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Polymerization method for preparing fluorine-containing alternating copolymer through gradual transfer-addition-ending step by step with free radicals under condition of visible light

A technology of alternating copolymers and polymerization methods, applied in the field of controlled sequence polymerization, can solve the problems of low polymer molecular weight, low monomer conversion rate, long polymerization reaction time, etc.

Active Publication Date: 2016-04-13
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved: Aiming at the disadvantages of long polymerization reaction time, low monomer conversion rate and low polymer molecular weight in the existing polymerization method, the present invention provides a method of using free radicals to gradually transfer-addition- Polymerization process for terminating the preparation of fluorine-containing alternating copolymers

Method used

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  • Polymerization method for preparing fluorine-containing alternating copolymer through gradual transfer-addition-ending step by step with free radicals under condition of visible light
  • Polymerization method for preparing fluorine-containing alternating copolymer through gradual transfer-addition-ending step by step with free radicals under condition of visible light
  • Polymerization method for preparing fluorine-containing alternating copolymer through gradual transfer-addition-ending step by step with free radicals under condition of visible light

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Embodiment 1

[0028] A polymerization method for preparing fluorine-containing alternating copolymers by using free radicals to gradually transfer-addition-terminate under visible light conditions. The preparation steps of the method are as follows:

[0029] (1) Mix 0.5mmol of 1,8-diiodoperfluorooctane, 0.5mmol of 1,4-bis(allyloxy)benzene, 0.025mmol of Ru(bpy) 3 Cl 2 , 0.175mmol of sodium ascorbate, and a mixed organic solvent composed of 3mL of acetonitrile and 1mL of methanol are all added to the reaction vessel, and a stirrer is added to the reactor, stirred to make the system homogeneous, and sealed after four deoxygenation operations Reaction vessel, obtains homogeneous polymerization system I;

[0030] (2) Set the temperature of the reaction vessel at 25°C and the rotation speed at 1800rpm, and conduct the polymerization reaction of the homogeneous polymerization system I under LED blue light illumination, and the reaction time is 24h;

[0031] (3) After the reaction, open the react...

Embodiment 2

[0033] A polymerization method for preparing fluorine-containing alternating copolymers by using free radicals to gradually transfer-addition-terminate under visible light conditions. The preparation steps of the method are as follows:

[0034] (1) Mix 0.5mmol of 1,8-diiodoperfluorooctane, 0.5mmol of 1,4-bis(enylbutyl)benzene, and 0.025mmol of Ru(bpy) 3 Cl 2 , 0.175mmol of sodium ascorbate, and a mixed organic solvent composed of 3mL of 1,4-dioxane and 1mL of methanol were all added to the reaction vessel, and a stirring bar was added to the reactor, and the system was stirred to make the system homogeneous. After the second deoxygenation operation, the reaction vessel is sealed to obtain the homogeneous polymerization system I;

[0035] (2) Set the temperature of the reaction vessel at 25°C and the rotation speed at 1800rpm, and conduct the polymerization reaction of the homogeneous polymerization system I under LED blue light illumination, and the reaction time is 24h;

[...

Embodiment 3

[0038] A polymerization method for preparing fluorine-containing alternating copolymers by using free radicals to gradually transfer-addition-terminate under visible light conditions. The preparation steps of the method are as follows:

[0039] (1) Mix 0.5mmol of 1,8-diiodoperfluorooctane, 0.5mmol of 1,7-octadiene, and 0.025mmol of Ru(bpy) 3 Cl 2 , 0.175mmol of sodium ascorbate, and a mixed organic solvent composed of 3mL of 1,4-dioxane and 1mL of methanol were all added to the reaction vessel, and a stirring bar was added to the reactor, and the system was stirred to make the system homogeneous. After the second deoxygenation operation, the reaction vessel is sealed to obtain the homogeneous polymerization system I;

[0040] (2) Set the temperature of the reaction vessel at 25°C and the rotation speed at 1800rpm, and conduct the polymerization reaction of the homogeneous polymerization system I under LED blue light illumination, and the reaction time is 24h;

[0041] (3) Af...

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Abstract

The invention provides a polymerization method for preparing fluorine-containing alternating copolymer through gradual transfer-addition-ending with free radicals under the condition of visible light. The preparation method includes the following steps that 1, two types of bifunctional monomers A and B, a photocatalyst, a reducing agent and mixed organic solvent are simultaneously added into a reaction reactor and stirred till a system is in a homogeneous phase, after deoxygenization is conducted four times, the reaction container is sealed, and a homogeneous polymerization system I is obtained; 2, the temperature of the reaction container is set to be 25 DEG C, the rotation speed is set to be 1500-2000 rpm, the homogeneous polymerization system I is subjected to a polymerization reaction under visible light, and the reaction time is 0.5-24 hours; 3, after the reaction is ended, the reaction container is opened, tetrahydrofuran is added to dilute the system, the diluted substance is poured into methyl alcohol for sediment, then suction filtration and drying are conducted, and the fluorine-containing alternating copolymer is obtained. By the application of the novel polymerization method, the fluorine-containing alternating copolymer is obtained successfully, and the polymerization method is a brand-new polymerization method.

Description

technical field [0001] The invention belongs to the technical field of sequence controllable polymerization, and in particular relates to a polymerization method for preparing fluorine-containing alternating copolymers by using free radicals to gradually transfer-addition-terminate under visible light conditions. Background technique [0002] Realizing organic chemical reactions under visible light conditions has always been the goal pursued by scientists. Since the concept of "photochemistry" was proposed in the 1970s, it has attracted widespread attention from scientists. (See T.P. Yoon, M.A. Ischay, J.Du, Nature Chemistry, 2010, 2:527-532 and D.A. Nicewicz, D.W.C. MacMillan, Science, 2008, 322:77-80). In recent years, the discovery of a series of cost-effective photocatalysts and their wide application have greatly promoted the development of photochemical reaction research, among which Ru(bpy) 3 Cl 2 It is an organometallic photocatalyst with wide application and high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F116/12C08F112/34C08F136/20C08F2/48
CPCC08F2/48C08F112/34C08F116/12C08F136/20C08F2438/00
Inventor 程振平徐天驰张丽芬朱秀林
Owner SUZHOU UNIV
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