CN1631966A - Permanent hydrophilic polytetrafluoroethylene microporous membrane and method for preparing same - Google Patents
Permanent hydrophilic polytetrafluoroethylene microporous membrane and method for preparing same Download PDFInfo
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- CN1631966A CN1631966A CN 200410084447 CN200410084447A CN1631966A CN 1631966 A CN1631966 A CN 1631966A CN 200410084447 CN200410084447 CN 200410084447 CN 200410084447 A CN200410084447 A CN 200410084447A CN 1631966 A CN1631966 A CN 1631966A
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Abstract
Disclosed are an internal hydrosoluble polytetrafluoroethylene film with micro holes for antibacterial in water and its preparing method. Mix the hydrophilic material and varicosity polytetrafluoroethylene resin powder, acquire the product through pressure, degreasing, extension and burning. The invention has solved the problem of internal hydrosoluble, it has simple technique and low cost, with the smallest bubble point pressure of 1.0-1.8kg/cm2, water filtration speed of 1-3m3/m2h (pressure of filtration is 0.006-0.009Mpa), can be directly applied in filtration of antibacterial in water, with remarkable economic and social benefits.
Description
Technical field
The present invention relates to a kind of polytetrafluoroethylmicroporous microporous membrane, relate in particular to a kind of hydrophilic polytetrafluoroethylmicroporous microporous membrane and preparation method thereof.
Background technology
Constantly increase and rapid economy development with world population, industry and domestic water demand and sewage emissions amount sharply increase, and directly cause the anxiety of water resources.The sewage of the annual discharging in the whole world at present reaches more than 4,000 hundred million tons, causes more than 50,000 hundred million tons of fresh water bodies contaminated, but also is the trend that goes from bad to worse.Various countries with waste water control as the most important thing.Changing rejected material to useful resource is the megatrend that global environmental protection turns to initial end to control from end treatment, is the inevitable requirement that realizes Sustainable development to the recycle of handling waste water.Take up an area of that volume is big, separation efficiency is low, the treatment capacity of unit volume equipment is little, applicable surface is narrow, shortcoming such as can't remove and comprise at present that the traditional solid-liquid separating equipment of settling pond exists subparticle.
Under this background, the micro-filtration technology of utilizing film to realize is developed rapidly.In numerous mould materials, polytetrafluoroethylmicroporous microporous membrane by the processing of two-way stretch technology, fusing point height (327 ℃), use temperature scope wide (200 ℃～260 ℃), frictional coefficient is little, smooth surface, the filtering accuracy height, filtration resistance is little, and energy consumption is low, no medium comes off, and especially has chemical resistant properties characteristics such as (the many highly corrosive media of ability) and lays a good foundation for its application aspect filtration.But the strong-hydrophobicity of film has also limited its application in water solution system is handled.
The hydrophilic modifying of current thin film mainly is by comprising the irradiation source of electron beam, plasma body etc., irradiation initiation grafting hydrophilic monomer, thus give the material hydrophilicity.The irradiation degree of depth such as electron beam are big, and are big to the mechanical property influence of material; Metal surface irradiation such as plasma body, the surface can only take place in graft reaction.The wetting ability complete processing of these polytetrafluoroethylmicroporous microporous membranes all fails to solve well the industrial production of the well behaved polytetrafluoroethylmicroporous microporous membrane of wetting ability.Only in the market hydrophilic polyfluortetraethylemicroporous microporous membrane product is that U.S. Gore company produces, and its aperture is 0.5 micron, and under the filter pressure of 0.09～0.12 MPa, water filtration speed is approximately 0.5 cubic metre/square metre hour, this product price height.
The applicant adopts blend method to prepare hydrophilic polyfluortetraethylemicroporous microporous membrane in " a kind of hydrophilic polyfluortetraethylemicroporous microporous membrane and working method thereof " (application number, 200410017158.6), but hydrophilicity is not lasting, and work-ing life is on the low side.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane and preparation method thereof, to overcome the film permanent hydrophilic problem that prior art exists.
For reaching above-mentioned purpose, the present invention is achieved in that
A kind of preparation method of permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane may further comprise the steps:
(1) hydrophilic polymer, metallic compound and coupling agent are mixed, form hydrophilic material, its parts by weight are: 1 part of hydrophilic polymer, 0.5～2 part of metallic compound, 0.001～0.05 part of coupling agent;
Said hydrophilic polymer is selected from sodium apolate, polyvinyl sulfonic acid potassium, polyethylene carboxylic acid sodium or acid polyethylene acid potassium;
Said metallic compound is selected from and is a kind of or its mixture in the oxide compound of aluminium, zinc or the oxyhydroxide;
Said coupling agent is selected from a kind of or its mixture in silane, titanic acid ester or the aluminic acid ester;
Said silane coupling agent general formula is R-SiX
3, wherein R represents amino, epoxy group(ing) or cyano group isoreactivity group, X be can hydrolysis alkoxyl group (as methoxyl group, oxyethyl group etc.) or chlorine, can adopt the commercially available prod, be the silane coupling agent of KH-550 or KH-792 as the trade mark;
Said titanic acid ester is isopropyl tri (dioctylpyrophosphato)titanate (TTOPP-38S); Said aluminic acid ester is the aluminic acid ester that contains 2～4 carbon atoms, can adopt the commercially available prod, is the aluminate coupling agent of TC-6 as the trade mark; )
(2) described hydrophilic material and expanded PTFE toner, liquid lubricant are mixed in proportion, left standstill 90～150 hours at 20～40 ℃, make toner and liquid lubricant thorough mixing, under 40～80 ℃ temperature, left standstill 10～20 hours then, form the tetrafluoroethylene material;
Its parts by weight are: 1 part of hydrophilic material, 1～20 part of expanded PTFE toner, 0.2～0.6 part of liquid lubricant;
Preferential adopt that degree of crystallinity is 98～99.9%, molecular weight is 2,000,000～1,000 ten thousand expanded PTFE toner, can adopt the commercially available prod, as the F-106 of Daikin company or the CD123 of Japan AGC company;
Liquid lubricant is selected from a kind of or its mixture in whiteruss, sherwood oil or the kerosene;
(3) described tetrafluoroethylene material is rolled into the tetrafluoroethylene base band under 40～60 ℃;
(4) with described tetrafluoroethylene base band at 100～300 ℃ of following longitudinal stretchings, be processed into the degreasing base band;
(5) with described degreasing base band decatize in water vapor, steam temperature is 90～120 ℃, and preferred steaming time is 10 minutes～24 hours;
(6) with described decatize degreasing base band at 80～200 ℃ of following cross directional stretchs, sintering typing then, preferred sintering temperature is 250～380 ℃, the time is 30 seconds～2 minutes, obtains into permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane.
According to optimized technical scheme of the present invention, hydrophilic material and tetrafluoroethylene material that step (2) is mixed are pressed into cylindrical blank, this blank is extruded club by the pushing machine, this club rolls into the tetrafluoroethylene base band then, adopts 40～60 ℃ hot blast drying in the calender line.
Another object of the present invention promptly provides a kind of permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane, by method for preparing.
Adopt U.S. Ku Erte disclosed method to detect, permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane by method for preparing of the present invention, its film micropore aperture is 0.1 micron～6 microns, when filter pressure was 0.006～0.009 MPa, water filtration speed was 1～4 cubic metre/square metre hour.
The invention has the beneficial effects as follows: the permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane that utilizes the present invention to prepare, technology is simple, cost is low.The permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane that utilizes the present invention to prepare, film micropore aperture are 0.1 micron～6 microns, and water filtration speed is 1～4 cubic metre/square metre hour (filter pressure is 0.006～0.009 MPa).This film can directly be widely used in the sewage water filtration industry, has remarkable economic efficiency and social benefit.
Description of drawings
Fig. 1 is the electron scanning micrograph of permanent hydrophilic polytetrafluoroethylmicroporous film
Embodiment
Embodiment 1
A kind of working method of permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane, its step is as follows:
1, the preparation of hydrophilic material: 1 kilogram of sodium apolate and 0.5 kilogram of aluminium sesquioxide powder and 0.001 kilogram of (KH550) silane coupling agent are mixed, obtain hydrophilic material;
2, batch mixing: with (F106 expanded PTFE toner, hydrophilic material and whiteruss are even by weight 1: 1: 0.3 mixed, left standstill 100 hours at 25 ℃, make toner and liquid lubricant thorough mixing, under 70 ℃ temperature, left standstill 15 hours then, form the tetrafluoroethylene material;
3, pressed compact and extruding: with the tetrafluoroethylene material that mixes on harder 30 ℃ be pressed into cylindrical blank, blank is extruded club by the pushing machine, roll into the tetrafluoroethylene base band through rolling press then, 150 microns of base band thickness adopt 50 ℃ of hot blast dryings in the calender line;
4, longitudinal stretching: with the tetrafluoroethylene base band, in 220 ℃ of baking ovens, carry out longitudinal stretching, lubricant volatilization in the drawing process, processing degreasing base band, degreasing base band thickness is 80 microns;
5, degreasing base band decatize 4 hours in 100 ℃ of water vapors;
6, cross directional stretch and sintering: with the vapour degreasing base band on expander 130 ℃ carry out cross directional stretch, at last 330 ℃ of following sintering heat setting types 30 seconds, preparation thickness is 30 microns permanent hydrophilic polytetrafluoroethylmicroporous film.
According to the permanent hydrophilic polytetrafluoroethylmicroporous film that above-mentioned steps makes, its membrane pore size is 1.8 microns, and water filtration speed is 3.980 cubic metres/square metre hours (filter pressure is 0.009 MPa).
See Fig. 1 according to the permanent hydrophilic polytetrafluoroethylmicroporous film scanning electron micrograph that above-mentioned steps makes.
Embodiment 2
A kind of working method of permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane, its step is as follows:
1, the preparation of hydrophilic material: with 1 kilogram of polyethylene carboxylic acid sodium, 1 kilogram of aluminium sesquioxide powder, 0.02 kilogram of (TC-6) aluminate coupling agent mixes, and obtains hydrophilic material;
2, batch mixing: with F106 expanded PTFE toner, hydrophilic material, with sherwood oil by weight 10: 1: 0.6 mixed is even, left standstill 150 hours at 35 ℃, make toner and liquid lubricant thorough mixing, under 65 ℃ temperature, left standstill 12 hours then, form the tetrafluoroethylene material;
3, pressed compact and extruding: with the tetrafluoroethylene material that mixes on harder 30 ℃ be pressed into cylindrical blank, blank is extruded club by the pushing machine, roll into the tetrafluoroethylene base band through rolling press then, 140 microns of base band thickness adopt 45 ℃ of hot blast dryings in the calender line;
4, longitudinal stretching: with the tetrafluoroethylene base band, in 200 ℃ of baking ovens, carry out longitudinal stretching, lubricant volatilization in the drawing process, processing degreasing base band, degreasing base band thickness is 65 microns;
5, degreasing base band decatize 20 hours in 120 ℃ of water vapors;
6, cross directional stretch and sintering: with the degreasing base band on expander 150 ℃ carry out cross directional stretch, at last 310 ℃ of following sintering heat setting types 1 minute, the preparation thickness be 32 microns permanent hydrophilic polytetrafluoroethylmicroporous films.
According to the permanent hydrophilic polytetrafluoroethylmicroporous film that above-mentioned steps makes, adopt U.S. Ku Er special formula method to measure, its membrane pore size is 1.4 microns, water filtration speed is 3.721 cubic metres/square metre hours (filter pressure is 0.006 MPa).
Embodiment 3
A kind of working method of permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane, its step is as follows:
1, the preparation of hydrophilic material: with 1 kilogram of polyethylene carboxylic acid sodium, 1.5 kilograms of Zinc oxide powders, 0.05 kilogram of TTOPP-38S coupling agent mixes, and obtains hydrophilic material;
2, batch mixing: with CD123 expanded PTFE toner, hydrophilic material, even by weight 1: 0.8: 0.5 mixed with liquid lubricant, left standstill 120 hours at 30 ℃, make toner and liquid lubricant thorough mixing, under 80 ℃ temperature, left standstill 10 hours then, form the tetrafluoroethylene material;
3, pressed compact and extruding: with the tetrafluoroethylene material that mixes on harder 30 ℃ be pressed into cylindrical blank, blank is extruded club by the pushing machine, roll into the tetrafluoroethylene base band through rolling press then, 140 microns of base band thickness adopt 60 ℃ of hot blast dryings in the calender line;
4, longitudinal stretching: with the tetrafluoroethylene base band, in 200 ℃ of baking ovens, carry out longitudinal stretching, lubricant volatilization in the drawing process, processing degreasing base band, degreasing base band thickness is 65 microns;
5, degreasing base band decatize 8 hours in 110 ℃ of water vapors;
6, cross directional stretch and sintering: with the degreasing base band on expander 200 ℃ carry out cross directional stretch, at last 310 ℃ of following sintering heat setting types 2 minutes, the preparation thickness be 32 microns permanent hydrophilic polytetrafluoroethylmicroporous films.
According to the permanent hydrophilic polytetrafluoroethylmicroporous film that above-mentioned steps makes, adopt U.S. Ku Er special formula method to measure, its membrane pore size is 4.1 microns, water filtration speed is 3.9 cubic metres/square metre hours (filter pressure is 0.009 MPa).
Claims (10)
1. the preparation method of a permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane is characterized in that, may further comprise the steps:
(1) hydrophilic polymer, metallic compound and coupling agent are mixed, form hydrophilic material;
Said hydrophilic polymer is selected from sodium apolate, polyvinyl sulfonic acid potassium, polyethylene carboxylic acid sodium or acid polyethylene acid potassium;
Said metallic compound is selected from and is a kind of or its mixture in the oxide compound of aluminium, zinc or the oxyhydroxide;
Said coupling agent is selected from a kind of or its mixture in silane, titanic acid ester or the aluminic acid ester;
(2) described hydrophilic material is mixed with expanded PTFE toner, liquid lubricant, form the tetrafluoroethylene material;
Its parts by weight are: 1 part of hydrophilic material, 1～20 part of expanded PTFE toner, 0.2～0.6 part of liquid lubricant;
(3) described tetrafluoroethylene material is rolled into the tetrafluoroethylene base band;
(4) with described tetrafluoroethylene base band longitudinal stretching, be processed into the degreasing base band;
(5) with described degreasing base band decatize in water vapor;
(6) with described decatize degreasing base band cross directional stretch, sintering typing then obtains into permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane.
2. method according to claim 1 is characterized in that, 1 part of hydrophilic polymer, 0.5～2 part of metallic compound, 0.001～0.05 part of coupling agent.
3. method according to claim 1 is characterized in that said silane coupling agent general formula is R-SiX
3, wherein R represents amino, epoxy group(ing) or cyano group, X be can hydrolysis alkoxyl group or chlorine; Said titanic acid ester is an isopropyl tri (dioctylpyrophosphato)titanate, and said aluminic acid ester is the aluminic acid ester that contains 2～4 carbon atoms.
4. method according to claim 1 is characterized in that, expanded PTFE toner degree of crystallinity is 98～99.9%, molecular weight is 2,000,000～10,000,000.
5. method according to claim 1 is characterized in that, liquid lubricant is selected from a kind of or its mixture in whiteruss, sherwood oil or the kerosene.
6. method according to claim 1, it is characterized in that, described tetrafluoroethylene material rolls into the tetrafluoroethylene base band under 40～60 ℃, described tetrafluoroethylene base band is at 100～300 ℃ of following longitudinal stretchings, described degreasing base band decatize in water vapor, and steam temperature is 90～120 ℃, steaming time is 10 minutes～24 hours, described decatize degreasing base band is at 80～200 ℃ of following cross directional stretchs, and sintering temperature is 250～380 ℃, obtains into permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane.
7. according to each described method of claim 1～6, it is characterized in that, hydrophilic material and tetrafluoroethylene material that step (2) is mixed are pressed into cylindrical blank, this blank is extruded club by the pushing machine, this club rolls into the tetrafluoroethylene base band then, adopts the hot blast drying in the calender line.
8. method according to claim 7 is characterized in that, adopts 40～60 ℃ hot blast drying in the calender line.
9. according to the permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane of each described method preparation of claim 1～8.
10. permanent hydrophilic polytetrafluoroethylmicroporous microporous membrane according to claim 9 is characterized in that, the film micropore aperture is 0.1 micron～6 microns, and when filter pressure was 0.006～0.009 MPa, water filtration speed was 1～4 cubic metre/square metre hour.
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| CN 200410084447 CN1631966A (en) | 2004-11-22 | 2004-11-22 | Permanent hydrophilic polytetrafluoroethylene microporous membrane and method for preparing same |
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| CN 200410084447 CN1631966A (en) | 2004-11-22 | 2004-11-22 | Permanent hydrophilic polytetrafluoroethylene microporous membrane and method for preparing same |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538395B (en) * | 2009-04-23 | 2010-12-08 | 宁波登天氟材有限公司 | Oil stain-resistant polyfluortetraethylene microporous membrane and processing method thereof |
| CN101920559A (en) * | 2010-06-09 | 2010-12-22 | 浙江格尔泰斯环保特材科技有限公司 | Preparation method and product of polytetrafluoroethylene (PTFE) film |
| CN102002201B (en) * | 2009-09-28 | 2012-09-05 | 浙江鹏孚隆科技有限公司 | Method for improving critical cracking thickness of PTFE (Polytetrafluoroethylene) resin emulsion and applications of modified PTFE resin emulsion to non-stick coatings |
| CN103961937A (en) * | 2014-04-30 | 2014-08-06 | 桐乡市健民过滤材料有限公司 | Membrane filter material with high temperature resistance and high flame retardancy and preparation method thereof |
| CN107177146A (en) * | 2017-07-26 | 2017-09-19 | 合肥梵腾环保科技有限公司 | A kind of weather-resistance flame-retardant high-performance glass surface protection film and preparation method thereof |
| CN107383716A (en) * | 2017-06-20 | 2017-11-24 | 中纺院（天津）科技发展有限公司 | A kind of polytetrafluoroethylmicroporous microporous membrane and preparation method thereof |
| CN107778500A (en) * | 2017-11-02 | 2018-03-09 | 浙江衢州鑫巨氟材料有限公司 | A kind of manufacture method of hydrophilic film super high molecular weight polytetrafluoroethylene (PTFE) |
| CN108786495A (en) * | 2018-06-13 | 2018-11-13 | 南通强生石墨烯科技有限公司 | A kind of antibacterial graphene oxide is modified PVDF hollow-fibre membranes and preparation method thereof |
| CN108912359A (en) * | 2018-06-12 | 2018-11-30 | 苏州优可发新材料科技有限公司 | A kind of high bubble pressure microporous teflon membran and preparation method thereof |
| CN108993174A (en) * | 2018-08-20 | 2018-12-14 | 宁波昌祺微滤膜科技有限公司 | A kind of ePTFE hydrophilic film of resistance to sodium hypochlorite and its preparation method and application |
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2004
- 2004-11-22 CN CN 200410084447 patent/CN1631966A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538395B (en) * | 2009-04-23 | 2010-12-08 | 宁波登天氟材有限公司 | Oil stain-resistant polyfluortetraethylene microporous membrane and processing method thereof |
| CN102002201B (en) * | 2009-09-28 | 2012-09-05 | 浙江鹏孚隆科技有限公司 | Method for improving critical cracking thickness of PTFE (Polytetrafluoroethylene) resin emulsion and applications of modified PTFE resin emulsion to non-stick coatings |
| CN101920559A (en) * | 2010-06-09 | 2010-12-22 | 浙江格尔泰斯环保特材科技有限公司 | Preparation method and product of polytetrafluoroethylene (PTFE) film |
| CN103961937A (en) * | 2014-04-30 | 2014-08-06 | 桐乡市健民过滤材料有限公司 | Membrane filter material with high temperature resistance and high flame retardancy and preparation method thereof |
| CN107383716A (en) * | 2017-06-20 | 2017-11-24 | 中纺院（天津）科技发展有限公司 | A kind of polytetrafluoroethylmicroporous microporous membrane and preparation method thereof |
| CN107177146A (en) * | 2017-07-26 | 2017-09-19 | 合肥梵腾环保科技有限公司 | A kind of weather-resistance flame-retardant high-performance glass surface protection film and preparation method thereof |
| CN107778500A (en) * | 2017-11-02 | 2018-03-09 | 浙江衢州鑫巨氟材料有限公司 | A kind of manufacture method of hydrophilic film super high molecular weight polytetrafluoroethylene (PTFE) |
| CN108912359A (en) * | 2018-06-12 | 2018-11-30 | 苏州优可发新材料科技有限公司 | A kind of high bubble pressure microporous teflon membran and preparation method thereof |
| CN108786495A (en) * | 2018-06-13 | 2018-11-13 | 南通强生石墨烯科技有限公司 | A kind of antibacterial graphene oxide is modified PVDF hollow-fibre membranes and preparation method thereof |
| CN108993174A (en) * | 2018-08-20 | 2018-12-14 | 宁波昌祺微滤膜科技有限公司 | A kind of ePTFE hydrophilic film of resistance to sodium hypochlorite and its preparation method and application |
| CN108993174B (en) * | 2018-08-20 | 2021-07-13 | 宁波昌祺微滤膜科技有限公司 | Sodium hypochlorite-resistant ePTFE hydrophilic membrane and preparation method and application thereof |
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