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Preparation method of block copolymer containing perfluoro-2, 2-dimethyl-1, 3-dioxole

A dioxole and block copolymer technology, applied in chemical engineering and fields, can solve problems such as unreported, achieve the effect of promoting separation, ensure effective oxygen-promoting transport efficiency, and increase oxygen selective permeability. Effect

Active Publication Date: 2019-09-17
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For fluorine-containing monomers, the most efficient living free radical polymerization method is iodine transfer polymerization, but iodine transfer polymerization is used to prepare perfluoro-2,2-dimethyl-1,3-dioxole-co -Tetrafluoroethylene copolymer and further preparation of block copolymers composed of it and polymers containing imidazole or pyridine groups have not been reported

Method used

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  • Preparation method of block copolymer containing perfluoro-2, 2-dimethyl-1, 3-dioxole
  • Preparation method of block copolymer containing perfluoro-2, 2-dimethyl-1, 3-dioxole

Examples

Experimental program
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Effect test

Embodiment 1

[0025]Add 100 grams of perfluoroheptane, 0.120 grams of diisopropyl peroxydicarbonate, and 0.062 grams of perfluoroiodobutane into the reaction kettle, seal the nitrogen and discharge oxygen until the oxygen concentration is less than 5ppm, and stir evenly; mix 20 grams of Perfluoro-2,2-dimethyl-1,3-dioxole and tetrafluoroethylene monomers (perfluoro-2,2-dimethyl-1,3-dioxole and tetrafluoroethylene The mass ratio of vinyl fluoride is 16.54:1) into the reaction kettle, stir evenly and heat up to 57°C, polymerize for 5 hours, cool to room temperature, remove unreacted tetrafluoroethylene monomer, and obtain iodine-terminated active poly(perfluoroethylene -2,2-Dimethyl-1,3-dioxole-co-tetrafluoroethylene) solution. To the resulting activated poly(perfluoro-2,2-dimethyl-1,3-dioxol-co-tetrafluoroethylene) solution was added 0.008 g of 1-vinyl cobalt complexable porphyrin imidazole, stir and heat up to 57°C, continue to polymerize for 4 hours, then cool to room temperature, the prod...

Embodiment 2

[0030] 100 grams of trifluorotrichloroethane / perfluoroheptane (perfluoroheptane: 30 wt%), 0.123 grams of diisopropyl peroxydicarbonate, and 0.236 grams of perfluoroiodohexane were added to the reaction kettle, and the Nitrogen exhausting oxygen until the oxygen concentration is less than 5ppm, stirring evenly; 20 grams of perfluoro 2,2-dimethyl-1,3-dioxole and tetrafluoroethylene monomer (perfluoro-2,2-di The mass ratio of methyl-1,3-dioxole to tetrafluoroethylene is 5.29:1) into the reaction kettle, stir evenly and heat up to 57°C, polymerize for 6 hours, cool to room temperature, and remove unreacted Tetrafluoroethylene monomer to obtain a solution of iodine-terminated living poly(perfluoro-2,2-dimethyl-1,3-dioxole-co-tetrafluoroethylene). To the resulting activated poly(perfluoro-2,2-dimethyl-1,3-dioxol-co-tetrafluoroethylene) solution was added 0.558 g of 4-vinyl cobalt complexable porphyrin Pyridine, stirred and raised to 57°C reaction setting temperature to continue pol...

Embodiment 3

[0035] 100 grams of trifluorotrichloroethane / perfluoro(2-n-butyltetrahydrofuran) (perfluoro(2-n-butyltetrahydrofuran): 30wt%), 0.123 grams of α-cumyl peroxyneodecanoate, Add 0.412 grams of 1,4-diiodoperfluorobutane into the reaction kettle, seal the nitrogen and discharge oxygen until the oxygen concentration is less than 5ppm, and stir evenly; add 20 grams of perfluoro 2,2-dimethyl-1,3-di Oxole and tetrafluoroethylene monomers (the mass ratio of perfluoro-2,2-dimethyl-1,3-dioxole to tetrafluoroethylene is 26.78:1) are added to the reactor , stir evenly and heat up to 50°C, polymerize for 6 hours, cool to room temperature, remove unreacted tetrafluoroethylene monomer, and obtain iodine-terminated active poly(perfluoro-2,2-dimethyl-1,3-diox Heterocyclopentene-co-tetrafluoroethylene) solution. To the resulting activated poly(perfluoro-2,2-dimethyl-1,3-dioxol-co-tetrafluoroethylene) solution was added 0.605 g of 4-butene that can complex cobalt porphyrin Pyridine, stir and heat...

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Abstract

The invention discloses a preparation method of a block copolymer containing perfluoro-2, 2-dimethyl-1, 3-dioxole. The preparation method comprises the steps of fully and evenly mixing an initiator, a chain transfer agent and a solvent according to a proportion, then adding the perfluoro-2, 2-dimethyl-1, 3-dioxole and a tetrafluoroethylene monomer according to a proportion, and carrying out an iodine transfer active free-radical polymerization reaction to obtain active poly(perfluoro-2, 2-dimethyl-1, 3-dioxole-co-tetrafluoroethylene); then, adding a vinyl monomer, which can be complexed with cobalt porphyrin, for polymerizing so as to obtain the block copolymer. The preparation method provided by the invention is simple in process, and the molecular weight and composition of the block copolymer are convenient to adjust and control. The block copolymer can be used for preparing a polymer separation film which is complexed with cobalt porphyrin and is not suitable for swelling in an organic solvent, and the polymer separation film is used for specific selective separation of organic gas and oxygen.

Description

technical field [0001] The invention belongs to the field of chemical engineering and technology, and in particular relates to a preparation method of a block copolymer containing perfluoro-2,2-dimethyl-1,3-dioxole. Background technique [0002] Poly(perfluoro-2,2-dimethyl- 1,3-Dioxole-co-tetrafluoroethylene) (P(PDD-co-TFE)) is a high-performance fluoropolymer, which has similar heat resistance to other fluoropolymers In addition to the advantages of chemical corrosion resistance, it also has the characteristics of high light transmittance, low refractive index, low dielectric constant, high glass transition temperature and free volume fraction, and high gas permeability. It has good application with separation membrane. [0003] Poly(perfluoro-2,2-dimethyl-1,3-dioxole-co-tetrafluoroethylene) is currently mainly produced by DuPont Company of the United States, the trade name is Telfon AF, and according to the PDD of the copolymer Content and molecular weight are divided i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F234/02C08F214/26C08F226/06
CPCC08F214/26C08F226/06C08F234/02C08F293/005
Inventor 余大洋包永忠陈振华邵春明王树华
Owner ZHEJIANG UNIV
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