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A kind of preparation method of fluorine-containing super oleophobic microporous film

A technology of microporous membrane and super oleophobic, applied in flat products, other household appliances, protective clothing, etc., can solve the problems of no air permeability, low oil resistance, uncomfortable wearing, etc., to avoid deflagration and explosion, high waterproof, High safety effect

Active Publication Date: 2019-10-01
ZHEJIANG HYPROOF TECH CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] CN1373792A (public date: 2002-10-9) discloses a transparent elastomer composition obtained by coagulation of fluororesin particle emulsion and elastomer particle emulsion with an average particle diameter of 20 to 150 nanometers, wherein the fluororesin particle is Evenly and finely dispersed in the elastomer, since the fluororesin particles are uniformly and finely dispersed in the elastomer in advance, it is possible to provide an elastomer molded product with excellent mechanical strength, abrasion resistance and transparency, but such an elastomer Because the particle size of the fluororesin is too small and the molecular weight is not high enough, the composition cannot be expanded into a fluorine-containing microporous film
These two technical schemes are similar, all are open to use polytetrafluoroethylene, superhydrophobic polymer (number average molecular weight 5000-250000) such as fluorine-containing alkyl acrylate, and flammable and explosive lubricating oil to mix together Remove the film, the obtained film has low tensile strength <20MPa, low oil resistance (only No. 3 oil resistance), and the anti-fouling and washing resistance of the composite film fabric is poor
[0006] CN103158310A (disclosure date: 2013-06-19) discloses a highly oil-repellent and waterproof seamless polytetrafluoroethylene puffed sheet and a preparation method thereof. Compounded with polyurethane resin coating, the resulting film has no air permeability, no oil repellency (only No. 1 oil resistance), and the composite fabric has poor moisture permeability and is uncomfortable to wear
[0007] CN104760381A (disclosure date: 2015-07-08) discloses a preparation method of polytetrafluoroethylene waterproof and moisture-permeable fabric to enhance moisture permeability, which discloses the use of polytetrafluoroethylene and flammable and explosive lubricating oil to form a film, After adding microporous polyurethane coating, the resulting film has low air permeability, no oleophobicity (only resistant to No. 1 oil), poor flame retardancy, and is not suitable for high-end applications

Method used

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  • A kind of preparation method of fluorine-containing super oleophobic microporous film

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preparation example Construction

[0025] A kind of preparation method of fluorine-containing super-oleophobic microporous membrane comprises the steps:

[0026] S1 The fluorine-containing mixture is evenly stirred in a non-shearing manner, without adding lubricating oil, directly poured into the embryo cylinder barrel, and after exhausting, the embryo is pressed at 20°C to 100°C to make a cylindrical paste Mixed embryonic column;

[0027] S2 Extrude the germ column of the pasty mixture through a pusher at 20°C to 100°C, and then calender it into strips;

[0028] S3 Stretch the strip unidirectionally or biaxially at 100°C-200°C, and finally heat-set it at 200°C-390°C to obtain a fluorine-containing super-oleophobic microporous membrane;

[0029] The fluorine-containing mixture includes the following components in weight percentage: 50% to 90% of component A, 3% to 25% of component B, 0% to 35% of component C, and 0% to 3% of component D ; Among them, A component includes high molecular weight polytetrafluoroe...

Embodiment 1

[0049] The preparation of embodiment 1 high molecular weight polytetrafluoroethylene copolymerization dispersion resin

[0050]In a horizontal autoclave with an internal volume of about 1000 liters, first add 500 liters of deionized water, 20 kg of high-purity paraffin (melting point 50 ° C ~ 85 ° C), and 180 grams of perfluorooctanoic acid ammonium, and vacuumize the inside of the autoclave Exhaust oxygen (up to oxygen content99.999% in the still to make the inner pressure of the still reach about 22 kg. Then 300 grams of perfluoroethyl vinyl ether (C 2 f 5 -OCF=CF 2 ) as a comonomer, start to add in the kettle at a rate of 10 grams per minute, and add 0.8 grams of ammonium persulfate (dissolved in 500 milliliters of water in advance) as an initiator in the kettle to start the copolymerization reaction, and the temperature in the kettle is maintained at 80 ~ 100°C, feed tetrafluoroethylene gas during the reaction to maintain the pressure in the kettle at about 20 kg. Cont...

Embodiment 2

[0051] The preparation of embodiment 2 polyurethane acrylate prepolymer

[0052] In a reaction kettle with an internal volume of about 200 liters, the jacket is first heated to 100°C, the kettle is vacuumed and nitrogen dehumidified, and 26.2 kg (containing about 200 moles of NCO isocyanate) 4,4'-dicyclohexylmethane is added Diisocyanate HMDI, start stirring, the temperature in the kettle rises to about 100°C, then add 60 kg (containing about 60 moles of -OH hydroxyl groups) of polypropylene glycol (molecular weight about 2000) to the kettle, react for about 90 minutes, add 18.2 Kg (containing about 140 mol-OH hydroxyl groups) hydroxyethyl methacrylate, the temperature in the kettle is maintained at about 100 ° C, and after about one hour of reaction, a polyurethane acrylate prepolymer with a viscous liquid is obtained. After cooling It is a liquid at 50°C, indicating that the melting point is lower than 50°C.

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Abstract

The invention discloses a method for preparing a fluorine-containing super-oleophobic microporous membrane. A specifically developed fluorine-containing mixed material is adopted as a raw material, and the fluorine-containing mixed material comprises the following components in percentage by weight: 50-90% of a component A, 3-25% of a component B, 0-35% of a component C and 0-3% of a component D, wherein the component A comprises a high molecular weight polytetrafluoroethylene homopolymerization or copolymer dispersion resin; the component B comprises one or more fluorine-containing alkyl acrylate monomers; the component C comprises one or more fluorine-free acrylate; and the component D comprises a high-temperature free radical initialize. As no lubricating oil which is liable to combust and explode is used, the membrane is high in security; and in addition, the prepared fluorine-containing super-oleophobic microporous membrane has relatively good properties of water resistance, breathability, oil stain resistance and water washing resistance, and requirements of new-generation waterproof breathable protection clothes are met.

Description

technical field [0001] The invention relates to the technical field of special fluorine-containing super-oleophobic microporous membranes used in anti-wind, snow and rain, lightweight, warm-keeping and breathable protective clothing fabrics, in particular to a preparation method of a fluorine-containing super-oleophobic microporous membrane. Background technique [0002] Fluorine-containing polymers, especially homopolymerized, modified, or copolymerized resins of tetrafluoroethylene have excellent physical and mechanical properties and chemical stability, and are widely used in chemical materials, mechanical electronics, aerospace, military protection, new materials and new energy, etc. There are a wide range of applications in various fields. After blending high-molecular-weight polytetrafluoroethylene dispersion resin with lubricating oil, it is extruded in paste state, extruded, deoiled, stretched in one direction or two directions, and finally shaped to obtain expanded ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F291/04C08F291/12C08F220/24C08F220/18C08L51/00C08L51/08A41D31/10A41D31/04B29C69/02B29L7/00
CPCA41D31/04A41D31/14B29C69/02B29L2007/00C08F259/08C08F283/008C08J5/18C08J2351/00C08J2351/08C08F220/1811
Inventor 吴慧生杨颖
Owner ZHEJIANG HYPROOF TECH CO LTD
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