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Process for the preparation of unsaturated fluoropolymers

A polymer and unsaturated technology, which is applied in the field of preparation of unsaturated fluoropolymers, can solve the problems of difficulty in controlling the content of unsaturated bonds in the product, removal of alkali and phase transfer catalyst, etc., and achieves fast reaction, shortened reaction time, low cost effect

Active Publication Date: 2019-09-06
DALIAN MARITIME UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process does not use organic solvents, under the action of excessive alkaline reagents and high temperatures, side reactions have occurred: (1) fluoropolymer chain cracking reaction and degradation, (2) a large number of alkalis produce hydroxyl groups, (3) Carboxyl groups are generated by peroxidation; the unsaturated bond content of the modified product is difficult to control, and the residual alkali and phase transfer catalyst cannot be simply removed from the product
Up to now, there is no report on the preparation method of unsaturated fluoropolymers at home and abroad

Method used

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  • Process for the preparation of unsaturated fluoropolymers
  • Process for the preparation of unsaturated fluoropolymers
  • Process for the preparation of unsaturated fluoropolymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 10 g of fluoropolymer (vinylidene fluoride-hexafluoropropylene copolymer) in 100 mL of ethyl acetate, and place it in a 500 mL one-necked flask. Add phase transfer catalyst trioctylmethylammonium chloride (0.25g) successively, add 5wt% potassium hydroxide aqueous solution 150g, react under 400KW microwave for 120 minutes. After the reaction, the system was separated for 10 minutes, the upper organic phase was extracted, and purified by adding n-hexane, the solvent was rotary evaporated, and the product was vacuum-dried at 55-70° C. for 24 hours. The product was subjected to infrared spectroscopy (FTIR), NMR ( 19 F-NMR, CFCl 3 as standard) and chlorine iodine method double bond content is tested and quantitatively analyzed: 19 The calculation result of the characteristic peak of the unsaturated double bond by F-NMR is 1.94 mol%, and the calculation result of the double bond titration is 0.19 mmol / g.

Embodiment 2-4

[0033] Carry out preparation, test, calculation method according to embodiment 1, the difference is the difference in the amount of phase transfer catalyst trioctylmethyl ammonium chloride, the specific results are shown in table 1.

[0034] Table 1

[0035]

Embodiment 5-7

[0037] The preparation, testing and calculation methods were carried out according to Example 1, with the difference that the amount of organic solvent used was 100-120 ml, and the specific results are shown in Table 2.

[0038] Table 2

[0039]

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Abstract

The invention discloses a method for preparing an unsaturated fluorine-containing polymer. A fluorine-containing polymer is adopted as a raw material and dissolved in an organic solvent, the mixture can be placed in a variable-frequency microwave tester to be subjected to a one-pot reaction of Hofmann and Zaitsev under the action of alkali or alkali and a small amount of catalyst, and the content-controllable fluorine-containing polymer with high unsaturated bond content can be obtained within a short time. The method has the advantages that the process is simple, reacting is fast, cost is low, the reaction solvent can be recycled, the yield is 95% or above, and strict pollution control measures are not needed. The product is wide in application range, and can be applied as an intermediate, a processing compounding agent and the like of the functional fluorine-containing polymer.

Description

technical field [0001] The present invention relates to a process for the preparation of unsaturated fluoropolymers. Background technique [0002] Fluoropolymers have been widely used in different fields and industries because of their excellent properties. As an important intermediate and processing compounding agent in the fluorine-containing material preparation industry, unsaturated fluorine-containing polymers have broad market prospects and important application values. [0003] At present, 3M Corporation and Dow Corning Corporation of the United States are mainly engaged in the research and development of unsaturated fluoropolymers in the world. There are many side reactions, complex post-treatment process, serious pollution and other shortcomings, but large-scale production has not been realized. Among them, the preparation method invented by 3M Company of the United States is to directly add fluoropolymer, excess solid base and phase transfer catalyst into the ext...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/26C08F214/22
Inventor 廖明义李东翰
Owner DALIAN MARITIME UNIVERSITY