Method for preparing fluorine-containing nonionic surfactant

A non-ionic surface and active agent technology, applied in chemical instruments and methods, transportation and packaging, dissolution, etc., can solve the problems of unavailable raw materials, safety risks, high temperature and high pressure of reaction conditions, etc., and achieve process controllability and reaction conditions Gentle, high-yield effect

Active Publication Date: 2017-06-13
济南齐氟新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the above existing problems in the prior art in the preparation of fluorine-containing nonionic surfactants, the raw materials are not easy to obtain, the reaction conditions are high temperature and high pressure, and there are safety risks. Preparation method of high-efficiency fluorine-containing nonionic surfactant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Under the protection of nitrogen, add 153 grams (0.28 mol) of perfluorooctyl iodide and 1.15 grams of di-tert-butyl peroxide into a 500 ml four-neck flask equipped with stirring, thermometer, constant pressure dropping funnel and condenser, and stir gradually The temperature was raised to 140° C., and 115 g (0.273 mol) of vinyl polyoxyethylene ether with an average molecular weight of about 420 was slowly added dropwise. After the addition, 0.4 g of di-tert-butyl peroxide was added, and the temperature was maintained at 140-150° C. for 3 hours. Heating was stopped, the negative pressure was -0.07MPa, simple distillation was carried out, and the temperature was lowered to obtain 255 grams of dark yellow viscous liquid with a yield of 96.2%.

Embodiment 2

[0024] Under the protection of nitrogen, add 200 grams (0.35 mol) of perfluoroalkyl iodide and 1.5 grams of di-tert-butyl peroxide into a 1000 ml four-necked flask equipped with stirring, thermometer, constant pressure dropping funnel and condenser, and stir gradually The temperature was raised to 140° C., and 215 g (0.34 mol) of allyl polyoxyethylene ether with an average molecular weight of about 630 was slowly added dropwise. After the addition, 0.5 g of di-tert-butyl peroxide was added, and the temperature was maintained at 140-150° C. for 4 hours. Heating was stopped, the negative pressure was -0.08MPa, simple distillation was carried out, and the temperature was lowered to obtain 388 grams of dark yellow viscous liquid, with a yield of 94.8%.

Embodiment 3

[0026] Under the protection of nitrogen, add 161 grams (0.36 mol) of perfluorohexyl iodide and 1.2 grams of benzoyl peroxide into a 500 ml four-neck flask equipped with stirring, thermometer, constant pressure dropping funnel and condenser, and gradually raise the temperature to 75 °C, 78 g (0.354 mol) of vinyl polyoxyethylene ether with an average molecular weight of about 220 was slowly added dropwise. After the addition, 0.4 g of benzoyl peroxide was added, and the temperature was maintained at 75-85° C. for 3 hours. Heating was stopped, the negative pressure was -0.07MPa, simple distillation was carried out, and 220 grams of yellow viscous liquid was obtained by cooling. Yield 93.2%.

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PUM

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Abstract

The invention relates to the technical field of fluorine-containing nonionic surfactants and in particular relates to a method for preparing a fluorine-containing nonionic surfactant. The preparation method comprises the following steps: reacting perfluoroalkyl iodides with polyoxyethylene ethers containing vinyl or allyl, removing light components from the obtained products, thereby obtaining the nonionic surfactant. The preparation method disclosed by the invention is readily available in raw materials, mild and safe in reaction conditions, easily controllable in process and high in yield, and the yield reaches 93% or higher.

Description

technical field [0001] The invention relates to the technical field of fluorine-containing nonionic surfactants, in particular to a preparation method of fluorine-containing nonionic surfactants. Background technique [0002] Fluorine-containing nonionic surfactants can greatly reduce the surface tension of aqueous solutions at very low dosages, and are widely used. For example, it can be used as lubricant and softener in various chemical industries. It is especially important to be used as a dispersant, leveling agent, and antifouling agent in water-based inks and coatings, and to be used on various low surface energy materials. It can also be used as a release agent in plastics, rubber and other industries. [0003] Relevant patents at home and abroad have introduced it, all of which use perfluoroalkyl alcohol as the initial raw material, and react with ethylene oxide under the action of a catalyst to obtain the product: [0004] R f CH 2 CH 2 OH + n CH 2 CH 2 ...

Claims

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Application Information

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IPC IPC(8): C08G65/337B01F17/42C09K23/42
CPCC08G65/337C09K23/007
Inventor 张立亭
Owner 济南齐氟新材料技术有限公司
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