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Preparation method and application of super-hydrophobic fluorine-containing block copolymer microspheres

A block copolymer, super-hydrophobic technology, applied in coatings, anti-corrosion coatings, etc., can solve the problems of increased polymer toxicity, difficulty in removal and conversion, complex preparation process, etc., to achieve fewer operation steps, reduce environmental problems and products. post-processing problems, molecular weight controllable effect

Active Publication Date: 2017-08-04
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there are many disadvantages in using dithioester derivatives as chain transfer reagents, as may increase the toxicity of polymer, the preparation process of dithioester is more complicated, make polymer have certain color and smell; tougher

Method used

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  • Preparation method and application of super-hydrophobic fluorine-containing block copolymer microspheres
  • Preparation method and application of super-hydrophobic fluorine-containing block copolymer microspheres

Examples

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Embodiment 1

[0031] A method for preparing superhydrophobic fluorine-containing block copolymer microspheres, comprising:

[0032] The 1L reactor was evacuated to remove moisture and air, followed by carbon dioxide and then evacuated three times; 0.7g perfluoroiodohexane (C 6 f 13 1) chain transfer agent is added in the reactor, and then adding 15g mass percent is 9:1 vinylidene fluoride and perfluoro-n-propyl vinyl ether, then 0.07g tert-butyl peroxypivalate is added to the reactor, and then Use a high-pressure plunger pump to press carbon dioxide into the reactor to heat the reactor to 80°C. After the reactor pressure reaches 40MPa, after 22 hours of heat preservation polymerization, slowly open the valve to recover carbon dioxide and remaining monomers to obtain poly(vinylidene fluoride- co-perfluoro-n-propyl vinyl ether) macromolecular chain transfer agent;

[0033] Then add 30g of perfluorooctyl ethyl acrylate into the reaction kettle and vacuumize it, add 0.2g of tert-butyl peroxyp...

Embodiment 2

[0036] A method for preparing superhydrophobic fluorine-containing block copolymer microspheres, comprising:

[0037] Vacuumize the 1L reactor to remove moisture and air, pass carbon dioxide and then evacuate, repeat three times; 0.1g perfluoroiodobutane (C 4 f 9 1) chain transfer agent is added in the reactor, then adding 5g mass percent is 5:1 vinylidene fluoride and perfluoro-n-propyl vinyl ether, then 0.02g tert-butyl peroxypivalate is added to the reactor, and then Press carbon dioxide into the reactor with a high-pressure plunger pump, heat the reactor to 60°C, and make the pressure of the reactor reach 10 MPa. After 5 hours of heat preservation polymerization, slowly open the valve to recover carbon dioxide and remaining monomers to obtain poly(vinylidene fluoride) -co-perfluoro-n-propyl vinyl ether) macromolecular chain transfer agent;

[0038]Add 5g of perfluorooctyl ethyl acrylate to the reactor and vacuumize it, add 2g of dibenzoyl peroxide to the reactor, then pr...

Embodiment 3

[0041] A method for preparing superhydrophobic fluorine-containing block copolymer microspheres, comprising:

[0042] The 1L reaction kettle was vacuumized to remove moisture and air, and then carbon dioxide was evacuated, and repeated three times; 10g perfluorooctane iodide (C 8 f 17 1) chain transfer agent is added in the reactor, then adding 100g mass percentage is vinylidene fluoride and perfluoro-n-propyl vinyl ether of 20:1, 5g dibenzoyl peroxide is added to the reactor, and then with a high-pressure plunger The pump presses carbon dioxide into the reactor, heats the reactor to 90°C, and makes the pressure of the reactor reach 40MPa. After 24 hours of thermal insulation polymerization, slowly open the valve to recover carbon dioxide and remaining monomers to obtain poly(vinylidene fluoride-co-perfluoro n-propyl vinyl ether) macromolecular chain transfer agent;

[0043] Add 100g of perfluorooctyl ethyl acrylate to the reactor and vacuumize it, add 5g of dibenzoyl peroxi...

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Abstract

The invention provides a preparation method and application of a super-hydrophobic fluorine-containing block copolymer microspheres and belongs to the field of preparation of polymer materials. The method for preparing the microspheres comprises the following steps: with perfluoroalky iodide as a chain transfer agent, preparing a scCO2 hydrophobic poly(vinylidene fluoride-co-heptafluoropropyl trifluorovinyl ether) macro-chain transfer agent in a reactor by adopting controlled free radical polymerization with iodine-containing compounds in which the polymerization condition is close to that in traditional industrial production; and with scCO2 as a solvent, adding a fluorinated acrylate monomer for reaction continuously, thereby obtaining the super-hydrophobic fluorine-containing block copolymer microspheres. According to the method disclosed by the invention, the super-hydrophobic fluorine-containing block copolymer microspheres are directly prepared in scCO2 through a polymerization-induced self-assembly process by adopting a one-step process, the operating steps are less, the polymerization reaction condition is close to that in the traditional industrial production, and the product is controllable in molecular weight and narrow in molecular weight distribution and can effectively solve the environmental problem brought by usage of an organic solvent and a dispersing agent.

Description

technical field [0001] The invention relates to the field of polymer material preparation, in particular to a preparation method and application of superhydrophobic fluorine-containing block copolymer microspheres. Background technique [0002] Due to its unique structure, fluorine-containing polymers exhibit many special properties, such as: fluorine atoms have lower polarizability, smaller van der Waals radius The bond energy of the C-F bond is as high as 485k J mol -1 , is the chemical bond with the largest bond energy among all covalent single bonds. The presence of a large number of C-F bond groups makes fluorine-containing polymers exhibit excellent chemical corrosion resistance, heat resistance, durability, weather resistance and friction resistance. In view of its excellent performance, this type of special polymer Polymers are widely used in many fields. [0003] Block copolymer microspheres are a new type of functional polymer materials, which are widely used i...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F2/38C08F2/34C09D153/00C09D5/08
CPCC08F2/34C08F2/38C08F293/005C09D5/08C09D153/00
Inventor 张书香朱忠凯张炉青徐安厚宗传永张亚彬
Owner UNIV OF JINAN
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