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Illumination polymerization method of block copolymers of main chain type semi-fluorine alternating copolymers

A technology of alternating copolymers and block copolymers, which is applied in the field of photopolymerization of block copolymers, can solve the problems of single variety, single variety of fluorine-containing polymers, and weak structure designability, etc., and achieve simple and safe operation Effect

Active Publication Date: 2019-08-30
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, the currently available fluoropolymers are limited by the types of monomers, which make them single in variety and poor in structure design, and it is difficult to meet the requirements of materials for diversification of polymer structures.
The inventors have recently developed a stepwise transfer addition of α,ω-diiodoperfluoroalkanes (as monomer A) and α,ω-nonconjugated dienes (as monomer B) for visible-light-induced catalytic polymerization- A new polymerization method of free radical termination (Step Transfer-Addition&Radical-Termination, hereinafter referred to as START), through the structural design of non-conjugated diene monomer B, a new type of "semifluoro" alternating copolymer with various polymer structures and adjustable molecular weight can be obtained (AB) n (Note: Since the A monomer chain in this type of alternating copolymer is perfluorocarbon, in order to distinguish it from other types of fluoropolymers, it is called "semi-fluoro" alternating copolymer, where n represents the degree of polymerization) , which opens up a new way of thinking and provides a feasible polymerization method for solving the above-mentioned problem of single species of fluorine-containing polymers

Method used

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  • Illumination polymerization method of block copolymers of main chain type semi-fluorine alternating copolymers
  • Illumination polymerization method of block copolymers of main chain type semi-fluorine alternating copolymers
  • Illumination polymerization method of block copolymers of main chain type semi-fluorine alternating copolymers

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Experimental program
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Effect test

Embodiment 1

[0057] Add 5mmol monomer methyl methacrylate to be polymerized, 0.01mmol alternating fluoropolymer macroinitiator (AB 1 ) n , 0.002mmol photocatalyst tris(2,2'-bipyridine) ruthenium dichloride (Ru(bpy) 3 Cl 2 ), 0.01mmol sodium ascorbate (AsAc-Na), 0.5mL acetone, after the deoxygenation operation, choose to carry out the polymerization reaction at room temperature under the irradiation of 485nm LED blue light. After the reaction reached the predetermined time, the reaction tube was opened, and a small amount of polymer solution was extracted to carry out the proton nuclear magnetic resonance spectrum ( 1 H NMR) test and calculate the conversion rate and nuclear magnetic molecular weight (M n,NMR ). The rest of the polymer solution was dissolved in a certain amount of tetrahydrofuran, over neutral Al 2 o 3 After the column, add a precipitating agent to precipitate, stand still, suction filter, and vacuum dry to obtain a block copolymer of "semifluoro" alternating copolyme...

Embodiment 2

[0062] Add different monomers (5mmol) to be polymerized in the photoreaction tube, 0.025mmol alternating fluoropolymer macromolecular initiator (AB1 ) n , 0.005mmol photocatalyst tris(2,2'-bipyridine) ruthenium dichloride (Ru(bpy) 3 Cl 2 ), 0.025mmol sodium ascorbate (AsAc-Na), 0.5mL acetone, after the deoxygenation operation, choose to carry out the polymerization reaction at room temperature under the irradiation of 485nm LED blue light. Among them, (AB 1 ) n The molecular weight is 4000g / mol, and the PDI is 1.40. After the reaction reached the predetermined time, the reaction tube was opened, and a small amount of polymer solution was extracted to carry out the proton nuclear magnetic resonance spectrum ( 1 H NMR) test and calculate the conversion rate and nuclear magnetic molecular weight (M n,NMR ). The rest of the polymer solution was dissolved in a certain amount of tetrahydrofuran, over neutral Al 2 o 3 After the column, a precipitant was added for precipitatio...

Embodiment 3

[0067] Add 5mmol monomer methyl methacrylate to be polymerized, 0.01mmol different alternating fluoropolymer macroinitiators (AB 1 ) n A. (AB 2 ) n or (AB 3 ) n , 0.002mmol photocatalyst tris(2,2'-bipyridine) ruthenium dichloride (Ru(bpy) 3 Cl 2 ), 0.01mmol sodium ascorbate (AsAc-Na), 0.5mL acetone, after the deoxygenation operation, choose to carry out the polymerization reaction at room temperature under the irradiation of 485nm LED blue light. Among them, (AB 1 ) n A. (AB 2 ) n or (AB 3 ) n The molecular weight and PDI are 6400g / mol, 1.75; 2200g / mol, 1.28; 9800g / mol, 1.91, respectively.

[0068] After the reaction reached the predetermined time, the reaction tube was opened, and a small amount of polymer solution was extracted to carry out the proton nuclear magnetic resonance spectrum ( 1 H NMR) test and calculate the conversion rate and nuclear magnetic molecular weight (M n,NMR ). The rest of the polymer solution was dissolved in a certain amount of tetrah...

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Abstract

The invention relates to an illumination polymerization method of block copolymers of main chain type semi-fluorine alternating copolymers. The method comprises the following steps: under a protectiveatmosphere, a methacrylate monomer and a semi-fluorine alternating copolymer (AB)n macroinitiator are subjected to photo-controlled living radical polymerization in an organic solvent at 20-30 DEG Cunder the action of a photocatalyst, the polymerization reaction is carried out under the condition of illumination of 390 nm to 590 nm for at least half an hour, and the block copolymers of the mainchain type polyolefin, polyester or polyether semi-fluorine alternating copolymers are obtained. The polymerization method is carried out under the condition of visible light irradiation, the polymerization process has the characteristic of living radical polymerization, and the molecular weight distribution of the prepared polymers is relatively narrow.

Description

technical field [0001] The invention relates to the technical field of polymer preparation, in particular to a photopolymerization method of a block copolymer of a main chain type "semifluoro" alternating copolymer. Background technique [0002] The emergence of topological polymers not only expands the performance of polymer materials, but also makes the correlation between polymer structure and performance more obvious. This correlation is of great significance for customizing polymer materials, and the regulation of polymer topology is in Polymer synthetic chemistry is an important research direction. Common polymer topologies include linear, star, comb, ring, hyperbranched, and dendritic structures, and there are a large number of related literature reports. On the other hand, from the perspective of the chemical structure of the polymer chain, the properties of the polymer are closely related to its chain structure, and fluoropolymers have always played an important ro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F2/46
CPCC08F293/005C08F2/46C08F4/80C08F2438/01C08F2/50C08F220/305C08F220/325C08F220/14C08F220/34C08G61/04C08G2261/124C08G2261/146C08G2261/1642C08K5/1535
Inventor 程振平成健楠张丽芬涂凯王金英朱秀林
Owner SUZHOU UNIV
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