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A novel perfluorocyclobutyl-containing macroinitiator for atom transfer radical polymerization and its preparation method and use

A macromolecular initiator, perfluorocyclobutyl technology, which is applied in the field of preparation of macromolecular initiators, can solve the problems of introducing commercial monomers into composite fluoropolymers, restricting the development of PFCB-type polymers, etc., and achieves good resistance. Effects of solvent and chemical stability, low surface energy, high hydrophobicity and oleophobicity

Active Publication Date: 2017-05-10
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the relatively high polymerization temperature (>150°C) and unique polymerization mechanism, the current research on PFCB-type polymers mainly focuses on the preparation of PFCB-containing homopolymers by thermal cyclopolymerization of different trifluorovinyl aryl ether monomers. At the same time, limited by the design and synthesis of functional groups linking trifluorovinyl in monomers, it is difficult to introduce general commercial monomers into trifluorovinyl aryl ether monomers to obtain Composite fluoropolymers, these two factors limit the development of PFCB-type polymers

Method used

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  • A novel perfluorocyclobutyl-containing macroinitiator for atom transfer radical polymerization and its preparation method and use
  • A novel perfluorocyclobutyl-containing macroinitiator for atom transfer radical polymerization and its preparation method and use
  • A novel perfluorocyclobutyl-containing macroinitiator for atom transfer radical polymerization and its preparation method and use

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Embodiment 1

[0047] The concrete steps of the preparation method of the amphiphilic graft copolymer containing perfluorocyclobutyl of the present invention are as follows:

[0048] (1) Add dimethyl sulfoxide to 5-methoxy resorcinol, stir to make it dissolve, the weight volume ratio of 5-methoxy resorcinol and dimethyl sulfoxide is 5:200g / mL, decompress the mixed solution with an oil pump, bubble the solution with nitrogen to remove the oxygen in the solution, under the protection of nitrogen, add cesium carbonate, the weight ratio of cesium carbonate to 5-methoxyresorcinol is 45 :5, after bubbling in the solution with nitrogen, add 1,2-dibromotetrafluoroethane, the weight ratio of 1,2-dibromotetrafluoroethane and 5-methoxy resorcinol is 35: 5. Heat up to 40°C, stir for 3 days, stop heating, cool the reaction mixture to room temperature, add water and stir, the volume ratio of water to dimethyl sulfoxide is 100:200, then add dichloromethane, dichloromethane The volume ratio with dimethyl ...

Embodiment 2

[0057] The concrete steps of the preparation method of the amphiphilic graft copolymer containing perfluorocyclobutyl of the present invention are as follows:

[0058] (1) Add dimethyl sulfoxide to 5-methoxy resorcinol, stir to make it dissolve, the weight volume ratio of 5-methoxy resorcinol and dimethyl sulfoxide is 10:200g / mL, decompress the mixed solution with an oil pump, bubble the solution with nitrogen to remove the oxygen in the solution, under the protection of nitrogen, add cesium carbonate, the weight ratio of cesium carbonate to 5-methoxyresorcinol is 55 :10, after bubbling in the solution with nitrogen, add 1,2-dibromotetrafluoroethane, the weight ratio of 1,2-dibromotetrafluoroethane and 5-methoxy resorcinol is 45: 10. Heat up to 60°C, stir for 1 day, stop heating, cool the reaction mixture to room temperature, add water and stir, the volume ratio of water to dimethyl sulfoxide is 300:200, then add dichloromethane, dichloromethane The volume ratio with dimethy...

Embodiment 3

[0067] (1) Add 5-methoxyresorcinol (7.0 g, 0.05 mol) and dimethyl sulfoxide (200 mL) into a 500 mL three-necked flask, and stir to dissolve the quinone. After decompressing with an oil pump for 30 minutes, nitrogen was bubbled into the solution for 30 minutes to remove oxygen in the solution. Under nitrogen, cesium carbonate (48.9 g, 0.15 mol) was added. After bubbling nitrogen into the solution for 30 min, 1,2-dibromotetrafluoroethane (38.9 g, 0.15 mol) was added. The temperature was raised to 50° C. and stirred for 2 days. Stop heating, transfer the reaction mixture to a 1L beaker, after the system is cooled to room temperature, add water (200mL), stir for 10min, then add dichloromethane (100mL), separate the organic phase, and wash the organic phase with water (50mL×3). The aqueous phases were combined and extracted with n-hexane (50 mL×3). The organic phases were combined and dried over anhydrous magnesium sulfate. Filter with suction and remove the solvent with a rot...

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Abstract

The invention discloses a novel perfluorocyclobutyl-containing macroinitiator for atom transfer radical polymerization (ATRP) and a preparation method and application of the novel perfluorocyclobutyl-containing macroinitiator. The preparation method comprises the following main steps: (1) taking methoxydiphenol and 1, 2-dibromotetrafluoroethane as raw materials, and synthesizing novel trifluorovinyl aryl ether; (2) synthesizing polymers, namely PFCB-OMe with different molecular weights by utilizing (2 phi + 2 phi) thermal cyclization polymerization of novel trifluorovinyl aryl ether; (3) exploring deprotection reaction conditions to obtain polymers, namely PFCB-OH with different degrees of deprotection, and simultaneously preparing a macroinitiator PFCB-BA; and (4) preparing a grafted copolymer, namely PFCB-P tBMA by utilizing ATRP reaction between commercial tert-butyl methacrylate and PFCB-BA.

Description

technical field [0001] The invention relates to the technical fields of organic chemistry and polymer synthesis chemistry, in particular to a preparation method of a novel perfluorocyclobutyl-containing macromolecular initiator for atom transfer radical polymerization. Background technique [0002] In 1993, researchers from The Dow Chemical Company of the United States developed a new type of fluorine-containing polymer - perfluorocyclobutyl (PFCB) aryl ether polymer. This type of polymer combines the engineering thermoplasticity of polyarylether and the stability of fluorocarbon part, and has the advantages of low dielectric constant, high thermal and thermal oxidation stability, excellent optical properties and good processability. It has broad application prospects in waveguides, optical devices and coatings for spacecraft. PFCB-type polymers are generally obtained by (2π+2π) thermal cyclopolymerization of trifluorovinyl aryl ether. This thermally initiated step-growth ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/48C08F283/06C08F220/18
Inventor 朱园勤洪将剑李世宁闭丽萍李光华黄祖强
Owner GUANGXI UNIV