CN104785130A - Hydrophilic biaxially-oriented polytetrafluoroethylene microporous membrane - Google Patents
Hydrophilic biaxially-oriented polytetrafluoroethylene microporous membrane Download PDFInfo
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- CN104785130A CN104785130A CN201510193688.4A CN201510193688A CN104785130A CN 104785130 A CN104785130 A CN 104785130A CN 201510193688 A CN201510193688 A CN 201510193688A CN 104785130 A CN104785130 A CN 104785130A
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Abstract
The invention relates to the technical field of membranes and particularly provides a hydrophilic biaxially-oriented polytetrafluoroethylene microporous membrane. The water flux of the film is 1200-3000 kg/h.sq.m (1 kilogram force of pressure/sq.cm). A processing method of the hydrophilic biaxially-oriented polytetrafluoroethylene microporous membrane comprises the following steps: mixing materials: uniformly mixing polytetrafluoroethylene resin powder, liquid lubricating oil and inorganic salt powder according to the weight ratio of 1:(0.2-0.28):(0.01-0.2) and leaving to stand at the temperature of 40-80 DEG C for 10-16 hours to form a polytetrafluoroethylene material, wherein the degree of crystallinity of the polytetrafluoroethylene resin powder tested by virtue of differential scanning calorimetry is 98-99.9% and the number-average molecular weight is 2000-10000 thousands; compacting and calendering; longitudinally drawing; transversely drawing and carrying out heat setting. The polytetrafluoroethylene microporous membrane provided by the invention can be formed in one time, and the membrane is endowed with integral hydrophilic performance through the processing method.
Description
Technical field
The present invention relates to the technical field of film, a kind of hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane is provided particularly.
Background technology
The polytetrafluoroethylmicroporous microporous membrane shaping through biaxial tension can form the microstructure of " fibril-node ", be made up of a large amount of micropore, add that polytetrafluoroethylmaterial material itself has acid and alkali-resistance, the characteristic such as corrosion-resistant, high temperature resistant, be therefore widely used in air and water filtration field of purification.But in water filtration field, need hydrophilic film, polytetrafluoroethylene (PTFE) itself has strong-hydrophobicity, therefore needs hydrophilic modifying.At present about the existing a large amount of report of method of PTFE material performing hydrophilic modification on surface.Main method has chemical graft hydrophilic radical method, high-energy radiation (electron beam etc.) initiation grafting hydrophilic radical method, action of plasma to introduce the method such as surface hydroxyl and carboxyl.But there is the technical problems such as apparatus expensive, modified effect be not good in these methods.
Such as CN102872732A (2013-1-16) discloses a kind of hydrophilic modification method of microporous teflon membran, use fluorine-containing polyether glycol solution impregnation microporous teflon membran, then a kind of hydrophilic cross-linking network polyurethane polymer is generated with polyisocyanates in microporous teflon membran polymerisation under certain conditions, and obtained hydrophilic microporous teflon membran, but the overall hydrophily of this film haves much room for improvement.
Summary of the invention
The object of this invention is to provide a kind of can one-shot forming, give the hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane of film integral hydrophilicity.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
A kind of hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane, the water flux of film is 1200-3000 kg/hour square metre (pressure 1 Kilogram Force Per Square Centimeter); The processing method of described polytetrafluoroethylmicroporous microporous membrane comprises the following steps:
(1) batch mixing: teflon resin powder, lubricating oil and inorganic salts powder are mixed evenly by weight for 1:0.2-0.28:0.01-0.2, leaves standstill 10-16 hour at the temperature of 40-80 DEG C, forms 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: described polytetrafluoroethylene (PTFE) base band is carried out longitudinal stretching in the baking oven of 180-300 DEG C, 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.According to processing film technique of the present invention, adopt the method for blended inorganic salts in raw material, inorganic salts provide hydrophily first, and two is that inorganic salts can keep stable, not aging in film manufacturing process.Obtain hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane thus, inorganic salts give film integral hydrophily.In use, inorganic salts can be dissolved in water film, as long as but film is forever placed in water environment, in certain outer pressure, water can continue through film, can not have influence on the usability of film.Owing to adopting blending method, film can one-shot forming, does not need to carry out follow-up modification work.
As preferably, described inorganic salts powder is powdered sodium carbonate or calcium carbonate powder.
Select specific inorganic salts powder, the polytetrafluoroethylmicroporous microporous membrane that hydrophilicity is good can be obtained, and contribute to biaxial tension when preparing.
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 hydrophilic performance, can not reduce aperture because film dimensions is shunk, therefore the horizontal and vertical size of film is kept.
As preferably, described 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 according to mass ratio 1:(1-2 by nanoscale sodium carbonate, mass concentration): (0.02-0.05): (10-30): (0.01-0.03) is placed in closed container, practical Ultrasound Instrument dispersion, suction filtration, form elementary water wetted material, then elementary water wetted material absolute ethyl alcohol is continued suction filtration 10-30 hour, after vacuum drying, obtain nanoscale sodium carbonate water wetted material.
The nanoscale sodium carbonate water wetted material adopting the method to prepare has synergistic function to the polytetrafluoroethylmicroporous microporous membrane that preparation has the good stability of the dimension of excellent hydrophilic and biaxial tension.
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 teflon resin powder, lubricating oil and powdered sodium carbonate in described step (1) is 1:0.25:0.018.
Detailed description of the invention
Embodiment one:
1, batch mixing: the ratio being 1:0.2:0.01 according to weight ratio by teflon resin powder, atoleine, powdered sodium carbonate is mixed evenly, 16 hours are left standstill at the temperature of 40 DEG C, toner is fully mixed with fluid lubricant, 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: by polytetrafluoroethylene (PTFE) base band longitudinal stretching in 180 DEG C of baking ovens, 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, water flux is 1200 kgs/hour square metres (pressure 1 Kilogram Force Per Square Centimeters).
Embodiment two:
1, batch mixing: the ratio being 1:0.28:0.2 according to weight ratio by teflon resin powder, benzinum, powdered sodium carbonate is mixed evenly, 10 hours are left standstill at the temperature of 80 DEG C, toner is fully mixed with fluid lubricant, 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: by polytetrafluoroethylene (PTFE) base band longitudinal stretching in 300 DEG C of baking ovens, obtains 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, water flux is 2500 kgs/hour square metres (pressure 1 Kilogram Force Per Square Centimeters).
Embodiment three:
1, batch mixing: the ratio being 1:0.25:0.1 according to weight ratio by teflon resin powder, kerosene, powdered sodium carbonate is mixed evenly, 12 hours are left standstill at the temperature of 60 DEG C, toner is fully mixed with fluid lubricant, 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: by polytetrafluoroethylene (PTFE) base band longitudinal stretching in 220 DEG C of baking ovens, obtains 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, water flux is 2000 kgs/hour square metres (pressure 1 Kilogram Force Per Square Centimeters).
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, water flux is 2600 kgs/hour square metres (pressure 1 Kilogram Force Per Square Centimeters).
Embodiment five
With embodiment two, 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 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, water flux is 2800 kgs/hour square metres (pressure 1 Kilogram Force Per Square Centimeters).
Embodiment six
With embodiment three, 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 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, water flux is 3000 kgs/hour square metres (pressure 1 Kilogram Force Per Square Centimeters).
Embodiment seven
With embodiment six, select calcium carbonate unlike inorganic salts powder.The polytetrafluoroethylmicroporous microporous membrane material prepared by said method, water flux is 2000 kgs/hour square metres (pressure 1 Kilogram Force Per Square Centimeters).
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 (9)
1. a hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane, is characterized in that: the water flux of described polytetrafluoroethylmicroporous microporous membrane is 1200-3000 kg/hour square metre (pressure 1 Kilogram Force Per Square Centimeter); The processing method of described polytetrafluoroethylmicroporous microporous membrane comprises the following steps:
(1) batch mixing: teflon resin powder, lubricating oil and inorganic salts powder are mixed evenly by weight for 1:0.2-0.28:0.01-0.2, leaves standstill 10-16 hour at the temperature of 40-80 DEG C, forms 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: described polytetrafluoroethylene (PTFE) base band is carried out longitudinal stretching in the baking oven of 180-300 DEG C, 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 hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane according to claim 1, is characterized in that: described inorganic salts powder is powdered sodium carbonate or calcium carbonate powder.
3. a kind of hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane according to claim 2, is characterized in that: described lubricating oil is the one in atoleine, benzinum, kerosene.
4. a kind of hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane 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 hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane according to claim 4, it is characterized in that: described powdered sodium carbonate is nanoscale sodium carbonate water wetted material, concrete preparation method 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 elementary water wetted material, then elementary water wetted material absolute ethyl alcohol is continued suction filtration 10-30 hour, nanoscale sodium carbonate water wetted material is obtained after vacuum drying.
6. a kind of hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane according to claim 5, is characterized in that: after carrying out Ultrasound Instrument dispersion, nitrogen is passed into closed container, is 40-70 DEG C and adds thermal agitation 15-30min, and then carry out suction filtration in temperature.
7. a kind of hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane 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 hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane 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 hydrophily biaxial tension polytetrafluoroethylmicroporous microporous membrane according to claim 5, is characterized in that: the weight ratio of teflon resin powder, lubricating oil and powdered sodium carbonate in described step (1) is 1:0.25:0.018.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111389227A (en) * | 2020-04-26 | 2020-07-10 | 颇尔(河北)环保设备有限公司 | Modified polytetrafluoroethylene hollow fiber membrane and preparation method and application thereof |
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2015
- 2015-04-23 CN CN201510193688.4A patent/CN104785130B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111389227A (en) * | 2020-04-26 | 2020-07-10 | 颇尔(河北)环保设备有限公司 | Modified polytetrafluoroethylene hollow fiber membrane and preparation method and application thereof |
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Address after: 313000, building 10, science and Technology Pioneer Park, eight Li Town, Wuxing District, Huzhou, Zhejiang Patentee after: ZHEJIANG LUCKING ENVIRONMENTAL PROTECTION CO., LTD. Address before: 313000, building 10, science and Technology Pioneer Park, eight Li Town, Wuxing District, Huzhou, Zhejiang Patentee before: HUZHOU LUCKING ENVIRONMENTAL PROTECTION CO., LTD. |
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Address after: 313000 building 10, science and Technology Pioneer Park, eight Li Dian Town, Wuxing District, Huzhou, Zhejiang. Patentee after: Zhejiang green net environmental protection Polytron Technologies Inc Address before: 313000 building 10, science and Technology Pioneer Park, eight Li Dian Town, Wuxing District, Huzhou, Zhejiang. Patentee before: ZHEJIANG LUCKING ENVIRONMENTAL PROTECTION CO., LTD. |