CN104802429A - Method for improving porosity rate of two-way stretching polytetrafluoroethylene micropore thin film - Google Patents
Method for improving porosity rate of two-way stretching polytetrafluoroethylene micropore thin film Download PDFInfo
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- CN104802429A CN104802429A CN201510193726.6A CN201510193726A CN104802429A CN 104802429 A CN104802429 A CN 104802429A CN 201510193726 A CN201510193726 A CN 201510193726A CN 104802429 A CN104802429 A CN 104802429A
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Abstract
The invention relates to the technical field of thin films, and particularly provides a method for improving the porosity rate of a two-way stretching polytetrafluoroethylene micropore thin film. The method comprises the following steps: (1) mixing materials: uniformly mixing polytetrafluoroethylene resin powder and liquid lubricating oil according to the weight ratio of 1:(0.2-0.28), performing still standing for 10-16 h at the temperature of 40-80 DEG C, so as to form a polytetrafluoroethylene material; (2) compaction and calendering: compacting the polytetrafluoroethylene material into cylindrical blank at the temperature of 30-50 DEG C, squeezing the blank into rod-like material through a compactor at the temperature of 40-60 DEG C, and then calendering into a polytetrafluoroethylene baseband through a calender at the temperature of 40-60 DEG C; (3) longitudinal stretching and water vapor treatment: conducting longitudinal stretching on the polytetrafluoroethylene baseband at 180-300 DEG C, and then conducting water vapor treatment for 0.5-5 min, so as to obtain a defatted baseband; (4) transversal stretching and heat shaping: conducting transversal stretching on the defatted baseband at 180-210 DEG C, then conducting sintering shaping at 250-380 DEG C with the sintering time of 20-80 s, so as to obtain the heat-shaped thin film. According to the method, the porosity rate can reach up to 86-92%, the process is simple, and the cost is low.
Description
Technical field
The present invention relates to the technical field of film, a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity is provided particularly.
Background technology
Be the high-tech product integrating the functions such as waterproof, moisture-inhibiting, Air permenbility be large through the polytetrafluoroethylmicroporous microporous membrane that biaxial tension is shaping, this film is widely used in the field such as function clothes, dedusting.To the film for dust removal field, for ensureing large air flux, porosity should be tried one's best height.At disclosed patent such as ZL200510061828.9, ZL200710069975.X, be generally teflon resin powder and lubricating oil is mixed, pressed compact, calendering, longitudinal stretching, the operation such as cross directional stretch and thermal finalization complete.Facts have proved, through the film that above-mentioned operation is processed, porosity is lower.
Summary of the invention
The object of this invention is to provide a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
Improve a method for biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity,
Comprise the following steps:
(1) batch mixing: teflon resin powder, lubricating oil are mixed evenly by weight for 1:0.2-0.28, leave standstill 10-16 hour at the temperature of 40-80 DEG C, form polytetrafluoroethylene (PTFE) material; The differential scanning calorimetry test degree of crystallinity of described teflon resin powder is 98-99.9%, number-average molecular weight is 200-1000 ten thousand;
(2) pressed compact and calendering: by described polytetrafluoroethylene (PTFE) material at 30-50 DEG C, harder is pressed into cylindrical blank, blank is extruded club by pushing machine at the temperature of 40-60 DEG C, then at 40-60 DEG C, is rolled into polytetrafluoroethylene (PTFE) base band through calender;
(3) longitudinal stretching and steam treatment: described polytetrafluoroethylene (PTFE) base band is carried out longitudinal stretching in the baking oven of 180-300 DEG C, then through steam treatment 0.5-5min, obtains degreasing base band;
(4) cross directional stretch and thermal finalization: by described degreasing base band cross directional stretch at 180-210 DEG C, then 250-380 DEG C of sintering sizing, sintering time 20-80 second, obtains heat-setting thin-film.
Teflon resin powder can adopt commercially available prod, as the product of Daikin company F106, Japan AGC company CD123.Polytetrafluoroethylene (PTFE) has can form fibril under shear action, can form the microstructure of " fibril-node ", form a large amount of micropore thus under stretching action.Polytetrafluoroethylene (PTFE) forms fibril under shear action, and under super drawing, fibril is extending, and the present invention proposes method for steam treatment, steam treatment makes polytetrafluoroethylene (PTFE) deliquescing, in follow-up cross directional stretch process, fibril more easily extends, and therefore obtains high porosity.As preferably, under pressure is 0.5-0.8MPa, carry out steam treatment 0.5-5min.
As preferably, described lubricating oil is the one in atoleine, benzinum, kerosene.
As preferably, the processing method of described polytetrafluoroethylmicroporous microporous membrane also comprises described heat-setting thin-film spraying cooling water, obtain film lateral shrinkage and be less than 2% and the longitudinal contraction rate polytetrafluoroethylmicroporous microporous membrane that is less than 3%, concrete spraying method is described cooling water temperature is 10-20 DEG C, cool water shower time 5-20 second, hydraulic pressure 1000-10000 handkerchief, makes the film after thermal finalization be down to rapidly 20 DEG C.
Owing to adopting cold water process after film thermal sizing, reduce film temperature rapidly, cool time is short, effective, and technique is simple, and processing cost is low; In use or storing process, while maintenance good porosity performance, can not reduce aperture because film dimensions is shunk, therefore the horizontal and vertical size of film is kept.
As preferably, also comprise during described step (1) batch mixing and add 0.01-0.2 weight portion nanoscale sodium carbonate material, the concrete preparation method of nanoscale sodium carbonate material is: by nanoscale sodium carbonate, mass concentration is the ethanol of 95%, hydrazine hydrate solution, dodecyl sodium sulfate and crown ether are according to mass ratio 1:(1-2): (0.02-0.05): (10-30): (0.01-0.03) is placed in closed container, practical Ultrasound Instrument dispersion, suction filtration, form primary material, then elementary water wetted material absolute ethyl alcohol is continued suction filtration 10-30 hour, nanoscale sodium carbonate material is obtained after vacuum drying.
Adopt that the nanoscale sodium carbonate water wetted material prepared of the method has good porosity to preparation, the polytetrafluoroethylmicroporous microporous membrane of dimensional stability of hydrophily and biaxial tension has synergistic function, this may be because this component is to improving steam treatment thus to improve the microstructure of polytetrafluoroethylene fibrils-node helpful.
As preferably, after carrying out Ultrasound Instrument dispersion, nitrogen is passed into closed container, be 40-70 DEG C in temperature and add thermal agitation 15-30min.
As preferably, described nanoscale sodium carbonate, mass concentration be 95% ethanol, hydrazine hydrate solution, dodecyl sodium sulfate and crown ether mass ratio be 1:1.5:0.04:16:0.02.
As preferably, in described batch mixing step with also comprise soft-bake step between pressed compact and calendaring processes, the insulating box specifically described polytetrafluoroethylene (PTFE) material being placed in 30-40 DEG C leaves standstill 12-24h.Soft-bake step can improve the stability of film hydrophilic performance and bidirectional size.
As preferably, the weight ratio of the teflon resin powder in described step (1), lubricating oil and nano-calcium carbonate sodium powder is 1:0.25:0.018.
Detailed description of the invention
Embodiment one:
1, batch mixing: the ratio being 1:0.2 according to weight ratio by teflon resin powder, atoleine is mixed evenly, leaves standstill 16 hours, toner is fully mixed with fluid lubricant at the temperature of 40 DEG C, forms polytetrafluoroethylene (PTFE) material;
2, pressed compact and calendering: polytetrafluoroethylene (PTFE) material is pressed into cylindrical blank at 30 DEG C on harder, extrudes club by pushing machine by blank, then at 40 DEG C, is rolled into polytetrafluoroethylene (PTFE) base band through calender at the temperature of 40 DEG C;
3, longitudinal stretching and steam treatment: by described polytetrafluoroethylene (PTFE) base band longitudinal stretching in 180 DEG C of baking ovens, then through steam treatment 30 seconds, obtains degreasing base band;
4, cross directional stretch and thermal finalization: by described degreasing base band cross directional stretch at 180 DEG C, then 380 DEG C of sintering sizings, sintering time 20 seconds, obtains heat-setting thin-film.
By hydrophilic polyfluortetraethylemicroporous microporous film material prepared by said method, film porosity reaches 86%.
Embodiment two:
1, batch mixing: the ratio being 1:0.28 according to weight ratio by teflon resin powder, benzinum is mixed evenly, leaves standstill 10 hours, toner is fully mixed with fluid lubricant at the temperature of 80 DEG C, forms polytetrafluoroethylene (PTFE) material;
2, pressed compact and calendering: polytetrafluoroethylene (PTFE) material is pressed into cylindrical blank at 50 DEG C on harder, extrudes club by pushing machine by blank, then at 60 DEG C, is rolled into polytetrafluoroethylene (PTFE) base band through calender at the temperature of 60 DEG C;
3, longitudinal stretching and and steam treatment: by described polytetrafluoroethylene (PTFE) base band longitudinal stretching in 300 DEG C of baking ovens, then through steam treatment 5 minutes, obtain degreasing base band;
4, cross directional stretch and thermal finalization: by described degreasing base band cross directional stretch at 210 DEG C, then 250 DEG C of sintering sizings, sintering time 80 seconds, obtains heat-setting thin-film;
The polytetrafluoroethylmicroporous microporous membrane material prepared by said method, film porosity reaches 88%.
Embodiment three:
1, batch mixing: the ratio being 1:0.25 according to weight ratio by teflon resin powder, kerosene is mixed evenly, leaves standstill 12 hours, toner is fully mixed with fluid lubricant at the temperature of 60 DEG C, forms polytetrafluoroethylene (PTFE) material;
2, pressed compact and calendering: polytetrafluoroethylene (PTFE) material is pressed into cylindrical blank at 40 DEG C on harder, extrudes club by pushing machine by blank, then at 50 DEG C, is rolled into polytetrafluoroethylene (PTFE) base band through calender at the temperature of 50 DEG C;
3, longitudinal stretching and steam treatment: by described polytetrafluoroethylene (PTFE) base band longitudinal stretching in 220 DEG C of baking ovens, then through steam treatment 1 minute, obtain degreasing base band;
4, cross directional stretch and thermal finalization: by described degreasing base band cross directional stretch at 200 DEG C, then 280 DEG C of sintering sizings, sintering time 60 seconds, obtains heat-setting thin-film;
The polytetrafluoroethylmicroporous microporous membrane material prepared by said method, film porosity reaches 90%.
Embodiment four
With embodiment one, the weight ratio unlike teflon resin powder, lubricating oil and powdered sodium carbonate is 1:0.25:0.018.
In batch mixing step with also comprise soft-bake step between pressed compact and calendaring processes, the insulating box specifically described polytetrafluoroethylene (PTFE) material being placed in 30 DEG C leaves standstill 12h.
By heat-setting thin-film spraying cooling water after thermal finalization, obtain film lateral shrinkage and be less than 2% and the longitudinal contraction rate polytetrafluoroethylmicroporous microporous membrane that is less than 3%, concrete spraying method is described cooling water temperature is 10 DEG C, 5 seconds cool water shower time, hydraulic pressure 1000 handkerchief, makes the film after thermal finalization be down to rapidly 20 DEG C.
Powdered sodium carbonate is nanoscale sodium carbonate water wetted material, concrete preparation method is: be that the ethanol of 95%, hydrazine hydrate solution, dodecyl sodium sulfate and crown ether are placed in closed container according to mass ratio 1:1:0.02:10:0.03 by nanoscale sodium carbonate, mass concentration, practical Ultrasound Instrument dispersion, nitrogen is passed into closed container, is 40 DEG C in temperature and adds thermal agitation 15min; Suction filtration, forms elementary water wetted material, then elementary water wetted material absolute ethyl alcohol is continued suction filtration 10 hours, obtains nanoscale sodium carbonate water wetted material after vacuum drying.
The polytetrafluoroethylmicroporous microporous membrane material prepared by said method, film porosity reaches 91%.
Embodiment five
With embodiment two, be mixed evenly unlike the ratio being 1:0.2:0.01 according to weight ratio by teflon resin powder, atoleine, powdered sodium carbonate.
In batch mixing step with also comprise soft-bake step between pressed compact and calendaring processes, the insulating box specifically described polytetrafluoroethylene (PTFE) material being placed in 40 DEG C leaves standstill 24h.
By heat-setting thin-film spraying cooling water after thermal finalization, obtain film lateral shrinkage and be less than 2% and the longitudinal contraction rate polytetrafluoroethylmicroporous microporous membrane that is less than 3%, concrete spraying method is described cooling water temperature is 20 DEG C, 20 seconds cool water shower time, hydraulic pressure 10000 handkerchief, makes the film after thermal finalization be down to rapidly 20 DEG C.
Powdered sodium carbonate is nanoscale sodium carbonate water wetted material, concrete preparation method is: be that the ethanol of 95%, hydrazine hydrate solution, dodecyl sodium sulfate and crown ether are placed in closed container according to mass ratio 1:2:0.05:30:0.01 by nanoscale sodium carbonate, mass concentration, practical Ultrasound Instrument dispersion, nitrogen is passed into closed container, is 70 DEG C in temperature and adds thermal agitation 30min; Suction filtration, forms elementary water wetted material, then elementary water wetted material absolute ethyl alcohol is continued suction filtration 10-30 hour, obtains nanoscale sodium carbonate water wetted material after vacuum drying.
The polytetrafluoroethylmicroporous microporous membrane material prepared by said method, film porosity reaches 92%.
Embodiment six
With embodiment three, be mixed evenly unlike the ratio being 1:0.28:0.2 according to weight ratio by teflon resin powder, benzinum, powdered sodium carbonate.
In batch mixing step with also comprise soft-bake step between pressed compact and calendaring processes, the insulating box specifically described polytetrafluoroethylene (PTFE) material being placed in 38 DEG C leaves standstill 20h.
By heat-setting thin-film spraying cooling water after thermal finalization, obtain film lateral shrinkage and be less than 2% and the longitudinal contraction rate polytetrafluoroethylmicroporous microporous membrane that is less than 3%, concrete spraying method is described cooling water temperature is 15 DEG C, 12 seconds cool water shower time, hydraulic pressure 8000 handkerchief, makes the film after thermal finalization be down to rapidly 20 DEG C.
Powdered sodium carbonate is nanoscale sodium carbonate water wetted material, concrete preparation method is: be that the ethanol of 95%, hydrazine hydrate solution, dodecyl sodium sulfate and crown ether are placed in closed container according to mass ratio 1:1.5:0.04:16:0.02 by nanoscale sodium carbonate, mass concentration, practical Ultrasound Instrument dispersion, nitrogen is passed into closed container, is 50 DEG C in temperature and adds thermal agitation 20min; Suction filtration, forms elementary water wetted material, then elementary water wetted material absolute ethyl alcohol is continued suction filtration 20 hours, obtains nanoscale sodium carbonate water wetted material after vacuum drying.
The polytetrafluoroethylmicroporous microporous membrane material prepared by said method, film porosity reaches 92%.
This specific embodiment is only explanation of the invention; it is not limitation of the present invention; those skilled in the art can make to the present embodiment the amendment not having creative contribution as required after reading this description, as long as but be all subject to the protection of Patent Law in right of the present invention.
Claims (10)
1. improve a method for biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity, it is characterized in that comprising the following steps:
(1) batch mixing: teflon resin powder, lubricating oil are mixed evenly by weight for 1:0.2-0.28, leave standstill 10-16 hour at the temperature of 40-80 DEG C, form polytetrafluoroethylene (PTFE) material; The differential scanning calorimetry test degree of crystallinity of described teflon resin powder is 98-99.9%, number-average molecular weight is 200-1000 ten thousand;
(2) pressed compact and calendering: by described polytetrafluoroethylene (PTFE) material at 30-50 DEG C, harder is pressed into cylindrical blank, blank is extruded club by pushing machine at the temperature of 40-60 DEG C, then at 40-60 DEG C, is rolled into polytetrafluoroethylene (PTFE) base band through calender;
(3) longitudinal stretching and steam treatment: described polytetrafluoroethylene (PTFE) base band is carried out longitudinal stretching in the baking oven of 180-300 DEG C, then through steam treatment 0.5-5min, obtains degreasing base band;
(4) cross directional stretch and thermal finalization: by described degreasing base band cross directional stretch at 180-210 DEG C, then 250-380 DEG C of sintering sizing, sintering time 20-80 second, obtains heat-setting thin-film.
2. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to claim 1, is characterized in that: described lubricating oil is the one in atoleine, benzinum, kerosene.
3. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to claim 2, is characterized in that: under pressure is 0.5-0.8MPa, carry out steam treatment 0.5-5min.
4. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to claim 3, it is characterized in that: the processing method of described polytetrafluoroethylmicroporous microporous membrane also comprises described heat-setting thin-film spraying cooling water, obtain film lateral shrinkage and be less than 2% and the longitudinal contraction rate polytetrafluoroethylmicroporous microporous membrane that is less than 3%, concrete spraying method is described cooling water temperature is 10-20 DEG C, cool water shower time 5-20 second, hydraulic pressure 1000-10000 handkerchief, makes the film after thermal finalization be down to rapidly 20 DEG C.
5. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to claim 4, it is characterized in that: also comprise during described step (1) batch mixing and add 0.01-0.2 weight portion nanoscale sodium carbonate material, the concrete preparation method of nanoscale sodium carbonate material is: by nanoscale sodium carbonate, mass concentration is the ethanol of 95%, hydrazine hydrate solution, dodecyl sodium sulfate and crown ether are according to mass ratio 1:(1-2): (0.02-0.05): (10-30): (0.01-0.03) is placed in closed container, practical Ultrasound Instrument dispersion, suction filtration, form primary material, then elementary water wetted material absolute ethyl alcohol is continued suction filtration 10-30 hour, nanoscale sodium carbonate material is obtained after vacuum drying.
6. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to claim 5, it is characterized in that: after carrying out Ultrasound Instrument dispersion, nitrogen is passed into closed container, is 40-70 DEG C in temperature and adds thermal agitation 15-30min, and then carry out suction filtration.
7. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to claim 6, is characterized in that: described nanoscale sodium carbonate, mass concentration be 95% ethanol, hydrazine hydrate solution, dodecyl sodium sulfate and crown ether mass ratio be 1:1.5:0.04:16:0.02.
8. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to any one of claim 1-7, it is characterized in that: in described batch mixing step with also comprise soft-bake step between pressed compact and calendaring processes, the insulating box specifically described polytetrafluoroethylene (PTFE) material being placed in 30-40 DEG C leaves standstill 12-24h.
9. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to claim 5, is characterized in that: the weight ratio of the teflon resin powder in described step (1), lubricating oil and nano-calcium carbonate sodium powder is 1:0.25:0.018.
10. a kind of method improving biaxial tension polytetrafluoroethylmicroporous microporous membrane porosity according to any one of claim 1-9, is characterized in that: described polytetrafluoroethylmicroporous microporous membrane porosity is 86-92%.
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| CN105331024A (en) * | 2015-11-23 | 2016-02-17 | 安徽国泰印务有限公司 | Flame-retardant calendered film and production process thereof |
| CN105694311A (en) * | 2016-03-29 | 2016-06-22 | 苏颖颖 | Preparation method of two-way stretching waterproof polytetrafluoroethylene film |
| CN105835383A (en) * | 2016-05-12 | 2016-08-10 | 武汉纺织大学 | Manufacturing method for two-way-stretching nylon fiber porous film |
| 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 |
| CN107487005A (en) * | 2017-07-25 | 2017-12-19 | 浙江理工大学 | A kind of preparation method of unsymmetric structure polytetrafluoroethylene (PTFE) micro-pore aeration film |
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| CN105331024A (en) * | 2015-11-23 | 2016-02-17 | 安徽国泰印务有限公司 | Flame-retardant calendered film and production process thereof |
| CN105694311A (en) * | 2016-03-29 | 2016-06-22 | 苏颖颖 | Preparation method of two-way stretching waterproof polytetrafluoroethylene film |
| CN105835383A (en) * | 2016-05-12 | 2016-08-10 | 武汉纺织大学 | Manufacturing method for two-way-stretching nylon fiber porous film |
| CN108295667A (en) * | 2017-01-13 | 2018-07-20 | 宁波大学 | A kind of positive osmosis composite membrane and preparation method thereof based on large aperture basement membrane |
| 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 |
| CN107487005A (en) * | 2017-07-25 | 2017-12-19 | 浙江理工大学 | A kind of preparation method of unsymmetric structure polytetrafluoroethylene (PTFE) micro-pore aeration film |
| CN108189435A (en) * | 2018-01-19 | 2018-06-22 | 全椒光太胶粘制品有限公司 | A kind of Medical isolating film material quick forming fabri-cation technique |
| CN108579432A (en) * | 2018-05-21 | 2018-09-28 | 宁波通冠电气自动化设备有限公司 | A kind of preparation method, filter core and the filtration system of the reverse osmosis PTFE film of ultrafiltration micropore |
| CN109192818A (en) * | 2018-09-08 | 2019-01-11 | 佛山皖和新能源科技有限公司 | A kind of method that evening chemical corrosion prepares polycrystalline silicon suede |
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| CN111793244B (en) * | 2020-07-22 | 2022-12-27 | 苏州天澜生物材料科技有限公司 | Supermolecule perfluoro gel and preparation method thereof |
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