CN112619451B - Preparation method of hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane - Google Patents
Preparation method of hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane Download PDFInfo
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- CN112619451B CN112619451B CN202011360252.7A CN202011360252A CN112619451B CN 112619451 B CN112619451 B CN 112619451B CN 202011360252 A CN202011360252 A CN 202011360252A CN 112619451 B CN112619451 B CN 112619451B
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- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 69
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 69
- 239000012528 membrane Substances 0.000 title claims abstract description 62
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 31
- 238000001471 micro-filtration Methods 0.000 title claims abstract description 24
- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims description 34
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 230000006835 compression Effects 0.000 claims description 11
- 238000007906 compression Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000011148 porous material Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 238000007598 dipping method Methods 0.000 claims description 7
- 239000006184 cosolvent Substances 0.000 claims description 6
- 239000003350 kerosene Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- BHTJEPVNHUUIPV-UHFFFAOYSA-N pentanedial;hydrate Chemical compound O.O=CCCCC=O BHTJEPVNHUUIPV-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000010687 lubricating oil Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 abstract description 14
- 238000012986 modification Methods 0.000 abstract description 14
- 230000002045 lasting effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 229920002521 macromolecule Polymers 0.000 abstract description 2
- 238000004804 winding Methods 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 230000004907 flux Effects 0.000 description 11
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- CNPVJWYWYZMPDS-UHFFFAOYSA-N 2-methyldecane Chemical compound CCCCCCCCC(C)C CNPVJWYWYZMPDS-UHFFFAOYSA-N 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the technical field of material surface modification, and particularly relates to a preparation method of a hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane. According to the invention, PVA is adopted to carry out hydrophilic modification on the PTFE micro-filtration membrane, PVA macromolecules can be inserted into the nodes of the PTFE micro-filtration membrane and are tightly combined with PTFE through physical winding action, so that a compact hydrophilic modification layer is formed on the surface of the membrane, the hydrophilicity of the membrane is improved, and then the membrane is immersed in glutaraldehyde and dried, so that PVA molecules are fully crosslinked on the surface of a PTFE hollow tube, the hydrophilic stability of the membrane is improved, and the purpose of lasting hydrophilic is achieved.
Description
Technical Field
The invention belongs to the technical field of material surface modification, and particularly relates to a preparation method of a hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane.
Background
Polytetrafluoroethylene (PTFE) microfiltration membranes have found wide application in the fields of chemical, pharmaceutical, wastewater treatment, and the like due to their excellent physical and chemical properties. At present, the PTFE hollow fiber microfiltration membrane is mostly manufactured through the procedures of prepressing, stretching, high-temperature sintering and the like, and in the preparation process, the compression ratio, the stretching multiplying power, the sintering temperature, the sintering time and the like can influence the separation performance of the membrane, so that the parameters are controlled in proper ranges to be particularly important. Meanwhile, PTFE has limited its application in the field of liquid separation due to its strong hydrophobicity, and its surface must be hydrophilically modified.
The hydrophilic modification method of the PTEF microfiltration membrane surface in the prior art mainly comprises chemical and physical modification, high-energy radiation grafting modification, plasma treatment modification, high-temperature melting, filling modification and the like, and the main defects of the method are that the surface of the membrane after surface modification is poor in hydrophilicity and unstable. Therefore, development of a novel hydrophilic modification method is needed to prepare a high-performance PTFE hollow fiber microfiltration membrane.
Disclosure of Invention
The invention aims at solving the problems in the prior art and provides a preparation method of a hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane, wherein the microfiltration membrane prepared by the preparation method has higher porosity, pure water flux and lasting hydrophilicity.
The above object of the present invention can be achieved by the following technical solutions: a method for preparing a hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane, which comprises the following steps:
s1, mixing polytetrafluoroethylene resin with a cosolvent, and uniformly stirring to obtain a mixture;
s2, pre-pressing the mixture obtained in the step S1 into a cylinder shape, and extruding the cylinder shape into a PTFE solid hollow tube;
s3, stretching and sintering the solid hollow tube obtained in the step S2 to prepare a porous PTFE hollow tube;
s4, dipping and coating the porous PTFE hollow tube obtained in the step S3 with a hydrophilic polyvinyl alcohol (PVA) aqueous solution, drying, dipping in a glutaraldehyde aqueous solution, and drying to obtain the durable hydrophilic PTFE hollow fiber microfiltration membrane.
According to the invention, PVA is adopted to carry out hydrophilic modification on the PTFE micro-filtration membrane, PVA macromolecules can be inserted into the nodes of the PTFE micro-filtration membrane and are tightly combined with PTFE through physical winding action, so that a compact hydrophilic modification layer is formed on the surface of the membrane, the hydrophilicity of the membrane is improved, and then the membrane is immersed in glutaraldehyde and dried, so that PVA molecules are fully crosslinked on the surface of a PTFE hollow tube, the hydrophilic stability of the membrane is improved, and the purpose of lasting hydrophilic is achieved.
Preferably, the cosolvent in the step S1 is at least one of kerosene and lubricating oil (Isopar G).
Preferably, in the step S1, the mass fraction of the polytetrafluoroethylene resin is 60-85%, and the mass fraction of the cosolvent is 15-40%.
Preferably, the extrusion compression ratio at the extrusion in the step S2 is 450-580.
Preferably, the sintering temperature of the stretch sintering in the step S3 is 220-290 ℃, the sintering time is 1-5min, the stretching multiplying power is 2.2-2.8, the stretching temperature is 60-80 ℃, and the stretching rate is 3-6m/min. The porosity of the film produced under this condition is high.
Preferably, the PVA concentration in the step S4 is 1-1.5%, the dipping time is 1.5-3h, and the temperature is 55-65 ℃.
Preferably, in the step S4, the concentration of glutaraldehyde in the glutaraldehyde aqueous solution is 1-5%, the pH value of the glutaraldehyde aqueous solution is 1-2, the soaking time is 1.5-3h, and the temperature is 55-65 ℃. Glutaraldehyde can exert a crosslinking effect at a certain acidity.
Preferably, the PTFE hollow fiber microfiltration membrane prepared in the step S4 has a pore diameter of 0.1-0.4 μm and a porosity of 40-50%.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts stretching sintering of a specific process to prepare the PTFE hollow fiber microfiltration membrane, and obtains permanent hydrophilicity after PVA hydrophilic modification and glutaraldehyde further crosslinking. The membrane prepared by the process has the characteristics of higher porosity, pure water flux and lasting hydrophilicity.
Detailed Description
The following are specific examples of the present invention and illustrate the technical scheme of the present invention, but the present invention is not limited to these examples. Unless otherwise indicated, all materials used in the examples of the present invention are those commonly used in the art, and all methods used in the examples are those commonly used in the art.
Example 1
Weighing 60% PTFE resin (raw materials are from Japanese Dajin) and 40% kerosene according to mass percentage, mixing and melting, pre-pressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 450, and extruding a hollow tube; stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 2.2, the stretching temperature is 60 ℃, the sintering temperature is 220 ℃, the sintering time is 1min, the stretching speed is 3m/min, and finally the PTFE hollow fiber membrane with the pore diameter of 0.1-0.4 mu m and the porosity of 40% is obtained;
soaking the prepared PTFE hollow fiber membrane in industrial alcohol, taking out, soaking in 1% PVA water solution at 55deg.C for 1.5 hr, then soaking in 1% glutaraldehyde water solution, adjusting pH to 2, soaking at 50deg.C for 1.5 hr, and then soaking in clear water for washingThe method comprises the steps of carrying out a first treatment on the surface of the Finally, the film is dried at a low temperature of 30 ℃ for standby. The pure water flux of the modified PTFE membrane measured at 0.1MPa is 4560L/m 2 h。
Example 2
Weighing 70% PTFE resin (raw materials are from Japanese Dajin) and 30% isopar G according to mass percentage, mixing and melting, pre-pressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 468, and extruding a hollow tube; stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 2.3, the stretching temperature is 65 ℃, the sintering temperature is 280 ℃, the sintering time is 2min, the stretching speed is 3.5m/min, and finally the PTFE hollow fiber membrane with the pore diameter of 0.1-0.4 mu m and the porosity of 42% is obtained;
putting the prepared PTFE hollow fiber membrane into industrial alcohol for full infiltration, taking out, putting into 1.2% PVA aqueous solution, soaking for 2 hours at 60 ℃, then putting into 2% glutaraldehyde aqueous solution, adjusting the pH value to be 1, soaking for 2 hours at 60 ℃, then putting into clear water for soaking and washing, and finally drying the membrane at 35 ℃ for later use. The pure water flux of the modified PTFE membrane measured at 0.1MPa is 5760L/m 2 h。
Example 3
Weighing 80% PTFE resin (raw materials are from Japanese Dajin) and 20% isopar G according to mass percentage, mixing and melting, pre-pressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 500, and extruding a hollow tube; stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 2.5, the stretching temperature is 80 ℃, the sintering temperature is 270 ℃, the sintering time is 3min, the stretching speed is 4m/min, and finally the PTFE hollow fiber membrane with the pore diameter of 0.1-0.4 mu m and the porosity of 50% is obtained;
putting the prepared PTFE hollow fiber membrane into industrial alcohol for full infiltration, taking out, putting into 1.5% PVA aqueous solution, soaking for 2h at 60 ℃, then putting into 5% glutaraldehyde aqueous solution, adjusting the pH value to be 1, soaking for 1.5h at 60 ℃, then putting into clear water for soaking and washing, and finally drying the membrane at a low temperature of 40 ℃ for standby. The pure water flux of the modified PTFE membrane measured at 0.1MPa is 6420L/m 2 h。
Example 4
Weighing 65% PTFE resin (raw materials are from Japanese Dajin) and 35% kerosene according to mass percentage, mixing and melting, pre-pressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 520, and extruding a hollow tube; stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 2.6, the stretching temperature is 80 ℃, the sintering temperature is 280 ℃, the sintering time is 4min, the stretching speed is 1m/min, and finally the PTFE hollow fiber membrane with the pore diameter of 0.1-0.4 mu m and the porosity of 45% is obtained;
putting the prepared PTFE hollow fiber membrane into industrial alcohol for full infiltration, taking out, putting into 1% PVA aqueous solution, soaking for 1.5h at 60 ℃, then putting into 3% glutaraldehyde aqueous solution, adjusting the pH value to be 1, soaking for 1.5h at 60 ℃, then putting into clear water for soaking and washing, and finally drying the membrane at low temperature of 30 ℃ for later use. Pure water flux of 5460L/m for 0.1MPa measurement of modified PTFE film 2 h。
Example 5
Weighing 80% PTFE resin (raw materials are from Japanese big gold) and 20% isopar G according to mass percentage, mixing and melting, pre-pressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 580, and extruding a hollow tube; stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 2.8, the stretching temperature is 70 ℃, the sintering temperature is 290 ℃, the sintering time is 5min, the stretching speed is 6m/min, and finally the PTFE hollow fiber membrane with the pore diameter of 0.1-0.4 mu m and the porosity of 43% is obtained;
putting the prepared PTFE hollow fiber membrane into industrial alcohol for full infiltration, taking out, putting into 1% PVA water solution for soaking for 3 hours at 60 ℃, then putting into 1% glutaraldehyde water solution, adjusting the pH value to be 2, soaking for 3 hours at 60 ℃, then putting into clear water for soaking and washing, and finally drying the membrane at a low temperature of 40 ℃ for standby. The pure water flux of the modified PTFE membrane measured at 0.1MPa is 5720L/m 2 h。
Comparative example 1
The method comprises the steps of weighing 90% of PTFE resin (raw materials are from Japanese big gold) according to the mass percentage, mixing and melting with 10% of isopar G, prepressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 361, and extruding a hollow tube. And (3) stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 3.2, the stretching temperature is 30 ℃, the sintering temperature is 320 ℃, and the stretching speed is 1m/min, so that the PTFE hollow fiber membrane with a certain pore diameter and porosity is finally obtained. The porosity of the obtained PTFE membrane was measured to be 30%, and the pure water flux was measured to be 0.
Putting the prepared PTFE hollow fiber membrane into industrial alcohol for full infiltration, taking out, putting into 1.5% PVA aqueous solution, soaking for 2h at 60 ℃, then putting into 5% glutaraldehyde aqueous solution, adjusting the pH value to be 1, soaking for 1.5h at 60 ℃, then putting into clear water for soaking and washing, and finally drying the membrane at a low temperature of 40 ℃ for standby. Pure water flux of 1230L/m for 0.1MPa measurement of modified PTFE film 2 h, which is far lower than the membrane flux prepared by the invention.
Comparative example 2
Weighing 80% PTFE resin (raw materials are from Japanese Dajin) and 20% isopar G according to mass percentage, mixing and melting, pre-pressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 500, and extruding a hollow tube; stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 2.5, the stretching temperature is 80 ℃, the sintering temperature is 270 ℃, the stretching speed is 4m/min, and finally the PTFE hollow fiber membrane with the pore diameter of 0.1-0.4 mu m and the porosity of 50% is obtained;
without hydrophilic modification, PTFE cannot be filtered at all and water cannot pass through the pores of the membrane surface.
Comparative example 3
PTFE resin is weighed and SiO accounting for 1 percent of the total amount of the materials is added 2 Nanoparticle, mixing with resin, and adding SiO-containing agent 2 Mixing and melting PTFE resin and Isopar G of the nano particles according to the mass percentages of 80% and 20%, pre-pressing a uniformly mixed and melted sample, putting the sample into an extruder, setting the compression ratio to be 500, and extruding a hollow tube; stretching and sintering the hollow tube, wherein the stretching multiplying power is set to be 2.5, the stretching temperature is 80 ℃, the sintering temperature is 270 ℃, the sintering time is 3min, the stretching speed is 4m/min, and finally the PTFE hollow fiber membrane with the pore diameter of 0.3-0.7 and the porosity of 35 percent is obtained, and the hollow fiber microfiltration membrane is added with SiO 2 Nanoparticles, which have improved hydrophilicity per se, have PTFE measured at 0.1MPaThe pure water flux of the membrane is 1240L/m only 2 h, which is far lower than the hydrophilic modified film prepared by the invention.
The embodiments herein are not exhaustive of the values of points in the technical scope of the invention claimed, and new technical solutions formed by equivalent substitution of single or multiple technical features in the technical solutions of the embodiments are also within the scope of the invention claimed, and all the parameters involved in the solutions of the invention are not mutually and non-replaceable unique combinations unless specifically stated.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (3)
1. The preparation method of the hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane is characterized by comprising the following steps of:
s1, mixing polytetrafluoroethylene resin with a cosolvent, and uniformly stirring to obtain a mixture;
s2, pre-pressing the mixture obtained in the step S1 into a cylinder shape, and extruding the cylinder shape into a PTFE solid hollow tube;
s3, stretching and sintering the solid hollow tube obtained in the step S2 to prepare a porous PTFE hollow tube;
s4, dipping and coating the porous PTFE hollow tube obtained in the step S3 with a hydrophilic polyvinyl alcohol aqueous solution, drying, dipping in a glutaraldehyde aqueous solution, and drying to obtain a durable hydrophilic PTFE hollow fiber microfiltration membrane;
in the step S1, the mass fraction of the polytetrafluoroethylene resin is 60-85%, and the mass fraction of the cosolvent is 15-40%;
the pushing compression ratio in the step S2 is 450-580;
the sintering temperature of the stretch sintering in the step S3 is 220-290 ℃, the sintering time is 1-5min, the stretching multiplying power is 2.2-2.8, the stretching temperature is 60-80 ℃, and the stretching rate is 3-6m/min;
the PVA concentration in the step S4 is 1-1.5%, the dipping time is 1.5-3h, the temperature is 55-65 ℃, the glutaraldehyde concentration in glutaraldehyde water solution is 1-5%, the pH value of glutaraldehyde water solution is 1-2, the dipping time is 1.5-3h, and the temperature is 50-60 ℃.
2. The method for preparing a hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane according to claim 1, wherein the cosolvent in the step S1 is at least one of kerosene and lubricating oil.
3. The method for preparing a hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane according to claim 1, wherein the pore size of the hollow fiber microfiltration membrane of PTFE prepared in step S4 is 0.1-0.4 μm and the porosity is 40-50%.
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| CN202011360252.7A CN112619451B (en) | 2020-11-27 | 2020-11-27 | Preparation method of hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane |
| AU2021104813A AU2021104813A4 (en) | 2020-11-27 | 2021-08-02 | Method for preparing hydrophilic polytetrafluoroethylene hollow fiber microfiltration membrane |
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| CN114832637A (en) * | 2022-05-11 | 2022-08-02 | 沈阳工业大学 | In-situ synthesis method for regulating and controlling pores and properties of carbon membrane surface interface |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08283447A (en) * | 1995-04-14 | 1996-10-29 | Sumitomo Electric Ind Ltd | Porous membrane made of hydrophilic tetrafluoroethylene resin and its production |
| JPH1028852A (en) * | 1996-07-15 | 1998-02-03 | Mitsubishi Rayon Co Ltd | Method for making polyolefin porous hollow fiber membrane hydrophilic |
| CN102872732A (en) * | 2012-10-22 | 2013-01-16 | 浙江理工大学 | Hydrophilic modification method for polytetrafluoroethylene microporous material |
| CN102941025A (en) * | 2012-11-20 | 2013-02-27 | 浙江理工大学 | Preparation method of teflon hollow fiber membrane for membrane distillation |
| CN103127842A (en) * | 2013-02-07 | 2013-06-05 | 浙江格尔泰斯环保特材科技有限公司 | Manufacturing method of hydrophilic teflon microporous membrane |
| CN103191654A (en) * | 2013-04-27 | 2013-07-10 | 中材科技股份有限公司 | Lasting hydrophilic modification method of polytetrafluoroethylene microporous membrane |
| CN103481528A (en) * | 2013-09-04 | 2014-01-01 | 湖州森诺氟材料科技有限公司 | Biaxially-oriented porous expanded polytetrafluoroethylene expanded hollow tubular membrane and preparation method thereof |
| CN104353370A (en) * | 2014-11-07 | 2015-02-18 | 中材科技股份有限公司 | Preparation method of hydrophilic PTFE (polytetrafluoroethylene) composite microporous membrane |
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2020
- 2020-11-27 CN CN202011360252.7A patent/CN112619451B/en active Active
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- 2021-08-02 AU AU2021104813A patent/AU2021104813A4/en not_active Ceased
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08283447A (en) * | 1995-04-14 | 1996-10-29 | Sumitomo Electric Ind Ltd | Porous membrane made of hydrophilic tetrafluoroethylene resin and its production |
| JPH1028852A (en) * | 1996-07-15 | 1998-02-03 | Mitsubishi Rayon Co Ltd | Method for making polyolefin porous hollow fiber membrane hydrophilic |
| CN102872732A (en) * | 2012-10-22 | 2013-01-16 | 浙江理工大学 | Hydrophilic modification method for polytetrafluoroethylene microporous material |
| CN102941025A (en) * | 2012-11-20 | 2013-02-27 | 浙江理工大学 | Preparation method of teflon hollow fiber membrane for membrane distillation |
| CN103127842A (en) * | 2013-02-07 | 2013-06-05 | 浙江格尔泰斯环保特材科技有限公司 | Manufacturing method of hydrophilic teflon microporous membrane |
| CN103191654A (en) * | 2013-04-27 | 2013-07-10 | 中材科技股份有限公司 | Lasting hydrophilic modification method of polytetrafluoroethylene microporous membrane |
| CN103481528A (en) * | 2013-09-04 | 2014-01-01 | 湖州森诺氟材料科技有限公司 | Biaxially-oriented porous expanded polytetrafluoroethylene expanded hollow tubular membrane and preparation method thereof |
| CN104353370A (en) * | 2014-11-07 | 2015-02-18 | 中材科技股份有限公司 | Preparation method of hydrophilic PTFE (polytetrafluoroethylene) composite microporous membrane |
Non-Patent Citations (1)
| Title |
|---|
| PTFE中空纤维膜的亲水改性;郭晓蓓;余佳彬;黎鹏;费传军;范凌云;;现代塑料加工应用(03);全文 * |
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