CN113413775A - Preparation method of polytetrafluoroethylene nano microporous membrane - Google Patents
Preparation method of polytetrafluoroethylene nano microporous membrane Download PDFInfo
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- CN113413775A CN113413775A CN202110774421.XA CN202110774421A CN113413775A CN 113413775 A CN113413775 A CN 113413775A CN 202110774421 A CN202110774421 A CN 202110774421A CN 113413775 A CN113413775 A CN 113413775A
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- polytetrafluoroethylene
- base band
- oil
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- microporous membrane
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- 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
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
-
- 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
Abstract
The invention discloses a preparation method of a polytetrafluoroethylene nanometer microporous membrane, and relates to the technical field of membrane preparation. The metal oxide is added into the extrusion assistant and then added into the polytetrafluoroethylene dispersion resin to obtain a mixed solution, and the materials are mixed more uniformly by using the cosolvent. And pressing the mixed materials into a blank by a blank making machine, extruding the blank into a paste by an extruder, calendering the paste on a calender to form an oil-containing base band, removing an extrusion aid in the oil-containing base band, transversely stretching and longitudinally stretching the deoiled base band, sintering and solidifying the transversely stretched base band, and naturally cooling the longitudinally stretched base band to obtain the polytetrafluoroethylene microporous nano-membrane. The polytetrafluoroethylene nanometer microporous membrane prepared by the method has better mechanical strength, waterproof moisture permeability, more uniform pore size distribution and improved thermal stability.
Description
Technical Field
The invention relates to the technical field of membrane preparation, in particular to a preparation method of a polytetrafluoroethylene nanometer microporous membrane.
Background
Polytetrafluoroethylene is a thermoplastic, known as "plastomer". The polytetrafluoroethylene has the excellent characteristics of stable chemical property, good sealing performance, corrosion resistance and the like, and is widely applied to the fields of clothes, medicine, pipelines, containers and the like, and the nano microporous membrane is one of the application fields of the polytetrafluoroethylene. The polytetrafluoroethylene nanometer microporous membrane is mutually connected with micropores through the microfine fibers, so that the polytetrafluoroethylene not only has the original excellent performance, but also has the advantages of high water permeability, high light transmittance, ventilation, wind resistance and the like.
In recent years, the development of the polytetrafluoroethylene microporous membrane is rapid, and various modes such as hydrophilic modification, filling modification and the like are developed, so that the research progress of the polytetrafluoroethylene microporous membrane is promoted, and the polytetrafluoroethylene microporous membrane can better meet the increasing demands of people. However, the existing process for producing the polytetrafluoroethylene microporous membrane is complex, the prepared polytetrafluoroethylene microporous membrane has poor waterproof and moisture permeability, uneven pore size distribution and needs to be improved in mechanical property and thermal stability.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a polytetrafluoroethylene nanometer microporous membrane, and the prepared polytetrafluoroethylene nanometer microporous membrane has better mechanical strength, waterproof moisture permeability, more uniform pore size distribution and improved thermal stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a polytetrafluoroethylene nanometer microporous membrane comprises the following steps:
(1) adding metal oxide into extrusion aid, then adding into polytetrafluoroethylene dispersion resin to obtain mixed solution, atomizing cosolvent, dispersing into the mixed solution, and fully stirring to uniformly mix materials;
(2) pressing the mixed materials into a blank by a blank making machine at the temperature of 50-80 ℃, then placing the blank on an extruder at the temperature of 50-100 ℃ to extrude the blank into paste, and placing the paste on a calender to form an oil-containing base band;
(3) removing the extrusion aid in the oil-containing base band, processing the oil-containing base band into a deoiled base band, transversely stretching the deoiled base band at the temperature of 220-320 ℃, and then longitudinally stretching the deoiled base band at the temperature of 250-320 ℃;
(4) sintering and curing the treated deoiled base band at the temperature of 330 ℃ and 380 ℃ for 2-4h, and naturally cooling to room temperature to prepare the polytetrafluoroethylene nano microporous membrane.
Preferably, the mass ratio of the polytetrafluoroethylene dispersion resin, the extrusion aid, the metal oxide and the cosolvent is 1 (0.2-0.5) to (0.01-0.05): (0.1-0.3).
Preferably, the particle size of the polytetrafluoroethylene dispersion resin is 10 to 40 μm, and the particle size of the metal oxide is less than 75 μm.
Preferably, the metal oxide is one or more of alumina, titania, silica, zinc oxide, and copper oxide.
Preferably, the polytetrafluoroethylene dispersion resin has a crystallinity of greater than 98% and a molecular weight of 200 to 1200 ten thousand.
Preferably, in the step (1), the extrusion aid is one of lubricating oil, solvent oil and paraffin oil.
Preferably, in step (1), the cosolvent is tween 80.
Preferably, in the step (3), the method for removing the extrusion aid in the oil-containing base belt comprises the following steps: and (3) putting the oil-containing base band into an oven to be dried for 10-15 h.
Preferably, in step (3), the stretching rate of the transverse stretching and the longitudinal stretching is 0.03 to 0.33/min.
Compared with the prior art, the metal oxide is added into the polytetrafluoroethylene dispersion resin, and the metal elements in the metal oxide can destroy C-F bonds in the polytetrafluoroethylene dispersion resin, so that polar groups such as carbon-carbon double bonds, carbonyl groups, carboxyl groups and the like exist in the polytetrafluoroethylene dispersion resin, the surface energy of the polytetrafluoroethylene dispersion resin is greatly enhanced, and the wettability of the polytetrafluoroethylene dispersion resin is improved. In addition, the metal element in the metal oxide and the C element in the polytetrafluoroethylene dispersion resin can form a chemical bond, so that the mechanical strength and the stability of the material are enhanced.
The particle size of the polytetrafluoroethylene dispersion resin is 10-40 mu m, the particle size of the metal oxide is less than 75 mu m, and the polytetrafluoroethylene dispersion resin and the metal oxide under the particle size can better play a synergistic effect mutually, so that the finally prepared microporous membrane has more excellent performance.
According to the invention, the deoiling base belt is transversely stretched at the temperature of 220-320 ℃, and then longitudinally stretched at the temperature of 250-320 ℃, so that the defects of thick middle part and thin two sides of the prepared polytetrafluoroethylene nanometer microporous membrane are avoided, and the pore size distribution of the nanometer microporous membrane is more uniform. In the stretching process, the stretching speed can influence the aperture of the finally prepared polytetrafluoroethylene nanometer microporous membrane, and the applicant finds that when the stretching speed is 0.03-0.33/min, the aperture distribution of the polytetrafluoroethylene nanometer microporous membrane is more uniform, and the waterproof and moisture permeable effects are better.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
All the starting materials in the present invention, the sources of which are not particularly limited, may be either commercially available or prepared according to conventional methods well known to those skilled in the art.
All the raw materials used in the present invention are not particularly limited in purity, and the present invention preferably employs a purity which is conventional in the field of analytical purification or composite materials.
Example 1
1 part of titanium dioxide was added to 20 parts of solvent oil, followed by addition to 100 parts of polytetrafluoroethylene dispersion resin to obtain a mixed solution. Wherein the polytetrafluoroethylene dispersion resin has a crystallinity of 99.8% and a molecular weight of 1000 ten thousand. Atomizing 10 parts of tween 80, dispersing the tween 80 into the mixed solution, and fully stirring to uniformly mix the materials. Pressing the mixed materials into a blank by a blank making machine at 50 ℃, then placing the blank on an extruder at 80 ℃ to extrude the blank into a paste, and placing the paste on a calender to calender the paste to form an oil-containing base band; putting the oil-containing base band into an oven to be dried for 10h, removing solvent oil in the oil-containing base band, processing the oil-containing base band into a deoiled base band, transversely stretching the deoiled base band at 220 ℃, and then longitudinally stretching the deoiled base band at 250 ℃; sintering and curing the treated deoiled base band at 330 ℃ for 3h, and naturally cooling to room temperature to prepare the polytetrafluoroethylene nano microporous membrane.
Example 2
3 parts of titanium dioxide was added to 60 parts of solvent oil, followed by addition to 300 parts of polytetrafluoroethylene dispersion resin to obtain a mixed solution. Wherein the polytetrafluoroethylene dispersion resin has a crystallinity of 99.8% and a molecular weight of 1000 ten thousand. And (3) atomizing 30 parts of tween 80, dispersing the tween 80 into the mixed solution, and fully stirring to uniformly mix the materials. Pressing the mixed materials into a blank by a blank making machine at 50 ℃, then placing the blank on an extruder at 80 ℃ to extrude the blank into a paste, and placing the paste on a calender to calender the paste to form an oil-containing base band; putting the oil-containing base band into an oven to be dried for 10h, removing solvent oil in the oil-containing base band, processing the oil-containing base band into a deoiled base band, transversely stretching the deoiled base band at 220 ℃, and then longitudinally stretching the deoiled base band at 250 ℃; sintering and curing the treated deoiled base band at 330 ℃ for 3h, and naturally cooling to room temperature to prepare the polytetrafluoroethylene nano microporous membrane.
Example 3
5 parts of titanium dioxide was added to 100 parts of solvent oil, followed by addition to 500 parts of polytetrafluoroethylene dispersion resin to obtain a mixed solution. Wherein the polytetrafluoroethylene dispersion resin has a crystallinity of 99.8% and a molecular weight of 1000 ten thousand. 50 parts of Tween 80 is atomized, dispersed into the mixed solution and fully stirred to uniformly mix the materials. Pressing the mixed materials into a blank by a blank making machine at 50 ℃, then placing the blank on an extruder at 80 ℃ to extrude the blank into a paste, and placing the paste on a calender to calender the paste to form an oil-containing base band; putting the oil-containing base band into an oven to be dried for 10h, removing solvent oil in the oil-containing base band, processing the oil-containing base band into a deoiled base band, transversely stretching the deoiled base band at 220 ℃, and then longitudinally stretching the deoiled base band at 250 ℃; sintering and curing the treated deoiled base band at 330 ℃ for 3h, and naturally cooling to room temperature to prepare the polytetrafluoroethylene nano microporous membrane.
Comparative example 1
50 parts of solvent oil was added to 100 parts of polytetrafluoroethylene dispersion resin to obtain a mixed solution. Wherein the polytetrafluoroethylene dispersion resin has a crystallinity of 99.8% and a molecular weight of 1000 ten thousand. 50 parts of Tween 80 is atomized, dispersed into the mixed solution and fully stirred to uniformly mix the materials. Pressing the mixed materials into a blank by a blank making machine at 50 ℃, then placing the blank on an extruder at 80 ℃ to extrude the blank into a paste, and placing the paste on a calender to calender the paste to form an oil-containing base band; putting the oil-containing base band into an oven to be dried for 10h, removing solvent oil in the oil-containing base band, processing the oil-containing base band into a deoiled base band, transversely stretching the deoiled base band at 220 ℃, and then longitudinally stretching the deoiled base band at 250 ℃; sintering and curing the treated deoiled base band at 330 ℃ for 3h, and naturally cooling to room temperature to prepare the polytetrafluoroethylene nano microporous membrane.
Comparative example 2
To 80 parts of solvent oil was then added 300 parts of polytetrafluoroethylene dispersion resin to obtain a mixed solution. Wherein the polytetrafluoroethylene dispersion resin has a crystallinity of 99.8% and a molecular weight of 1000 ten thousand. 50 parts of Tween 80 is atomized, dispersed into the mixed solution and fully stirred to uniformly mix the materials. Pressing the mixed materials into a blank by a blank making machine at 50 ℃, then placing the blank on an extruder at 80 ℃ to extrude the blank into a paste, and placing the paste on a calender to calender the paste to form an oil-containing base band; putting the oil-containing base band into an oven to be dried for 10h, removing solvent oil in the oil-containing base band, processing the oil-containing base band into a deoiled base band, transversely stretching the deoiled base band at 220 ℃, and then longitudinally stretching the deoiled base band at 250 ℃; sintering and curing the treated deoiled base band at 330 ℃ for 3h, and naturally cooling to room temperature to prepare the polytetrafluoroethylene nano microporous membrane.
The polytetrafluoroethylene nanoporous films prepared in the above examples 1-3 and comparative examples 1-2 were tested to measure the properties of the materials.
The pore size of the microporous membrane is measured by using an AutoPore V mercury intrusion instrument, and the strength of the microporous membrane is measured by using an INSTRON electronic brute force instrument.
The performance test results are shown in table 1:
TABLE 1 Performance of the nanoporous membranes prepared in examples 1-3 and comparative examples 1-2
As can be seen from the data in Table 1, compared with the PTFE microporous nano-film prepared in the comparative examples 1-2, the PTFE microporous nano-film prepared in the examples 1-3 of the present invention has the advantages of uniform pore size distribution, better waterproof and moisture permeable effects, higher tensile strength, and better mechanical properties.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A preparation method of a polytetrafluoroethylene nanometer microporous membrane is characterized by comprising the following steps:
(1) adding metal oxide into extrusion aid, then adding into polytetrafluoroethylene dispersion resin to obtain mixed solution, atomizing cosolvent, dispersing into the mixed solution, and fully stirring to uniformly mix materials;
(2) pressing the mixed materials into a blank by a blank making machine at the temperature of 50-80 ℃, then placing the blank on an extruder at the temperature of 50-100 ℃ to extrude the blank into paste, and placing the paste on a calender to form an oil-containing base band;
(3) removing the extrusion aid in the oil-containing base band, processing the oil-containing base band into a deoiled base band, transversely stretching the deoiled base band at the temperature of 220-320 ℃, and then longitudinally stretching the deoiled base band at the temperature of 250-320 ℃;
(4) sintering and curing the treated deoiled base band at the temperature of 330 ℃ and 380 ℃ for 2-4h, and naturally cooling to room temperature to prepare the polytetrafluoroethylene nano microporous membrane.
2. The method for preparing the polytetrafluoroethylene microporous nano-membrane according to claim 1, wherein the mass ratio of the polytetrafluoroethylene dispersion resin, the extrusion aid, the metal oxide and the cosolvent is 1 (0.2-0.5) to (0.01-0.05): (0.1-0.3).
3. The method of preparing a polytetrafluoroethylene microporous membrane according to claim 1, wherein the particle size of the polytetrafluoroethylene dispersion resin is 10 to 40 μm, and the particle size of the metal oxide is less than 75 μm.
4. The method of claim 1, wherein the metal oxide is one or more of alumina, titania, silica, zinc oxide, and copper oxide.
5. The method of claim 1, wherein the polytetrafluoroethylene-dispersed resin has a crystallinity of greater than 98% and a molecular weight of 200 to 1200 ten thousand.
6. The method for preparing a polytetrafluoroethylene microporous membrane according to claim 1, wherein in step (1), the extrusion aid is one of lubricating oil, solvent oil and paraffin oil.
7. The method for preparing a polytetrafluoroethylene nanopore membrane according to claim 1, wherein in step (1), the cosolvent is tween 80.
8. The method for preparing a polytetrafluoroethylene microporous nano-membrane according to claim 1, wherein the method for removing the extrusion aid in the oil-containing base tape in step (3) comprises the following steps: and (3) putting the oil-containing base band into an oven to be dried for 10-15 h.
9. The method of preparing a polytetrafluoroethylene microporous membrane according to claim 1, wherein the stretching rate of the transverse stretching and the longitudinal stretching in step (3) is 0.03 to 0.33/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114130223A (en) * | 2021-10-19 | 2022-03-04 | 安徽元琛环保科技股份有限公司 | Preparation method of PTFE (polytetrafluoroethylene) membrane with high filtering efficiency |
| CN114179467A (en) * | 2021-11-03 | 2022-03-15 | 浙江汇文新材料科技有限公司 | Production process of nano down jacket fabric |
| CN114247300A (en) * | 2021-12-28 | 2022-03-29 | 湖北聚孚膜科技有限公司 | Anti-pollution PTFE hollow fiber microfiltration membrane and preparation method thereof |
| CN116395920A (en) * | 2023-06-09 | 2023-07-07 | 成都硕特科技股份有限公司 | Oil removal device and oil removal method for coal chemical wastewater |
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| CN114130223A (en) * | 2021-10-19 | 2022-03-04 | 安徽元琛环保科技股份有限公司 | Preparation method of PTFE (polytetrafluoroethylene) membrane with high filtering efficiency |
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| CN114179467A (en) * | 2021-11-03 | 2022-03-15 | 浙江汇文新材料科技有限公司 | Production process of nano down jacket fabric |
| CN114247300A (en) * | 2021-12-28 | 2022-03-29 | 湖北聚孚膜科技有限公司 | Anti-pollution PTFE hollow fiber microfiltration membrane and preparation method thereof |
| CN116395920A (en) * | 2023-06-09 | 2023-07-07 | 成都硕特科技股份有限公司 | Oil removal device and oil removal method for coal chemical wastewater |
| CN116395920B (en) * | 2023-06-09 | 2023-09-05 | 成都硕特科技股份有限公司 | Oil removal device and oil removal method for coal chemical wastewater |
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