CN113521880B - Photothermal regeneration mask core layer material and preparation method thereof - Google Patents
Photothermal regeneration mask core layer material and preparation method thereof Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/30—Antimicrobial, e.g. antibacterial
- A41D31/305—Antimicrobial, e.g. antibacterial using layered materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0036—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions by adsorption or absorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/10—Particle separators, e.g. dust precipitators, using filter plates, sheets or pads having plane surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/10—Particle separators, e.g. dust precipitators, using filter plates, sheets or pads having plane surfaces
- B01D46/12—Particle separators, e.g. dust precipitators, using filter plates, sheets or pads having plane surfaces in multiple arrangements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/261—Drying gases or vapours by adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/065—More than one layer present in the filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physical Education & Sports Medicine (AREA)
- Respiratory Apparatuses And Protective Means (AREA)
- Filtering Materials (AREA)
Abstract
The invention discloses a core layer material of a photo-thermal regeneration mask, which is a nano carbon/non-woven or woven cloth/porous material ternary composite material consisting of an inner skin-friendly layer, an intermediate core filter layer and an outer hydrophobic layer. The ternary composite structure material has extremely high stability, has the advantages of water resistance, ventilation, photo-thermal sterilization and the like, and can be widely applied to the rapid preparation of virus protection filter layer materials. The photo-thermal regeneration mask obtained by utilizing the composite material has the advantages of rapid temperature rise and sterilization under illumination, the bacterial filtration efficiency is over 99 percent, the particle filtration efficiency is over 96 percent, and the level of the mask exceeds that of a medical surgical mask; the preparation method is simple, is convenient to operate, does not need the procedures of high polymer adhesive, heating or pretreatment and the like, and is suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of protective articles, and particularly relates to a core layer material of a photo-thermal regeneration mask and a preparation method thereof.
Background
Most of the current medical mask core filter layers adopt non-woven fabrics prepared by taking polypropylene as a raw material, not only have basic functions such as hydrophobicity, but also have two very important functions, namely compactness for preventing virus diffusion and penetrability for allowing gas exchange. The virus filtering principle is physical adsorption and pore size isolation, and even if microporous carbon and other materials with high adsorption capacity are added, the filtration efficiency is reduced and the respiratory resistance is increased due to limited adsorption quantity. The expired water vapor is difficult to be rapidly discharged after long-time use. Therefore, the medical mask has the problems of disposability or short-term effect and the like.
The most effective protection technology at present is multilayer protection, but the long-term utilization of protection equipment is severely restricted by the problems of low connectivity of pore structure, low pore diameter and non-uniformity of key material microporous carbon in a core filter layer. In addition, the high polymer spinning fiber adopted by the framework material of the filter layer cannot be sterilized in a high-temperature, chemical or microwave mode and the like, so that the filter layer is difficult to recycle. In addition, in the traditional melt-blown non-woven fabric treatment process, surface impurities are usually required to be removed by pre-treating the non-woven fabric, and the surface-modified graphene is required to be subjected to functional treatment, and meanwhile, heating and long reaction time are also accompanied. More importantly, the melt-blown non-woven fabric serving as a mask filter layer is easy to damage the structure due to the erosion of the organic solvent, so that the filtering efficiency and the gas penetrability are affected.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a core layer material of a photo-thermal regeneration mask, which can realize the processing and preparation of the photo-thermal regeneration medical mask by preparing a nano carbon/non-woven or woven cloth/porous material ternary composite material and simply spraying without changing the existing medical mask process; the photo-thermal regeneration medical mask containing the graded ternary composite film has the characteristics of long-acting protection, recycling, and the like, has important economic and social benefits, and is suitable for popularization and application.
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
a preparation method of a core layer material of a photo-thermal regeneration mask comprises the following steps:
1) Preparing an organic alcohol aqueous solution I, adding a nano carbon material under the stirring condition, and performing ultrasonic dispersion to obtain nano carbon slurry;
2) Preparing an organic alcohol aqueous solution II, adding a porous material under the stirring condition, and performing ultrasonic dispersion to obtain a porous material slurry;
3) Uniformly coating the nano carbon slurry obtained in the step 1) on one surface of non-woven fabric or textile cloth, and drying;
4) Uniformly coating the porous material slurry obtained in the step 2) on the other side of the non-woven fabric or the textile fabric, and drying; and obtaining the core layer material of the photo-thermal regeneration mask.
In the above scheme, the nano carbon material includes, but is not limited to, one or more of graphene, carbon nanotubes, carbon fibers, graphite, carbon black, amorphous carbon, and the like.
In the above scheme, the organic alcohol in step 1) or 2) is one or more of ethanol, propanol, isopropanol, glycerol and other organic alcohols; the water is purified water, deionized water or distilled water, etc.
In the scheme, the volume ratio of the water to the organic alcohol in the step 1) is 5-15:1; the mass fraction of the nano carbon in the obtained nano carbon slurry is more than 0.5 wt%; preferably 0.5 to 4wt%.
In the above scheme, the porous material in step 2) is a porous water-absorbing material such as a molecular sieve, a metal organic framework or water-absorbing silica gel.
In the scheme, the volume ratio of the water to the organic alcohol in the step 2) is 5-15:1, and the mass fraction of the porous material in the obtained porous material slurry is more than 0.5 wt%; preferably 1 to 16wt%.
In the above scheme, the non-woven fabric or woven fabric is one or more of melt-blown non-woven fabric for mask, melt-blown non-woven fabric for air filtration, medical gauze, silk, nylon cloth, cotton cloth, oxford cloth, flannel and synthetic fiber cloth.
In the above scheme, the coating method of the steps 3 and 4) comprises, but is not limited to, a rolling method, a coating method, a spraying method and the like, wherein the thickness of a coating layer formed by coating the nano carbon slurry on the surface of the non-woven fabric or the textile fabric is 10-100 μm; the thickness of the coating layer formed by coating the porous material slurry on the other side of the non-woven fabric or the textile fabric is 10-100 mu m.
The core layer material of the photo-thermal regeneration mask prepared according to the scheme has a ternary composite structure of nano carbon/non-woven or woven cloth/porous material; the application and preparation of the photo-thermal regeneration mask are realized, the core filter layer is improved from the traditional melt-blown non-woven fabric to a three-layer structure of nano carbon (graphene, carbon nano tube and the like)/melt-blown non-woven fabric/porous material (porous MIL-160, water-absorbing silica gel and the like), so that the mask can be penetrated efficiently and has high filterability, and the sterilization and the cyclic regeneration of the core filter layer can be realized under the photo-thermal temperature condition, thereby being applicable to the fields of novel coronaviruses, other respiratory infectious disease protection and the like.
Compared with the prior art, the invention has the beneficial effects that:
1) According to the invention, the porous material and the nano carbon are used as functional materials, and the nano carbon slurry and the porous material slurry are prepared, so that the nano carbon/non-woven or woven cloth/porous material core filter layer material with a three-layer structure can be rapidly prepared by adopting a physical spraying or pressing method under the condition of not changing the existing mask preparation process; the prepared nano carbon slurry and porous material slurry (for regulating the organic alcohol ratio) only spread on the surface of the melt-blown non-woven fabric and cannot be immersed into the melt-blown non-woven fabric, and then the nano carbon (graphene, carbon nano tube and the like) and porous material (MIL-160, water-absorbing silica gel and the like) are formed into a film on the surface of the melt-blown non-woven fabric by physical pressurization at room temperature, so that the structural integrity of the nano carbon slurry and the porous material is ensured; the whole preparation process does not need working procedures such as high polymer adhesive, heating or pretreatment, and the like, does not depend on complex equipment, has obvious effect, and the preparation process is suitable for common household self-use and factory batch production and has good marketing property.
2) The invention provides a ternary structure design of nano carbon/non-woven or woven cloth/porous material for the first time, wherein the porous material layer is used as a strong water absorption material, so that the virus activity can be reduced by rapid water absorption, the non-woven or woven cloth (melt-blown layer and the like) is used for isolating viruses, and the nano carbon layer can be rapidly heated to more than 90 ℃ under illumination due to excellent photo-thermal property, and the viruses can be killed at high temperature and the evaporated and adsorbed water can be killed cooperatively by photo-thermal and photo-catalytic.
3) The nano carbon/non-woven or woven cloth/porous material ternary composite material core filter layer obtained by the invention has high stability, the bacterial filtration efficiency reaches more than 99%, and the particle filtration efficiency reaches more than 95%; has the characteristics of long-acting protection, recycling, and the like, and is suitable for popularization and application.
Drawings
FIG. 1 is a scanning electron microscope image of the KN95 melt blown nonwoven spray coated industrial graphene surface of example 1;
FIG. 2 is a scanning electron microscope image of the KN95 meltblown nonwoven spray MOF surface of example 1;
FIG. 3 is a graph showing the temperature of the photo-thermal regeneration mask and the commercial mask obtained in example 1 over time under light irradiation;
Fig. 4 is a water vapor adsorption and desorption experiment of MIL-160 layer in the photo-thermal regeneration mask obtained in example 1;
FIG. 5 shows the results of measuring the bacterial filtration efficiency and the particle filtration efficiency of the photo-thermal regeneration mask obtained in example 1;
Fig. 6 is a scanning electron microscope image of the graphene nanoplatelet-meltblown surface of example 2.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the invention further, but are not to be construed as limiting the invention.
Example 1
A preparation method of a photothermal regeneration mask core layer material and a mask comprises the following steps:
1) 2 parts of mixed solution containing 10ml of ethanol and 90ml of water is prepared, 1g of industrial grade graphene powder and 1g of metal organic framework material MIL-160 are respectively added, and the graphene slurry and MIL-160 slurry are respectively prepared by ultrasonic dispersion;
2) Uniformly coating the graphene slurry on the surface of a KN95 melt-blown non-woven fabric, and drying; coating MIL-160 slurry on the other side of the KN95 melt-blown non-woven fabric, and drying; the thickness of the coating is controlled to be about 10 mu m;
3) And packaging the prepared graphene/KN 95 melt-blown non-woven fabric/MIL-160 ternary composite material core filter layer on a mask machine to form the photothermal regeneration mask.
The photo-thermal regeneration mask obtained in the embodiment is composed of two layers of non-woven fabrics and a graded ternary composite film core filter layer, as can be seen from fig. 1, graphene slurry is rolled onto the surface of melt-blown cloth, and multiple layers of graphene sheets are stacked on the melt-blown cloth fiber to form a layer of large-area compact graphene film, and the graphene film has the characteristics of ventilation and water resistance due to the porous characteristic of the nano material. As can be seen from the high-power SEM of the embedded graph in fig. 1, the graphene does not show a stacked state in a sheet form, but is self-assembled to form a three-dimensional porous structure similar to a flower shape, and the three-dimensional porous structure is only adsorbed on the polymer fiber, so that the graphene film is compact, firm and not easy to fall off.
As can be seen from fig. 2, the other surface of the KN95 melt-blown nonwoven fabric is covered with a film made of MILs-160 porous material, so as to form a graphene/KN 95 melt-blown nonwoven fabric/MILs-160 ternary composite material core filter layer. As can be seen from the high-power SEM of the inset in FIG. 2, MIL-160 nanoparticles are between a few hundred nanometers and 2 microns in size, with the particles aggregating around the meltblown fibers, with good water absorption properties.
FIG. 3 shows that the core filter layer material obtained in this example can be heated from room temperature to over 80 ℃ up to 93 ℃ within 10 seconds under ultraviolet and visible light; after the light is shielded, the surface temperature of the material is quickly restored to room temperature within 16 seconds, which proves that the material has excellent light-heat conversion performance and can quickly kill viruses under the light. The excellent photo-thermal conversion performance is mainly beneficial to the fact that the graphene slurry does not contain a high polymer adhesive, and the intrinsic physical properties of the carbon material can be maintained.
Further, the water absorption and dehydration performance of the MIL-160 layer in the photo-thermal regeneration mask obtained in the embodiment simulates the daily use condition, and the adopted test conditions are as follows: adsorbing water at room temperature with 90% humidity; water was desorbed at 90 ℃ with 0% humidity. As shown in the results of FIG. 4, the MIL-160 layer has good water absorption performance under the condition of high humidity at room temperature, the absolute value of water absorption amount is 9 mg, and the relative value is 0.5g water/gMIL-160, which shows that the water absorption layer has good water absorption characteristics. At a high temperature of 90 ℃, the MIL-160 layer can rapidly and completely desorb water, so that the mask can absorb water vapor to keep the filter layer dry in use and can desorb water at a high temperature to realize recycling.
Fig. 5 shows the test results of the medical surgical mask obtained in this example, and it can be seen from the graph that the bacterial filtration efficiency of the photo-thermal regeneration mask obtained in this example is more than 99%, the particle filtration efficiency is more than 96%, and the performance is better than that of the N95 mask. While the bacterial filtration efficiency and the particle filtration efficiency of commercial masks are only less than 94% and 79%, respectively.
Example 2
This example is substantially the same as example 1, except that the graphene is a graphene nanoplatelet and the coating thickness is 10 μm. As seen from fig. 6, a very good graphene film can be formed on KN95 melt-blown nonwoven fabric, regardless of whether it is industrial grade graphene powder or graphene nanoplatelets.
The obtained photo-thermal regeneration mask has good photo-thermal conversion performance and bacterial and particle filtering performance.
Example 3
This example is similar to example 1, except that the ethanol is replaced with ethylene glycol, and the ratio is unchanged.
The obtained photo-thermal regeneration mask has good photo-thermal conversion performance and bacterial and particle filtration efficiency.
Example 4
This example is substantially the same as example 1, except that the amount of hydrated ethanol used in step 1) is: 90mL of water and 12mL of ethanol.
Through detection, the photo-thermal regeneration mask obtained by the implementation has good photo-thermal conversion performance and bacteria and particle filtration efficiency.
Example 5
This example is substantially the same as example 1, except that the porous material is a commercial water absorbing silica gel.
Through detection, the photo-thermal regeneration mask obtained by the implementation has good photo-thermal conversion performance and bacteria and particle filtration efficiency.
Example 6
This example is substantially the same as example 1, except that the industrial graphene is used in an amount of 4g.
Through detection, the photo-thermal regeneration mask obtained by the implementation has good photo-thermal conversion performance and bacteria and particle filtration efficiency.
Example 7
This example is substantially the same as example 1 except that the KN95 meltblown nonwoven fabric is replaced with medical gauze.
Through detection, graphene and MIL-160 can still well form a compact porous film on the surface of the KN95 melt-blown non-woven fabric, the photo-thermal conversion performance is similar to that of example 1, and the bacterial and particle filtration efficiency is more than 95%.
Example 8
This example is substantially the same as example 1 except that the KN95 melt blown nonwoven fabric is replaced with nylon cloth, which is repeatedly folded into 3 layers and sewn with needle and thread.
Through detection, graphene and MIL-160 can still well form a compact porous membrane on the surface of nylon cloth, the photo-thermal conversion performance is similar to that of example 1, and the bacterial and particle filtration efficiency is over 95%.
Example 9
This example is substantially the same as example 1 except that the KN95 meltblown nonwoven fabric is replaced with cotton cloth, which is repeatedly folded into 3 layers and sewn with stitches.
Through detection, graphene and MIL-160 can still well form a compact porous membrane on the surface of cotton cloth, the photo-thermal conversion performance is similar to that of example 1, and the bacterial and particle filtration efficiency is more than 95%.
Example 10
This embodiment is substantially the same as embodiment 1 except that graphene is replaced with carbon nanotubes.
Through detection, the photo-thermal regeneration mask obtained by the implementation has good photo-thermal conversion performance and bacteria and particle filtration efficiency.
Comparative example 1
This comparative example is substantially the same as example 1, except that the water in step 2) is 100ml and the organic alcohol is 0ml. Through detection, the graphene and MIL-160 cannot be coated on the surface of the KN95 melt-blown non-woven fabric, and the graphene and MIL-160 are agglomerated and fall off after being dried. Furthermore, we tried other nanocarbon materials and porous materials, which failed to form dense porous films on melt blown nonwoven fabrics. .
Comparative example 2
This comparative example is substantially the same as example 1, except that water is 90mL and ethanol is 5mL. Through detection, the nano carbon and the porous material can not be coated on the surface of the KN95 melt-blown non-woven fabric, and the nano carbon and the porous material are agglomerated and fall off after being dried. Furthermore, we tried other nanocarbon materials and porous materials, which failed to form dense porous films on melt blown nonwoven fabrics.
Comparative example 3
This comparative example is substantially the same as example 1, except that water is 80mL and ethanol is 20mL. Through detection, after the nano carbon and the porous material are coated on the surface of the KN95 melt-blown non-woven fabric, the solvent permeates into the interior of the melt-blown non-woven fabric, so that the microstructure of the melt-blown fibers in the interior is damaged, and the bacterial and particle filtration efficiency is lower than 70%.
It is apparent that the above examples are only examples given for clarity of illustration and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And thus obvious variations or modifications to the disclosure are within the scope of the invention.
Claims (7)
1. The preparation method of the photothermal regeneration mask core layer material is characterized by comprising the following steps of:
1) Preparing an organic alcohol aqueous solution I, wherein the volume ratio of water to organic alcohol is 5-15:1; adding a nano carbon material under the stirring condition, and performing ultrasonic dispersion to obtain nano carbon slurry, wherein the mass fraction of nano carbon in the nano carbon slurry is more than 0.5 wt%;
2) Preparing an organic alcohol aqueous solution II, wherein the volume ratio of water to organic alcohol is 5-15:1; adding a porous material under stirring, and performing ultrasonic dispersion to obtain porous material slurry, wherein the mass fraction of the porous material in the porous material slurry is more than 0.5 wt%;
3) Uniformly coating the nano carbon slurry obtained in the step 1) on one surface of non-woven fabric or textile cloth, and drying;
4) Uniformly coating the porous material slurry obtained in the step 2) on the other side of the non-woven fabric or the textile fabric, and drying; and obtaining the core layer material of the photo-thermal regeneration mask.
2. The method according to claim 1, wherein the nanocarbon material comprises one or more of graphene, carbon nanotubes, carbon fibers, graphite, carbon black, and amorphous carbon.
3. The preparation method according to claim 1, wherein the organic alcohol in step 1) or 2) is one or more of ethanol, propanol, isopropanol and glycerol.
4. The method of claim 1, wherein the porous material in step 2) is a molecular sieve, a metal organic framework, or a porous water absorbing material.
5. The method according to claim 1, wherein the nonwoven fabric or woven fabric is one or more of a meltblown nonwoven fabric for mask, a meltblown nonwoven fabric for air filtration, medical gauze, silk, nylon cloth, cotton cloth, oxford cloth, flannel, and synthetic fiber cloth.
6. The method according to claim 1, wherein the coating method of steps 3) and 4) comprises a roll press method, a coating method or a spray method, and the nano carbon slurry is coated on the surface of the non-woven fabric or the textile fabric to form a coating layer with a thickness of 10-100 μm; the thickness of the coating layer formed by coating the porous material slurry on the other side of the non-woven fabric or the textile fabric is 10-100 mu m.
7. The core layer material of the photo-thermal regeneration mask prepared by the preparation method of any one of claims 1-6.
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CN101286564A (en) * | 2008-05-28 | 2008-10-15 | 中国科学院上海微系统与信息技术研究所 | Composite anode for direct methanol fuel cell and method for making the same |
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