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Preparation method of end-capped modified perfluoroalkyl polyether

A technology of perfluoroalkyl polyether and perfluoroalkyl, which is applied in the field of preparation of end-capped modified perfluoroalkyl polyether, which can solve the problems of low foam, surface tension, and inability to synthesize addition numbers, etc., and achieve low foam High performance, excellent application performance, and the effect of less by-products

Pending Publication Date: 2022-03-08
WUHAN OXIRAN SPECIALTY CHEM CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Based on the above deficiencies in the prior art, the technical problem to be solved by the present invention is to provide a synthesis process of capped modified perfluoroalkyl polyether that only needs two-step reactions to complete, which solves the problem of common ethylene oxide adding The problem of the addition number cannot be synthesized; provide a green and efficient synthesis scheme to reduce the synthesis cost, avoid the occurrence of reaction by-products and increase the yield; achieve lower foam and surface tension by capping, and provide more than conventional perfluoroalkane Better performance of based polyether

Method used

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  • Preparation method of end-capped modified perfluoroalkyl polyether
  • Preparation method of end-capped modified perfluoroalkyl polyether
  • Preparation method of end-capped modified perfluoroalkyl polyether

Examples

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Embodiment 1

[0025] Add 0.1 mol methoxypolyoxyethylene ether (MPEG-2000) and 0.1 mol potassium methylate to a 1 L stirred tank, check the air tightness of the reactor, replace the nitrogen for 3 times and pressurize to 300KPa, and wait for the reactor to After no pressure drop occurs within 1 hour, the temperature is raised to 100°C to 50°C, vacuumed to ≤-99.0KPa or above, and the alkoxide is maintained for 5 hours, and then perfluorooctyl iodide is slowly added dropwise for 2 hours. After the dropwise addition, use 5% phosphoric acid to adjust the pH to 5.0-5.5, dehydrate and filter to get the clear liquid to remove the salt. The appearance of the product is reddish, and the surface tension of 0.1% is 30.4 dyn / cm. The cloud point is 71.7°C (5% sodium chloride aqueous solution).

Embodiment 2

[0027] Add 0.1 mol methoxypolyoxyethylene ether (MPEG-2000) and 0.1 mol potassium methylate to a 1 L stirred tank, check the air tightness of the reactor, replace the nitrogen for 3 times and pressurize to 300KPa, and wait for the reactor to After there is no pressure drop within 1 hour, the temperature is raised to 100°C, vacuumed to ≤ -99.0KPa, and the product is kept in alkoxide for 5 hours, then slowly added perfluorooctyl iodide to the product, the drop time is 1 hour, dropwise The time is 2 hours. After the dropwise addition, adjust the pH with 5% phosphoric acid, dehydrate and filter to remove salt. The product has a light yellow appearance and a 0.1% surface tension of 25.6 dyn / cm. The cloud point is 75.8°C (5% sodium chloride aqueous solution).

Embodiment 3

[0029] Add 0.1 mol methoxypolyoxyethylene ether (MPEG-2000) and 0.1 mol sodium methoxide into a 1 L stirred tank, and check the airtightness of the reactor, and wait for no pressure drop in the reactor within 1 hour Raise the temperature to 100°C, evacuate to ≤-99.0KPa or above, keep the alkoxide for 5 hours, then slowly add perfluorooctyl iodide to the product, and the addition time is 2 hours. After the dropwise addition, adjust the pH with 5% phosphoric acid, dehydrate and filter to remove salt. The product has a pale yellow appearance and a 0.1% surface tension of 32.8 dyn / cm. The cloud point is 68.4°C (5% sodium chloride aqueous solution)

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Abstract

The invention discloses a preparation method of terminated modified perfluoroalkyl polyether, which is characterized in that perfluoroalkyl halide and low-carbon-chain alkoxy alkyl polyether are synthesized by a Wi l i amson synthesis method, and in the traditional way, perfluoroalkyl alcohol and ethylene oxide are reacted, and then terminated modification is carried out. By-products such as dioxane and the like are difficult to avoid no matter which acidic catalyst is adopted, meanwhile, due to the fact that acid catalysis is only suitable for small-molecule products and cannot cope with addition with the epoxy addition number larger than or equal to 3, otherwise, side reactions can be obviously aggravated, and the yield is sharply reduced. Meanwhile, the end-capped product is alkyl end-capped foam, so that the use effect of the product is better, and the surface tension is further reduced. And in the side reaction aspect, compared with acid catalysis, the product has the advantages of high purity, low cost, high atom utilization rate and the like. The method is an excellent synthesis scheme and can be used for replacing traditional perfluoroalkyl polyether related products.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a method for preparing end-capped modified perfluoroalkyl polyether. Background technique [0002] Perfluoroalkyl polyether is a surfactant with special properties that has been gradually commercialized in recent years. Different from ordinary surfactants, it mainly uses perfluoroalkyl groups as the hydrophobic part of the surfactant, and then introduces appropriate linking groups and hydrophilic groups as required, such as the polymer formed by the polymerization of ethylene oxide. Oxyethylene ether chain segments, according to the different properties of hydrophilic groups, form a series of low-foaming and high-surface-active fluorine-containing surfactant products such as defoamers, wetting agents, and special emulsifiers. [0003] Since the structure of the fluorine-containing surfactant replaces the hydrogen atom on the carbon chain with the fluorine atom, the st...

Claims

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Application Information

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IPC IPC(8): C08G65/337
CPCC08G65/337C08G2650/04
Inventor 宋天翔王亮宋文超戴荣明梁立春李正华刘思张静任凡
Owner WUHAN OXIRAN SPECIALTY CHEM CO
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