in hydrogen fluoride is small, it is necessary to add fluoride salts such as NaF or KF as supporting electrolytes, and these fluoride salts are usually very corrosive, and the continuous electrolysis time and life of the plate will be greatly shortened
In addition, relevant domestic and foreign literatures have some reports on the production research of other organic fluorine products, but there is no public report on the production method and process of the chemical synthesis of perfluorooctyl sulfonyl fluoride.

Method used

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  • Full-fluorine octyl sulfuryl fluoride production technology
  • Full-fluorine octyl sulfuryl fluoride production technology
  • Full-fluorine octyl sulfuryl fluoride production technology

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Experimental program
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Embodiment

[0021] The present invention uses bromooctane as a raw material, first undergoes sulfonation, and the reaction equation is as follows:

[0022]

[0023] Use alcohol as a solvent, control the reaction temperature between 80°C and 90°C, and react for 18 hours. When there is no oil flower-like liquid in the reaction tube, the reaction ends. The alcohol in the reaction residue is recovered and reused.

[0024] The product obtained by sulfonation is fully dried and sent to the chlorination section for chlorination.

[0025] The chlorination kettle needs to be cleaned and fully dried. Weigh the octyl sulfonate which is the reaction product of the first step, put phosphorus oxychloride into the reactor, start stirring, then add the weighed sulfonate into the reactor. The reaction equation for this step is:

[0026]

[0027] Keep the temperature of the kettle at 70° C. to 75° C. for 6 hours, and the reaction is basically completed. Wait until the temperature in the kettle dr...

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PUM

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Abstract

The invention relates to a production method for organic fluorine, in particular to a production process for perfluorooctane sulfonyl fluoride. The method comprises the following steps: (1) taking bromooctane as raw material, taking alcohol as solvent, and carrying out sulphonation through Na2SO3 to obtain CH3(CH2)7SO3Na; (2) chloridizing CH3(CH2)7SO3Na through phosphorus oxychloride to obtain CH3(CH2)7SO2Cl; (3) fluorinating CH3(CH2)7SO2Cl with triethanolamine as a catalyst to obtain CH3(CH2)7SO2F; (4) distilling CH3(CH2)7SO2F, collecting distillate within the temperature range from 110 DEG C to 120 DEG C to obtain high-purity octane sulfonyl fluoride; and (5) electrolyzing the high-purity octane sulfonyl fluoride to obtain perfluorooctane sulfonyl fluoride. The production method has the advantages of simple process and high yield.

Description

technical field [0001] The invention relates to a production method of organic fluorine, in particular to a production process of perfluorooctyl sulfonyl fluoride. Background technique [0002] Organic fluorine products are widely used in the field of fine chemicals due to their excellent performance. Before the 1940s, fluorination methods were limited to elemental fluorination. However, this method is extremely demanding on the reaction conditions, and usually needs to be carried out below -60°C. In 1941, J.H.Simons first carried out electrochemical fluorination. Due to confidentiality reasons, this method was not disclosed until 1949 by applying for a patent. Electrochemical fluorination enables the fluorination reaction to be carried out under relatively mild conditions. In 1946, 3M Company of the United States began to apply the Simons method to industry, and in 1952, batches were realized. At present, 3M is still in the leading position in the world in the research a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/08C07C309/80C07C303/02C25B3/28
Inventor 李书涛高伟
Owner 湖北恒新化工有限公司
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