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Porous ultra-high molecular weight poly fluorine-containing olefin hollow microspheres and preparation method thereof

An ultra-high molecular weight, fluorine-containing olefin technology, applied in the field of porous ultra-high molecular weight polyfluorine-containing olefin hollow microspheres and their preparation, can solve the problem that the viscosity of the polymer solution cannot meet the requirements of lithium batteries, the polymer molecular weight is low, and the production efficiency low problems, to achieve the effect of excellent industrialization prospects, excellent mechanical properties, and mild reaction conditions

Active Publication Date: 2022-07-22
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above-mentioned problems, the present invention provides a porous ultra-high molecular weight polyfluoroolefin microsphere and its preparation method, which solves the problem of the low molecular weight of the obtained polymer due to the long cycle and low production efficiency of the existing polyfluoroolefin production process. , so that the viscosity of the obtained polymer solution does not meet the requirements of lithium batteries and other technical problems

Method used

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  • Porous ultra-high molecular weight poly fluorine-containing olefin hollow microspheres and preparation method thereof
  • Porous ultra-high molecular weight poly fluorine-containing olefin hollow microspheres and preparation method thereof

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preparation example Construction

[0025] The preparation method of a porous ultra-high molecular weight polyfluoroolefin microsphere of the present invention adopts a metal nanoparticle catalyzed polymerization reaction system, and the polymerization method is suspension polymerization, comprising the following steps:

[0026] (1) The reaction kettle is evacuated and then filled with nitrogen to replace the air in the reaction kettle. The second monomer, catalyst, initiator, dispersant and deionized water are added in a certain mass ratio, and the reaction kettle is closed. Monomer: catalyst: initiator: dispersant: deionized water= 5~20: 0.0001~0.01: 0.1~1.0: 0.1~1.0: 300~800;

[0027] (2) The reaction kettle is heated to 30~60℃, the stirring speed is maintained at 500~1500 r / min, the porogen is added according to a certain mass ratio, and the stirring is uniform, wherein the second monomer: porogen=5~20: 0.1 ~1.0;

[0028] (3) Keep the temperature of the reaction kettle at 30~60°C, maintain the stirring spee...

Embodiment 1

[0033] First close the reaction kettle, vacuumize the reaction kettle, and then fill with nitrogen in a vacuum state to replace the air in the reaction kettle. In a stainless steel autoclave equipped with stirring, through the equipment feeding device, add 600 g of deionized water, 10 g of hexafluorobutyl methacrylate, 0.001 g of silver nanoparticles (spherical), 0.8 g of ethyl 2-bromoisobutyrate ester, 0.3 g polyvinyl alcohol, 0.3 g n-pentane.

[0034] The temperature of the reaction kettle was maintained at 50 °C, the stirring speed was maintained at 500 r / min, and the pressure of the kettle was increased to 3.5 MPa by filling with vinylidene fluoride. Maintained at 50 °C, the polymerization reaction time was 10 h. After the reaction is completed, the stirring is stopped, and the polymer product is centrifuged, washed and dried to obtain porous ultra-high molecular weight polyvinylidene fluoride hollow microspheres.

[0035] Measurement of particle size and pore size of mi...

Embodiment 2

[0039]First close the reaction kettle, vacuumize the reaction kettle, and then fill with nitrogen in a vacuum state to replace the air in the reaction kettle. In a stainless steel autoclave equipped with stirring, through the equipment feeding device, add 800 g of deionized water, 5 g of hexafluorobutyl methacrylate, 0.0001 g of silver nanoparticles (spherical), 0.1 g of ethyl 2-bromoisobutyrate ester, 0.1 g polyvinyl alcohol, 0.1 g n-pentane.

[0040] The temperature of the reaction kettle was maintained at 30 °C, the stirring speed was maintained at 800 r / min, and the pressure of the kettle was increased to 2.8 MPa by filling with vinylidene fluoride. Maintained at 30 °C, the polymerization reaction time was 15 h. After the reaction is completed, the stirring is stopped, and the polymer product is centrifuged, washed and dried to obtain porous ultra-high molecular weight polyvinylidene fluoride hollow microspheres.

[0041] The test procedure in Example 1 was repeated. Th...

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Abstract

The preparation method comprises the following steps: (1) vacuumizing a reaction kettle, introducing nitrogen, and adding a metal nano catalyst and reactants according to a certain mass ratio; (2) heating the reaction kettle to 30-60 DEG C, stirring at the rotating speed of 500-1500 r / min, and adding a pore-foaming agent; (3) maintaining the rotating speed at 500-1500 r / min, and filling a fluorine-containing monomer to reach the polymerization reaction pressure; and (4) centrifuging, washing and drying the polymerization product. The molecular weight of the obtained fluorine-containing olefin hollow microspheres is 1.5-3.0 times that of a polymer obtained through common free radical polymerization, the molecular weight distribution is narrow, the size of the microspheres is 10-200 m, and the pore diameter is 5-20 m. And the obtained product has high porosity and is applied to lithium battery binders, diaphragms and high-efficiency catalyst carriers. The method is mild in reaction condition, low in cost and environment-friendly, and has an excellent industrial prospect.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, in particular to a porous ultra-high molecular weight polyfluoroolefin hollow microsphere and a preparation method thereof. Background technique [0002] Fluoropolymers have good heat resistance, cold resistance, electrical insulation, chemical resistance and mechanical properties, and are excellent high temperature resistant materials and insulating materials. Fluoropolymers have a wide range of applications in construction, chemical, electronic, and automotive fields. Among them, the special molecular structure of polyvinylidene fluoride makes it have both and better properties than fluororesins and general resins, such as: excellent chemical resistance, high temperature resistance, weather resistance, UV resistance, dielectric properties, etc. The excellent properties of polyfluoroolefins make it widely used in lithium batteries, chemical engineering anticorrosion, piezoe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/14C08L27/16C08L27/18C08L27/14C08F114/20C08F214/22C08F220/24C08F214/24C08F214/18C08F214/28C08F214/26
CPCC08J9/141C08F114/20C08F214/22C08F214/26C08J2327/16C08J2203/14C08J2327/18C08J2327/14C08F220/24C08F214/24C08F214/182C08F214/28Y02E60/10
Inventor 唐浩东张攀攀何明慧韩文锋李瑛刘宗健
Owner ZHEJIANG UNIV OF TECH
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