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A kind of alternate copolymerization method for preparing fluoropolymer based on dibromo compound and diene monomer

A double-brominated compound and alternating copolymerization technology is applied in the field of alternating copolymerization of fluorine-containing polymers prepared based on double-brominated compounds and diene monomers, and achieves the effects of expanding the scope of application, high practical application value, and high research value.

Active Publication Date: 2019-06-25
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, whether it is a regular fluorine-containing functional polymer or a common functional polymer, there are very few reports on the preparation of brush-like polymers by graft polymerization.

Method used

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  • A kind of alternate copolymerization method for preparing fluoropolymer based on dibromo compound and diene monomer
  • A kind of alternate copolymerization method for preparing fluoropolymer based on dibromo compound and diene monomer
  • A kind of alternate copolymerization method for preparing fluoropolymer based on dibromo compound and diene monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Alternate Copolymerization of Dibromo Compounds and Non-conjugated Dienes via Free Radical Stepwise Transfer-Addition-Termination Polymerization in Mixed Solvent System of Dimethyl Carbonate and Acetonitrile

[0032] according to n A1 :n B1 :n fac-Ir(ppy)3 :n TBABr = 100:100:2:50 initial molar ratio, difunctional monomer A1 (1,8-dibromohexadecafluorooctane) (0.2799 g, 0.5 mmol), B1 (1,7-octadiene) (74.0 μL, 0.5 mmol), fac -Ir(ppy) 3(6.6 mg, 0.01mmol), TBABr (80.6 mg, 0.25 mmol) was added to the mixed solvent system of acetonitrile and dimethyl carbonate (V 乙腈 :V 碳酸二甲酯 =1:3), add a stirring bar, and seal the tube directly after four deoxygenation operations. Then transfer the ampoule to a magnetic stirrer with a set speed (1500 rpm) and carry out photopolymerization at room temperature under LED blue light illumination. After reaching the given time (20 h), take out and open the airtight container, and use the polymerization system to Tetrahydrofuran was dilute...

Embodiment 2

[0034] Influence of different bases as accelerators on the stepwise transfer-addition-termination polymerization of dibromo compounds and non-conjugated diene radicals in a mixed solvent system of dimethyl carbonate and acetonitrile

[0035] because fac -Ir(ppy) 3 Compared to Ru(bpy) 3 Cl 2 It has more excellent redox stability and longer excited state lifetime, so we first locked the metal photocatalyst as fac -Ir(ppy) 3 . Through literature research, we can know that the addition of alkali compounds will affect the excitation potential when the photocatalyst forms an excited state. Therefore, we add various base compounds to the current polymerization system to investigate the effect of base compounds as accelerators on the gradual transfer-addition-termination of polymerization of dibromo compounds and non-conjugated diene radicals. The results are shown in the following table 1.

[0036] Table 1. Effects of different bases on the stepwise transfer-addition-termina...

Embodiment 3

[0041] In the mixed solvent system of dimethyl carbonate and acetonitrile, the effects of different Lewis acids as accelerators on the stepwise transfer-addition-termination polymerization of dibromo compounds and non-conjugated diene radicals were investigated

[0042] In addition to regulating metal photocatalysts by adding base compounds fac -Ir(ppy) 3 In addition to the excited state redox potential, we also tried to add various Lewis acids to the system to build an oxidation catalytic cycle system to improve the polymerization efficiency. The specific results are shown in Table 2 below.

[0043] Table 2. Effects of different Lewis acids on the stepwise transfer-addition-termination polymerization of dibromocompounds and non-conjugated diene radicals

[0044]

[0045] Polymerization conditions: solution polymerization was carried out under room temperature LED blue light illumination conditions. The feeding ratio is [A1] 0 :[B1] 0 :[ fac -Ir(ppy) 3 ] 0 :[Accele...

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Abstract

The invention provides an alternating copolymerization method for preparing a fluoropolymer on the basis of a dibromide compound and a diene monomer. The alternating copolymerization method comprisesthe following steps: (1), adding two types of bifunctional monomers A and B, a metal photocatalyst and a promoter into a mixed organic solvent system, homogenizing the system by stirring in a reactioncontainer, performing deoxidizing operations for four times, and sealing the reaction container; (2), performing a polymerization reaction through photocatalysis; (3), after the reaction, adding tetrahydrofuran to dilute a polymerization system, pouring into methanol for precipitation, performing suction filtration and drying to obtain a needed alternating polymer. A perfluorodiiodide monomer isexpanded to a perfluorodibromide monomer and a common alkane dibromide compound, so that the application range of the monomers for the gradual transfer of free radicals, addition and termination polymerization is further expanded; moreover, the capability of the polymerization method in designing the microstructures of functional high molecular materials is also improved, and more selectivity is provided for obtaining functional polymers with different microstructures.

Description

technical field [0001] The invention relates to the technical field of sequence controllable polymerization, and relates to the extension of a bifunctional monomer in the existing free radical stepwise transfer-addition-termination polymerization report from perfluorodiiodide monomer to perfluorodibromine and common alkane A dibromine-like monomer realizes the alternate copolymerization of a dibromine compound and a non-conjugated diene, and specifically relates to an alternate copolymerization method for preparing a fluorine-containing polymer based on a dibromine compound and a diene monomer. Background technique [0002] Functional polymers with regular structures have always been a hot spot in the field of polymer science research. In fluorine chemistry, semifluoropolyolefin is a unique class of fluorine-containing polymer materials. Due to the strict alternating structure of perfluorinated segments and alkane segments in the polymer chain, it has been widely used since ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G61/04C08G61/02C08G61/12
Inventor 程振平徐天驰张丽芬朱秀林
Owner SUZHOU UNIV
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