CN113521880A - 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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- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
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- 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
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D39/14—Other self-supporting filtering material ; Other filtering material
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- 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
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- 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
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- 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
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- 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
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- 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
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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
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- B01D2239/065—More than one layer present in the filtering material
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- General Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Physical Education & Sports Medicine (AREA)
- Filtering Materials (AREA)
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Abstract
The invention discloses a photothermal regeneration mask core layer material, which is a nano carbon/non-woven or woven cloth/porous material ternary composite material consisting of an inner skin-friendly layer, a middle core filtering layer and an outer hydrophobic layer. The ternary composite structure material has extremely high stability, has the advantages of water resistance, air permeability, photo-thermal sterilization and the like, and can be widely applied to the rapid preparation of virus protection filter layer materials. The photothermal regeneration mask obtained by utilizing the composite material has the advantages of rapid temperature rise and virus killing by illumination, the bacterial filtration efficiency exceeds 99 percent, the particle filtration efficiency exceeds 96 percent, and the level of the medical surgical mask is exceeded; the preparation method is simple, convenient to operate, free of high-molecular adhesive, heating or pretreatment and other processes, and 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 photothermal regeneration mask and a preparation method thereof.
Background
Most of the core filter layers of the existing medical masks are made of non-woven fabrics made of polypropylene, and the core filter layers not only need to have basic functions such as hydrophobic property and the like, but also need to 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 aperture isolation, and even if high-adsorption-capacity materials such as microporous carbon are added, the filtration efficiency is reduced and the respiratory resistance is increased due to limited adsorption capacity. When the mask is used for a long time, the exhaled water vapor is difficult to be rapidly removed. Therefore, the medical mask has the problems of one-time use or short-term use and the like, and the problems of mask shortage and long-time face infection when the mask is worn in the peak period of epidemic outbreak are caused.
The most effective protection technology at present is multilayer protection, but the long-term utilization of the protection equipment is severely restricted by the problems of low connectivity of the pore structure of the key material microporous carbon in the core filter layer, uneven pore diameter and the like. In addition, the high molecular spinning fiber adopted by the framework material of the filter layer can not be sterilized by high temperature, chemistry or microwave and the like, so that the recycling of the filter layer is difficult to realize. In addition, the traditional melt-blown non-woven fabric treatment process usually needs to pretreat the non-woven fabric to remove surface impurities, and the surface modified graphene needs to be functionalized, and meanwhile, the heating and the long reaction time are also accompanied. More importantly, the melt-blown non-woven fabric used as the mask filter layer is easy to cause structural damage due to the erosion of organic solvents, thereby influencing the filtering efficiency and the gas permeability.
Disclosure of Invention
The invention mainly aims to provide a core layer material of a photothermal regeneration mask aiming at the defects in the prior art, and the processing and preparation of the photothermal regeneration medical mask can be realized by preparing a nano carbon/non-woven or woven cloth/porous material ternary composite material and simply spraying the nano carbon/non-woven or woven cloth/porous material ternary composite material without changing the prior medical mask process; the photothermal regeneration medical mask containing the graded ternary composite film has the characteristics of long-acting protection, cyclic regeneration and utilization and the like, has important economic and social benefits, and is suitable for popularization and application.
In order to achieve the purpose, the invention adopts the main technical scheme that:
a preparation method of a photothermal regeneration mask core layer material 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 porous material slurry;
3) uniformly coating the nano-carbon slurry obtained in the step 1) on one surface of non-woven fabric or woven fabric, 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 woven fabric, and drying; and obtaining the photothermal regeneration mask core layer material.
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 scheme, the organic alcohol in the 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 4 wt%.
In the scheme, the porous material in the 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 16 wt%.
In the scheme, the non-woven fabric or the textile fabric is one or more of melt-blown non-woven fabric for a mask, melt-blown non-woven fabric for air filtration, medical gauze, silk, nylon fabric, cotton fabric, oxford fabric, flannel and synthetic fiber fabric.
In the above scheme, the coating method in steps 3 and 4) includes, but is not limited to, a rolling method, a coating method, a spraying method, etc., and the thickness of the coating formed by coating the nanocarbon slurry on the surface of the non-woven fabric or the woven fabric is 10-100 μm; the thickness of the coating formed by coating the porous material slurry on the other side of the non-woven fabric or the woven fabric is 10-100 mu m.
The photothermal regeneration mask core layer material prepared according to the scheme has a ternary composite structure of nano carbon/non-woven or woven cloth/porous material; the core filter layer of the photothermal regeneration mask is improved from the traditional melt-blown non-woven fabric into 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 high-efficiency through and high filtering performance of the mask can be realized, the disinfection and the cyclic regeneration utilization of the core filter layer can be realized under the mild conditions of photothermal, and the photothermal regeneration mask is suitable for the fields of novel coronavirus and 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 (regulating and controlling the organic alcohol ratio) can only spread on the surface of the melt-blown non-woven fabric and can not be immersed into the melt-blown non-woven fabric, and then the nano carbon (graphene, carbon nano tubes and the like) and the porous material (MIL-160, water-absorbing silica gel and the like) are formed into a film on the surface of the melt-blown fabric by physical pressurization at room temperature, so that the structural integrity of the nano carbon slurry and the porous material slurry is ensured; the whole preparation process does not need the working procedures of high molecular adhesive, heating or pretreatment and the like, does not depend on complex equipment, has obvious effect, is suitable for common household use and factory batch production, and has good market popularization.
2) The invention firstly proposes to adopt a ternary structure design of nano carbon/non-woven or woven cloth/porous material, a porous material layer is used as a strong water-absorbing material, the nano carbon/non-woven or woven cloth/porous material can absorb water rapidly to reduce virus activity, the non-woven or woven cloth (a melt-blown layer and the like) is used for isolating viruses, and a nano carbon layer can be heated to above 90 ℃ rapidly under the illumination due to the excellent photo-thermal property, kills the viruses and evaporates the absorbed water at high temperature, thereby realizing the photo-thermal and photo-catalytic synergistic virus killing.
3) The core filter layer of the ternary composite material of the nano carbon/non-woven or woven cloth/porous material has high stability, the bacterial filtering efficiency reaches more than 99 percent, and the particle filtering efficiency reaches more than 95 percent; has the characteristics of long-acting protection, cyclic recycling and the like, and is suitable for popularization and application.
Drawings
FIG. 1 is a scanning electron microscope image of the surface of industrial graphene sprayed with KN95 melt-blown nonwoven fabric in example 1;
FIG. 2 is a scanning electron microscope image of the MOF surface sprayed with KN95 meltblown nonwoven fabric of example 1;
FIG. 3 is a graph of temperature versus time for the photothermal regeneration mask and commercial mask of example 1 under light;
FIG. 4 is a water vapor adsorption/desorption experiment of the MIL-160 layer of the photothermal regeneration mask obtained in example 1;
FIG. 5 shows the results of the measurement of the bacterial filtering efficiency and the particle filtering efficiency of the mask for photo-thermal regeneration obtained in example 1;
fig. 6 is a scanning electron microscope image of the graphene nanoplatelet-meltblown surface of example 2.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.
Example 1
A preparation method of a core layer material of a photothermal regeneration mask and a mask comprises the following steps:
1) preparing 2 parts of mixed solution containing 10ml of ethanol and 90ml of water, respectively adding 1g of industrial-grade graphene powder and 1g of metal organic framework material MIL-160, and respectively preparing graphene slurry and MIL-160 slurry by ultrasonic dispersion;
2) uniformly coating the obtained graphene slurry on the surface of KN95 melt-blown non-woven fabric, and drying; coating the MIL-160 slurry on the other side of the KN95 melt-blown non-woven fabric, and drying; controlling the thickness of the coating 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 photothermal regeneration mask obtained in this embodiment is composed of two layers of non-woven fabrics and a core filter layer of a hierarchical ternary composite membrane, as can be seen from fig. 1, a graphene slurry is rolled to the surface of a melt-blown fabric, multiple graphene sheets are stacked on fibers of the melt-blown fabric to form a large-area compact graphene membrane, and due to the porous characteristic of a nano material, the graphene membrane has the characteristics of ventilation and water resistance. As can be seen from the high-power SEM of the inset in fig. 1, graphene does not assume a sheet-like stacked state, but self-assembles to form a flower-like three-dimensional porous structure, and is only adsorbed on the polymer fiber, so that the graphene film is not only dense, but also firm and not easy to fall off.
As can be seen from fig. 2, the other surface of the KN95 meltblown nonwoven fabric is covered with a film made of MIL-160 porous material, so that a graphene/KN 95 meltblown nonwoven fabric/MIL-160 ternary composite core filter layer is formed. As can be seen from the high-power SEM of the inset in fig. 2, MIL-160 nanoparticles are between several hundred nanometers and 2 microns in size, and the particles are aggregated 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 ℃ within 10s, and can reach 93 ℃ at most under the irradiation of ultraviolet and visible light; after the light is shielded, the surface temperature of the material is quickly recovered to the room temperature within 16s, which shows that the material has excellent photo-thermal conversion performance and can quickly kill viruses under the light. The excellent photo-thermal conversion performance is mainly benefited by the fact that no high-molecular binder exists in the graphene slurry, and the intrinsic physical performance of the carbon material can be maintained.
Further, for the water absorption and dehydration performance of the MIL-160 layer in the photothermal regeneration mask obtained in this example, we simulated the daily use conditions, and the test conditions adopted were: adsorbing water at room temperature at 90% humidity; 0% humidity, 90 ℃ desorption of water. As shown in the results of FIG. 4, the MIL-160 layer had good water absorption properties under high humidity conditions at room temperature, with an absolute value of water absorption of 9mg and a relative value of 0.5g water/gMIL-160, indicating that the water-absorbing layer had good water absorption characteristics. At the high temperature of 90 ℃, the MIL-160 layer can rapidly and completely desorb water, thereby ensuring that the mask can adsorb water vapor to keep the filter layer dry in use and can realize the circulation of the desorbed water at the high temperature.
Fig. 5 shows the test results of the medical surgical mask obtained in the present example, and it can be seen that the photothermal regeneration mask obtained in the present example has a bacterial filtration efficiency of over 99%, a particle filtration efficiency of over 96%, and a performance superior to that of the N95 mask. Whereas the bacterial and particulate filtration efficiencies 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, both the industrial-grade graphene powder and the graphene nanosheet can form a very good graphene film on the KN95 melt-blown nonwoven fabric.
The obtained photothermal regeneration mask has good photothermal conversion performance and bacteria and particle filtering performance.
Example 3
This example is substantially the same as example 1, except that ethanol was replaced with ethylene glycol and the compounding ratio was not changed.
The obtained photothermal regeneration mask has good photothermal conversion performance and bacteria and particle filtering efficiency.
Example 4
This example is substantially the same as example 1, except that the amount of ethanol hydrate 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 filtering efficiency.
Example 5
This example is the same as example 1 except that the porous material was a commercial water-absorbent silica gel.
Through detection, the photo-thermal regeneration mask obtained by the implementation has good photo-thermal conversion performance and bacteria and particle filtering efficiency.
Example 6
This example is substantially the same as example 1, except that the amount of the industrial graphene used was 4 g.
Through detection, the photo-thermal regeneration mask obtained by the implementation has good photo-thermal conversion performance and bacteria and particle filtering efficiency.
Example 7
This example is substantially the same as example 1, except that KN95 meltblown nonwoven fabric was replaced with medical gauze.
Through detection, the graphene and the MIL-160 can still well form a compact porous membrane on the surface of the KN95 melt-blown nonwoven fabric, the photothermal conversion performance is similar to that of example 1, and the filtration efficiency of bacteria and particles exceeds 95%.
Example 8
This example is substantially the same as example 1 except that KN95 meltblown nonwoven fabric was replaced with nylon cloth, which was 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 the nylon cloth, the photothermal conversion performance is similar to that of example 1, and the filtration efficiency of bacteria and particles exceeds 95%.
Example 9
This example is similar to example 1 except that KN95 meltblown nonwoven fabric was replaced with cotton cloth, which was repeatedly folded into 3 layers and sewn with stitches.
Through detection, the graphene and the MIL-160 can still well form a compact porous membrane on the surface of cotton cloth, the photothermal conversion performance is similar to that of example 1, and the filtration efficiency of bacteria and particles is over 95%.
Example 10
This example is substantially the same as example 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 filtering efficiency.
Comparative example 1
This comparative example is substantially the same as example 1 except that 100ml of water and 0ml of organic alcohol are used in step 2). And through detection, the graphene and the MIL-160 can not be coated on the surface of the KN95 melt-blown non-woven fabric, and the graphene and the MIL-160 are agglomerated and fall off after being dried. Furthermore, other nanocarbon materials and porous materials have been tried, and a dense porous film cannot be formed on the melt-blown nonwoven fabric. .
Comparative example 2
This comparative example is the same as example 1 except that 90mL of water and 5mL of ethanol were used. Through detection, both the nano carbon and the porous material cannot 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, other nanocarbon materials and porous materials have been tried, and a dense porous film cannot be formed on the melt-blown nonwoven fabric.
Comparative example 3
This comparative example is the same as example 1 except that 80mL of water and 20mL of ethanol were used. Through detection, after the nanocarbon and the porous material are coated on the surface of the KN95 melt-blown non-woven fabric, the solvent penetrates into the melt-blown non-woven fabric, the microstructure of internal melt-blown fibers is damaged, and the filtering efficiency of bacteria and particles is lower than 70%.
It is apparent that the above embodiments are only examples for clearly illustrating and do not limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are therefore intended to be included within the scope of the invention as claimed.
Claims (9)
1. The preparation method of the photothermal regeneration mask core layer material is characterized by comprising 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 porous material slurry;
3) uniformly coating the nano-carbon slurry obtained in the step 1) on one surface of non-woven fabric or woven fabric, 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 woven fabric, and drying; and obtaining the photothermal regeneration mask core layer material.
2. The preparation method according to claim 1, wherein the nano carbon material comprises one or more of but not limited to 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 according to claim 1, wherein the volume ratio of the water to the organic alcohol in step 1) is 5-15: 1; the mass fraction of the nano carbon in the nano carbon slurry is more than 0.5 wt%.
5. The preparation method according to claim 1, wherein the porous material in step 2) is a molecular sieve, a metal organic framework or a porous water absorbing material.
6. The production method according to claim 1, wherein the volume ratio of the water to the organic alcohol in the step 2) is 5 to 15:1, and the mass fraction of the porous material in the obtained porous material slurry is 0.5 wt% or more.
7. The method according to claim 1, wherein the nonwoven fabric or woven fabric is one or more of melt-blown nonwoven fabric for mask, melt-blown nonwoven fabric for air filtration, medical gauze, silk, nylon fabric, cotton fabric, oxford fabric, flannel, and synthetic fiber fabric.
8. The preparation method according to claim 1, wherein the coating method in steps 3 and 4) includes but is not limited to a rolling method, a coating method or a spraying method, and the coating thickness formed by coating the nanocarbon slurry on the surface of the non-woven fabric or the woven fabric is 10-100 μm; the thickness of the coating formed by coating the porous material slurry on the other side of the non-woven fabric or the woven fabric is 10-100 mu m.
9. The photothermal regeneration mask core layer material prepared by the preparation method according to any one of claims 1 to 8.
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