CN103386256B - Method for preparing hollow fiber membranes and tubular membranes with microporous PTFE hybrid flat membrane wrapping method - Google Patents
Method for preparing hollow fiber membranes and tubular membranes with microporous PTFE hybrid flat membrane wrapping method Download PDFInfo
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- CN103386256B CN103386256B CN201310248985.5A CN201310248985A CN103386256B CN 103386256 B CN103386256 B CN 103386256B CN 201310248985 A CN201310248985 A CN 201310248985A CN 103386256 B CN103386256 B CN 103386256B
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Abstract
The invention discloses a method for preparing hollow fiber membranes and tubular membranes with a microporous PTFE hybrid flat membrane wrapping method. Dispersed PTFE resin and polyvinylidene fluoride resin are mixed with a liquid lubricant, and microporous PTFE hybrid flat membranes are prepared from the mixture through extrusion, calendaring, stretching and sintering. Then the microporous PTFE hybrid flat membranes are cut into membrane strips which wrap around supporting tubes, and finally the wrapped supporting tubes are sintered to obtain the hollow fiber membranes and the tubular membranes. The polyvinylidene fluoride resin added into the products of the invention has a melting point around 160 DEG C, fuses while sintered at a temperature between 250 and 340 DEG C, and can largely increase the hardness of the flat membranes after solidification, which facilitates slitting of the flat membranes. During the process of sintering after wrapping, the polyvinylidene fluoride resin contained in the flat membranes fuses again when sintered at a temperature between 260 and 340 DEG C, and thus can be used as overlapping parts between the wrapped flat membranes and as binders between the flat membranes and the microporous supporting tubes, so that the bonding strength is substantially improved.
Description
Technical field
The present invention relates to the preparation method of hollow-fibre membrane and tubular membrane, be specifically related to the method for a kind of pore type polytetrafluoroethylene (PTFE) hybrid flat looping legal system for hollow-fibre membrane and tubular membrane.
Background technology
UF membrane membrane module form mainly comprises plate and frame, hollow fiber form, rolling and tubular type four kinds of forms, and the membrane material form adopted is respectively Flat Membrane, hollow-fibre membrane, rolled film and tubular membrane.The features such as hollow-fibre membrane occupation of land is little, should not block up, easy to maintenance.
The features such as microporous teflon membran has that porosity is high, aperture is adjustable, high-low temperature resistant, corrosion-resistant, resistance to microbiological attack, have very important using value in UF membrane field.Microporous teflon membran mainly comprises Flat Membrane and hollow-fibre membrane, and it adopts decentralized polyflon, and the microstructure that this material can be formed under shear action " fibril-node ", fibril and node can form micropore.The master operation preparations such as Flat Membrane work flow is generally that raw material and lubricating oil are mixed, slaking, paste-extruded, calendering, degreasing, stretching, sintering sizing, wherein stretching can adopt unidirectional or biaxial tension.For the polytetrafluoroethylene film of processing porosity prosperity, mostly adopt the method for biaxial tension, i.e. first longitudinally rear horizontal method.Adopt biaxial tension technology, aperture controllable scope is large.The master operation preparations such as polytetrafluoroethylhollow hollow fiber membrane work flow is generally that raw material and lubricating oil are mixed, slaking, paste-extruded, degreasing, stretching, sintering sizing, because hollow-fibre membrane internal-and external diameter is less, are difficult to carry out cross directional stretch, generally be only longitudinal stretching, draw ratio is larger, and aperture is larger, porosity larger (Zhang Huapeng, Zhu Hailin, Wang Feng, Guo Yuhai, the preparation of polytetrafluoroethylhollow hollow fiber membrane, membrane science and technology, 2013,1,17-21).Therefore little, that porosity the is large simultaneously hollow-fibre membrane in processing aperture is difficult to.
In this context, occur multinomial with polytetrafluoroethylene film be filter course hollow-fibre membrane or tubular membrane wrapping technique, supporting layer can be polytetrafluoroethylene (PTFE) or other materials.As, adopt terylene (PET) fiber braided tube as stay pipe in patent 201110217618, application of adhesive in PET woven tube; By continuous for polytetrafluoroethylene film looping in PET woven tube, Flat Membrane adjacent during looping partly overlaps; Finally dry.By the aperture selecting Flat Membrane accurately can control polytetrafluoroethylhollow hollow fiber membrane, effectively improve the porosity of polytetrafluoroethylhollow hollow fiber membrane, thus promote the membrane flux of tunica fibrosa.In patent 200310124868.4, by the outer wrapped polytetrafluoroethylene film of polytetrafluoroethylhollow hollow fiber supporting layer, improve the performance of anti-blockage of polytetrafluoroethylhollow hollow fiber membrane.Polytetrafluoroethylene (PTFE) does not sinter by patent 201210547439 or half sintered membrane is wrapped on stay pipe, then sinters, and obtains wrapped type polytetrafluoroethylene (PTFE) ultra filtration tubular membrane.Patent 201120193277.2 by least one deck pore diameter range 0.02-0.5 μm, the expanded microporous polytetra fluoroethylene-EPTEE Flat Membrane looping of thickness 5-100 μm is on the polytetrafluoroethylhollow hollow fiber of 0.5-2 μm at pore diameter range, processing polytetrafluoroethylregenerated hollow-fibre membrane.Patent 200910225824.8 is by wrapped polytetrafluoroethylene (PTFE) film preparation polytetrafluoroethylene (PTFE) hollow membrane outside the braids such as polytetrafluoroethylene fibre, glass fibre, asbestos fibre.
Polytetrafluoroethylhollow hollow fiber membrane and tubular membrane are mostly for field of waste water treatment, and application mode generally adopts interior pressure or external pressure, but no matter adopt which kind of mode, and hollow-fibre membrane and tubular membrane must bear certain pressure.And although the method for looping can precisely control aperture, overlap between the Flat Membrane of looping, and Flat Membrane and backing material directly bond and must reach very high intensity.For decentralized polytetrafluoroethylmaterial material, by controlling sintering degree, and under certain temperature and pressure, self-adhesion to a certain degree can be realized, if patent 201110446377.6 is exactly the lubricating oil content controlled by sintering in polytetrafluoroethylmaterial material, realize the self-adhesion of material under heat.
For polytetrafluoroethylene film wrapping technique, except adhesion problem, the another one difficult problem faced is how polytetrafluoroethylene film cuts into strip material.For making hollow-fibre membrane and tubular membrane reach a higher water flux, must reduce the thickness of Flat Membrane, polytetrafluoroethylene film is very soft simultaneously as far as possible, cuts thin and the polytetrafluoroethylene film of softness is technical bottleneck.
Summary of the invention
In order to overcome Problems existing in background technology, the object of the present invention is to provide a kind of pore type polytetrafluoroethylene (PTFE) hybrid flat looping legal system for the method for hollow-fibre membrane and tubular membrane, the method is mixed decentralized polyflon, polyvinylidene fluoride resin and fluid lubricant, through extruding, roll, stretch, the technique such as sintering prepares pore type polytetrafluoroethylene (PTFE) hybrid flat, cut into belt type film again, looping is on stay pipe, and finally sintering forms.
The step of the technical solution used in the present invention is as follows:
(1) pore type polytetrafluoroethylene (PTFE) hybrid flat: by decentralized polyflon, polyvinylidene fluoride resin and fluid lubricant by weight percentage 1:0.02-0.08:0.2-0.3 evenly mix, 96 ~ 144 hours are left standstill at the temperature of 20 ~ 40 DEG C, then at the temperature of 40 ~ 80 DEG C, 10 ~ 16 hours are left standstill, at 20 ~ 30 DEG C, harder is pressed into cylindrical blank, blank is extruded club by plunger piston extrusion machine at the temperature of 40 ~ 60 DEG C, then at 40 ~ 60 DEG C, base band is rolled into through calender, described base band is carried out in the baking oven of 180 ~ 300 DEG C longitudinal stretching 1-6 doubly, carry out 2-5 cross directional stretch doubly again, finally sinter at 250-340 DEG C, 10 ~ 30 seconds time, obtain aperture 0.03-0.2 micron, the pore type polytetrafluoroethylene (PTFE) hybrid flat of thickness 5-50 micron,
(2) cut: the belt type film described pore type polytetrafluoroethylene (PTFE) hybrid flat being cut into width 5 ~ 9 mm wide;
(3) looping: by described belt type film spiral looping 1-10 layer on porous tubular support, obtains fasciated tube;
(4) sinter: described fasciated tube is sintered at 260-340 DEG C, time 20-80 second, prepare hollow-fibre membrane and tubular membrane.
The degree of crystallinity of described decentralized polyflon is 98 ~ 99.9%, molecular weight is 2,000,000 ~ 10,000,000.Adopt commercially available prod, as Ju Hua group 188, Daikin company F106.
Described fluid lubricant is atoleine, benzinum or kerosene.
Described porous tubular support is polytetrafluoroethylhollow hollow fiber membrane (as processed by patent 201010508798), porous ceramic pipe, stainless steel wire woven tube or carbon fiber knit pipe.
Described polyvinylidene fluoride resin, fusing point is about 160 DEG C.Adopt commercially available prod, as FR904, FR921 of Shanghai three Ai Fu new material limited company.
Compared with background technology, the beneficial effect that the present invention has is:
(1) the present invention adds polyvinylidene fluoride resin preparing in pore type polytetrafluoroethylene (PTFE) hybrid flat, its fusing point is about 160 DEG C, at the temperature of 250-340 DEG C, sinter melting, greatly can increase the hardness of Flat Membrane after solidifying, this is very beneficial for cutting of Flat Membrane.
(2) in the process that the present invention sinters after looping, because containing polyvinylidene fluoride resin in Flat Membrane, can melting again under 260-340 DEG C of sintering, between the Flat Membrane that can be used as looping, the binding agent of overlap and Flat Membrane and porous tubular support, strengthens adhesion strength greatly.
Detailed description of the invention
embodiment 1:
(1) pore type polytetrafluoroethylene (PTFE) hybrid flat: by 188 decentralized polyflons of Ju Hua group, the FR904 polyvinylidene fluoride resin of Shanghai Sanaifu New Material Co., Ltd and atoleine by weight percentage 1:0.02:0.3 evenly mix, 96 hours are left standstill at the temperature of 20 DEG C, then at the temperature of 40 DEG C, 10 hours are left standstill, at 20 DEG C, harder is pressed into cylindrical blank, blank is extruded club by plunger piston extrusion machine at the temperature of 60 DEG C, then at 40 DEG C, base band is rolled into through calender, described base band is carried out longitudinal stretching 1 times in the baking oven of 180 DEG C, carry out the cross directional stretch of 2 times again, finally sinter at 250 DEG C, 30 seconds time, obtain 0.03 micron, aperture, the pore type polytetrafluoroethylene (PTFE) hybrid flat of thickness 50 microns,
(2) cut: the belt type film described pore type polytetrafluoroethylene (PTFE) hybrid flat being cut into width 5 mm wide;
(3) looping: by described belt type film spiral looping 1 layer on the polytetrafluoroethylhollow hollow fiber membrane processed by patent 201010508798, obtains fasciated tube;
(4) sinter: described fasciated tube is sintered at 260 DEG C, 80 seconds time, prepares hollow-fibre membrane.
embodiment 2:
(1) pore type polytetrafluoroethylene (PTFE) hybrid flat: by 188 decentralized polyflons of Ju Hua group, the FR921 polyvinylidene fluoride resin of Shanghai Sanaifu New Material Co., Ltd and kerosene by weight percentage 1:0.08:0.2 evenly mix, 144 hours are left standstill at the temperature of 40 DEG C, then at the temperature of 80 DEG C, 16 hours are left standstill, at 30 DEG C, harder is pressed into cylindrical blank, blank is extruded club by plunger piston extrusion machine at the temperature of 40 DEG C, then at 60 DEG C, base band is rolled into through calender, described base band is carried out longitudinal stretching 6 times in the baking oven of 300 DEG C, carry out the cross directional stretch of 5 times again, finally sinter at 340 DEG C, 10 seconds time, obtain 0.2 micron, aperture, the pore type polytetrafluoroethylene (PTFE) hybrid flat of thickness 5 microns,
(2) cut: the belt type film described pore type polytetrafluoroethylene (PTFE) hybrid flat being cut into width 9 mm wide;
(3) looping: by described belt type film spiral looping 10 layers on porous ceramic pipe, obtains fasciated tube;
(4) sinter: described fasciated tube is sintered at 340 DEG C, 20 seconds time, preparation tubular membrane.
embodiment 3:
(1) pore type polytetrafluoroethylene (PTFE) hybrid flat: by the F106 decentralized polyflon of Daikin company, the FR921 polyvinylidene fluoride resin of Shanghai Sanaifu New Material Co., Ltd and benzinum by weight percentage 1:0.05:0.25 evenly mix, 100 hours are left standstill at the temperature of 30 DEG C, then at the temperature of 60 DEG C, 15 hours are left standstill, at 25 DEG C, harder is pressed into cylindrical blank, blank is extruded club by plunger piston extrusion machine at the temperature of 50 DEG C, then at 50 DEG C, base band is rolled into through calender, described base band is carried out longitudinal stretching 3 times in the baking oven of 200 DEG C, carry out the cross directional stretch of 3 times again, finally sinter at 280 DEG C, 20 seconds time, obtain 0.15 micron, aperture, the pore type polytetrafluoroethylene (PTFE) hybrid flat of thickness 20 microns,
(2) cut: the belt type film described pore type polytetrafluoroethylene (PTFE) hybrid flat being cut into width 7 mm wide;
(3) looping: by described belt type film spiral looping 5 layers in stainless steel wire woven tube, obtains fasciated tube;
(4) sinter: described fasciated tube is sintered at 280 DEG C, 60 seconds time, preparation tubular membrane.
embodiment 4:
(1) pore type polytetrafluoroethylene (PTFE) hybrid flat: by the F106 decentralized polyflon of Daikin company, the FR921 polyvinylidene fluoride resin of Shanghai Sanaifu New Material Co., Ltd and benzinum by weight percentage 1:0.06:0.25 evenly mix, 100 hours are left standstill at the temperature of 30 DEG C, then at the temperature of 60 DEG C, 15 hours are left standstill, at 25 DEG C, harder is pressed into cylindrical blank, blank is extruded club by plunger piston extrusion machine at the temperature of 50 DEG C, then at 50 DEG C, base band is rolled into through calender, described base band is carried out longitudinal stretching 4 times in the baking oven of 200 DEG C, carry out the cross directional stretch of 4 times again, finally sinter at 280 DEG C, 20 seconds time, obtain 0.18 micron, aperture, the pore type polytetrafluoroethylene (PTFE) hybrid flat of thickness 18 microns,
(2) cut: the belt type film described pore type polytetrafluoroethylene (PTFE) hybrid flat being cut into width 8 mm wide;
(3) looping: by described belt type film spiral looping 6 layers on carbon fiber knit pipe, obtains fasciated tube;
(4) sinter: described fasciated tube is sintered at 280 DEG C, 60 seconds time, preparation tubular membrane.
Claims (4)
1. pore type polytetrafluoroethylene (PTFE) hybrid flat looping legal system is for a method for hollow-fibre membrane and tubular membrane, and it is characterized in that, the step of the method is as follows:
(1) pore type polytetrafluoroethylene (PTFE) hybrid flat: by decentralized polyflon, polyvinylidene fluoride resin and fluid lubricant by weight percentage 1:0.02-0.08:0.2-0.3 evenly mix, 96 ~ 144 hours are left standstill at the temperature of 20 ~ 40 DEG C, then at the temperature of 40 ~ 80 DEG C, 10 ~ 16 hours are left standstill, at 20 ~ 30 DEG C, harder is pressed into cylindrical blank, blank is extruded club by plunger piston extrusion machine at the temperature of 40 ~ 60 DEG C, then at 40 ~ 60 DEG C, base band is rolled into through calender, described base band is carried out in the baking oven of 180 ~ 300 DEG C longitudinal stretching 1-6 doubly, carry out 2-5 cross directional stretch doubly again, finally sinter at 250-340 DEG C, 10 ~ 30 seconds time, obtain aperture 0.03-0.2 micron, the pore type polytetrafluoroethylene (PTFE) hybrid flat of thickness 5-50 micron,
(2) cut: the belt type film described pore type polytetrafluoroethylene (PTFE) hybrid flat being cut into width 5 ~ 9 mm wide;
(3) looping: by described belt type film spiral looping 1-10 layer on porous tubular support, obtains fasciated tube;
(4) sinter: described fasciated tube is sintered at 260-340 DEG C, time 20-80 second, prepare hollow-fibre membrane and tubular membrane.
2. a kind of pore type polytetrafluoroethylene (PTFE) hybrid flat looping legal system according to claim 1 is for the method for hollow-fibre membrane and tubular membrane, it is characterized in that: the degree of crystallinity of described decentralized polyflon is 98 ~ 99.9%, molecular weight is 2,000,000 ~ 10,000,000.
3. a kind of pore type polytetrafluoroethylene (PTFE) hybrid flat looping legal system according to claim 1 is for the method for hollow-fibre membrane and tubular membrane, it is characterized in that: described fluid lubricant is atoleine, benzinum or kerosene.
4. a kind of pore type polytetrafluoroethylene (PTFE) hybrid flat looping legal system according to claim 1 is for the method for hollow-fibre membrane and tubular membrane, it is characterized in that: described porous tubular support is polytetrafluoroethylhollow hollow fiber membrane, porous ceramic pipe, stainless steel wire woven tube or carbon fiber knit pipe.
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