CN114343273A - Antibacterial activated carbon mask and preparation method thereof - Google Patents
Antibacterial activated carbon mask and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an antibacterial activated carbon mask and a preparation method thereof. The antibacterial activated carbon mask comprises a photocatalyst melt-blown non-woven fabric outer layer, an activated carbon melt-blown non-woven fabric inner layer and a pure cotton spunlace non-woven fabric surface layer from outside to inside respectively; the photocatalyst melt-blown non-woven fabric layer is added with titanium dioxide doped with metal nickel and an antibacterial agent prepared from graphene oxide, ferric chloride and bacterial cellulose. The antibacterial activated carbon mask is prepared by combining the outer layer with the photocatalytic degradation effect, the copper-doped activated carbon filtering inner layer and the skin-friendly spunlace non-woven fabric surface layer, and has the advantages of simple preparation process, good matching property of each functional layer, good antibacterial performance, high filtering efficiency on particles and stable long-term service performance.
Description
Technical Field
The invention belongs to the technical field of masks, and particularly relates to an antibacterial activated carbon mask and a preparation method thereof.
Background
With the continuous development of science and technology, the continuous improvement of the living standard of people and the gradual and severe environmental pollution, the protection consciousness of people is strengthened, and the mask becomes a necessary product for life. The mask is generally a device worn on the mouth and nose for filtering air entering the mouth and nose so as to prevent harmful gas, smell and spray from leaching out of the mouth and nose of a wearer. The mask has a certain filtering effect on air entering the lung, has a very good effect when being worn in respiratory infectious diseases and working in dust and other polluted environments, and particularly becomes an article which is necessary to be worn when people go out in cities with serious haze.
Gauze mask on the market usually adopts multilayer gauze or non-woven fabrics to overlap and makes into the gauze mask, the gauze mask can cover nose and mouth when using, in order to reach the tiny granule in the filtered air, or when the dust degree in the air is very big, just need increase the number of piles of gauze or non-woven fabrics, or increase the weaving density of gauze or non-woven fabrics, can lead to the air permeability of gauze mask to reduce like this, carbon dioxide, heat, the gaseous state moisture that produce when people breathe can not go out, the people can produce the sensation of vexing, even cause the inside moisture condensation of material, produce the sensation of coolness, because the steam of exhalation flows hardly to discharge in the gauze mask, become the hotbed of bacterium, therefore it is very necessary to develop an antibiotic type gauze mask.
CN 112826162A discloses a method for manufacturing a biomass-based nitrogen-doped activated carbon mask, which uses triazine ring cross-linked cellulose as a biomass carbon source, uses triazine ring as a nitrogen source, and prepares holes through high-temperature carbonization and zinc chloride, so as to obtain biomass-based nitrogen-doped activated carbon, the pore structure is rich, the specific surface area is larger, a huge adsorption space is provided for fine particles such as PM2.5, and nitrogen is doped in the activated carbon layer structure to form a large amount of pyridine nitrogen, graphite nitrogen and other nitrogen-containing functional groups, lone pair electrons of the nitrogen-containing functional groups have a strong adsorption effect on formaldehyde, and can be used as active adsorption sites of formaldehyde, and the graphite nitrogen structure increases the electron cloud density around the carbon layer, so that the biomass-based nitrogen-doped activated carbon mask has an excellent adsorption effect on toxic gases such as formaldehyde and PM2.5 through electrostatic attraction on carbonyl positive ions in the formaldehyde structure. Although the mask prepared by the invention has excellent adsorption effect on formaldehyde gas and PM2.5, the preparation of the raw material triazine ring cross-linked cellulose for preparing the biomass-based nitrogen-doped activated carbon is very complicated, the triazine ring is used as a nitrogen source, the reaction condition is harsh, the cost is high, and the antibacterial effect is not strong.
Disclosure of Invention
In view of the defects of the prior art, the technical problem to be solved by the invention is to provide an antibacterial activated carbon mask and a preparation method thereof.
In order to achieve the aim, the invention provides an antibacterial activated carbon mask, which is characterized in that a photocatalyst melt-blown non-woven fabric outer layer, an activated carbon melt-blown non-woven fabric inner layer and a pure cotton spunlace non-woven fabric surface layer are sequentially stacked from top to bottom; placing the nose bridge strip in the middle of the upper end of the outer layer of the photocatalyst melt-blown non-woven fabric, and covering the nose bridge strip by the non-woven fabric; placing two ear belts at the left and right ends of the outer layer of the photocatalyst melt-blown non-woven fabric respectively; then hot pressing is carried out to obtain the product; the photocatalyst melt-blown non-woven fabric is characterized in that a composite nano antibacterial agent prepared from graphene oxide, ferric chloride and bacterial cellulose is added in the outer layer of the photocatalyst melt-blown non-woven fabric. The non-woven fabric used in the invention is a non-woven fabric, which is a non-woven fabric formed by directly utilizing high polymer slices, short fibers or filaments to form a net through air flow or machinery, then carrying out processes such as spunlace, needling, spun-bonding, melt-blowing and the like, and finally carrying out after-treatment, and is a novel fiber product with soft, air-permeable and planar structures. The spunbonded and melt-blown non-woven fabrics have a complex fiber stacking structure and three-dimensional random distribution of fibers, so that a large number of tiny gaps are contained in the materials, particles surround the fibers and pass through various types of bent channels or paths, resistance of air flow during passing can be greatly reduced, and meanwhile, the spunbonded and melt-blown non-woven fabrics have high production speed and excellent structural performance, so that the spunbonded and melt-blown non-woven fabrics are widely applied to the mask filtering market.
Titanium dioxide has the advantages of no toxicity, opaqueness, whiteness and brightness, good ultraviolet shielding effect, capability of generating electron transition to generate oxidizing free radicals in the presence of ultraviolet rays to have photocatalytic oxidation performance, and is widely applied to the field of photocatalysis as the most common photocatalyst. However, titanium dioxide has a weak photocatalytic ability in an environment where visible light or light is weak. According to the invention, metal nickel is doped in a common preparation method of titanium dioxide to improve the photocatalytic performance of the titanium dioxide, and the outer layer structure of the mask is prepared from the material.
Further preferably, the preparation method of the photocatalyst melt-blown non-woven fabric outer layer comprises the following steps:
s1, stirring and mixing cetyl trimethyl ammonium bromide, absolute ethyl alcohol and tetrabutyl titanate uniformly to obtain a light yellow solution I; then adding glacial acetic acid and water dropwise into the light yellow solution I; stirring and aging at 50-70 ℃ to obtain milky white gel; calcining the milky white gel at 450-550 ℃ for 3-5 h, naturally cooling, crushing and sieving to obtain titanium dioxide powder;
s2, adding nickel nitrate hexahydrate into water, and stirring to form a solution II; adding the titanium dioxide powder obtained in the step S1 into the solution II for ultrasonic dispersion, and then soaking for 10-15 h; filtering, drying the insoluble substance, calcining at 450-550 ℃ for 3-5 h, naturally cooling, crushing and sieving to obtain titanium dioxide powder, and obtaining nickel-doped titanium dioxide powder;
s3, uniformly dispersing the nickel-doped titanium dioxide powder obtained in the step S2, sodium dodecyl benzene sulfonate and water, and then mixing the uniformly dispersed titanium dioxide powder with the composite nano antibacterial agent to obtain a coating liquid; coating a coating liquid on one surface of the melt-blown non-woven fabric, wherein the coating amount is 6-8 g/m in terms of the amount of nickel-doped titanium dioxide powder2(ii) a Drying; and obtaining the photocatalyst melt-blown non-woven fabric outer layer.
Further preferably, the preparation method of the photocatalyst melt-blown non-woven fabric outer layer comprises the following steps:
s1, adding 0.5-1 part by weight of hexadecyl trimethyl ammonium bromide into 20-25 parts by weight of absolute ethyl alcohol at the temperature of 20-30 ℃, stirring to obtain a clear solution, adding 3-6 parts by weight of tetrabutyl titanate, and continuing stirring to obtain a light yellow solution I; then adding 1-1.5 parts by weight of glacial acetic acid and 2-3 parts by weight of water into the light yellow solution I; stirring and aging at 50-70 ℃ to obtain milky white gel; calcining the milky white gel at 450-550 ℃ for 3-5 h, naturally cooling to 20-30 ℃, and then crushing and sieving to obtain 300-500-mesh titanium dioxide powder;
s2, adding 5-10 parts by weight of nickel nitrate hexahydrate into 100-150 parts by weight of water, and stirring to form a solution II; adding 5-10 parts by weight of the titanium dioxide powder obtained in the step S1 into the solution II, performing ultrasonic dispersion for 30-60 min, and then soaking for 10-15 h; after filtering, drying the insoluble substance at 100-130 ℃ for 2-5 h, then calcining at 450-550 ℃ for 3-5 h, naturally cooling to 20-30 ℃, and crushing and sieving to obtain titanium dioxide powder with 300-500 meshes to obtain nickel-doped titanium dioxide powder;
s3, dispersing 5-10 parts by weight of the nickel-doped titanium dioxide powder obtained in the step S2, 0.2-0.5 part by weight of sodium dodecyl benzene sulfonate and 100-150 parts by weight of water, and then mixing with 0.1-0.2 part by weight of the composite nano antibacterial agent to obtain a coating liquid; coating a coating liquid on one surface of the melt-blown non-woven fabric, wherein the coating amount is 6-8 g/m in terms of the amount of nickel-doped titanium dioxide powder2(ii) a Drying; and obtaining the photocatalyst melt-blown non-woven fabric outer layer.
Preferably, the preparation method of the composite nano antibacterial agent in the step S3 is as follows:
10-15g of graphene oxide and 0.5-0.8g of FeCl3·6H2Dissolving O in 30-50mL of ethylene glycol to obtain a mixed solution 1, adding 1.5-2g of ammonium acetate and 0.5-1g of bacterial cellulose into the mixed solution 1, performing ultrasonic dispersion for 1-1.5h to obtain a mixed solution 2, transferring the mixed solution 2 into a polytetrafluoroethylene-lined autoclave, reacting at the temperature of 150 ℃ and 200 ℃ for 10-12h, filtering after the reaction is finished, collecting filter residues, respectively washing the filter residues with water and absolute ethyl alcohol for 3 times, and then placing the filter residues in a 50-70 ℃ drying box for drying for 10-12h to obtain the composite nano antibacterial agent.
Activated carbon is the most commonly used and cheap adsorbent at present, and is essentially a porous carbide, which is prepared by heating organic raw materials (such as shells, coal, wood and other materials rich in carbon and hydrogen) under the condition of isolating air to reduce non-carbon components (the process is called carbonization), and then reacting with gas to corrode the surface and generate a structure with developed micropores (the process is called activation). The activation process is a microscopic process, i.e. the surface erosion of a large amount of molecular carbides is point erosion, so that the surface of the activated carbon has numerous fine pores and a very rich pore structure, and the activated carbon has a developed microporous structure and a large specific surface area and can adsorb gas and liquid. The active carbon is added into the mask, so that particles with smaller diameters can be effectively prevented from invading the mouth and nose of a human body, and harmful gases such as benzene, formaldehyde, stink and the like in the air can be effectively blocked, so that the effects of dust prevention, poison prevention and bacteria prevention are achieved. Some prior arts study on benzene and toluene adsorbed by activated carbon, and experiments show that the activated carbon can effectively adsorb organic solvents and has certain selectivity.
The preparation raw material source of the activated carbon is rich, the preparation process is simple, and the activated carbon material with high surface area can be prepared by adding salt with low melting point and substances which are easy to react with carbon and etching the carbon matrix. Some researches can prepare the active carbon precursor with the specific surface area more than 2500m by carrying out hydrothermal decomposition on the active carbon precursor or adding cellulase, promoting a reaction agent to react with the carbon substrate at high temperature and adopting a multi-stage carbonization mode2Per gram of activated carbon. Although a high specific surface area favors the adsorption of harmful substances by the activated carbon. The inventor finds that the specific surface area is not the only factor influencing the adsorption of PM2.5, the increase of the active carbon reaction sites and the introduction of active substances to act with PM2.5 particles are more effective modes. Meanwhile, a large amount of activating substances are used for etching the activated carbon precursor, so that the preparation conditions are complicated, the cost is increased, and commonly used activating agents such as KOH, NaOH and ZnCl are adopted2The corrosion to the instrument is increased and more harmful gas is also discharged.
The preparation method of the activated carbon in the prior art generally comprises the steps of blending a carbon precursor with an activating agent or soaking the carbon precursor in an activating agent solution, then calcining in an inert gas, and washing out inorganic impurities to prepare the activated carbon with high specific surface area. The method does not depend on the high specific surface area of the activated carbon, and active species are formed in situ during calcination, so that the pore structure of the activated carbon can be blocked, and the overall activity is reduced; the appearance of active species on the surface of the active carbon is adjusted by adding a specific structure regulator.
Based on the above, the invention uses waste bamboo as the precursor of the active carbon, uses the trihydrate copper nitrate with small corrosion to the instrument and the structure regulator to prepare the active carbon with stronger functionality, and uses the active carbon as the effective material of the filter layer in the mask.
The preparation method of the activated carbon melt-blown non-woven fabric comprises the following steps:
(1) preparing bamboo powder;
(2) soaking bamboo powder in copper nitrate solution; after filtering, drying the insoluble substances, and then calcining the insoluble substances under inert gas to obtain copper-doped activated carbon;
(3) and mixing the copper-doped activated carbon with the dispersion liquid to obtain a coating liquid, and coating the coating liquid on the melt-blown non-woven fabric to obtain the activated carbon melt-blown non-woven fabric.
Further preferably, the preparation method of the activated carbon melt-blown non-woven fabric comprises the following steps:
(1) cleaning waste bamboo stalks, and drying at 80-120 ℃ for 6-8 h; then crushing to obtain bamboo powder;
(2) adding 2-5 parts by weight of copper nitrate trihydrate and 0.02-0.05 part by weight of a structure regulator into 100-150 parts by weight of water, and stirring to form a solution A; adding 5-10 parts by weight of the bamboo powder obtained in the step (1) into the solution A, and soaking for 12-15 hours; filtering, and drying the insoluble substances at the temperature of 60-80 ℃ for 6-8 h; calcining for 2-5 h at 650-850 ℃ in an inert gas atmosphere, naturally cooling to 20-30 ℃, washing the powder with water and acetone for three times respectively, drying for 6-8 h at 60-80 ℃, and crushing and sieving to obtain 300-500-mesh copper-doped activated carbon;
(3) dispersing 5-10 parts by weight of the copper-doped activated carbon obtained in the step (2), 0.2-0.5 part by weight of sodium dodecyl benzene sulfonate and 100-150 parts by weight of water to obtain a coating liquid; coating the coating liquid on two sides of the melt-blown non-woven fabric, wherein the coating amount is 30-60 g/m in terms of the amount of the copper-doped activated carbon2(ii) a And drying to obtain the activated carbon melt-blown non-woven fabric.
Preferably, the bamboo powder in the step (1) has a mesh number of 300-500 meshes.
Preferably, the structure regulator in the step (2) is at least one of 1-ethyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt, 1-butyl-2, 3-dimethylimidazole hexafluorophosphate, hexamethylenetetramine and ethylenediamine.
Further preferably, the structure regulator in the step (2) is 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt and hexamethylenetetramine in a mass ratio of (2-4): 1, and uniformly mixing to obtain the product.
Preferably, the temperature rise rate of the calcination in the step (2) is 2-10 ℃/min.
Preferably, the dispersing speed in the step (3) is 1200-1800 r/min.
The invention also provides a preparation method of the antibacterial activated carbon mask, which comprises the following steps: according to the preparation method of the common mask, the photocatalyst melt-blown non-woven fabric outer layer, the activated carbon melt-blown non-woven fabric inner layer and the pure cotton spunlace non-woven fabric surface layer are sequentially stacked from top to bottom; placing the nose bridge strip in the middle of the upper end of the outer layer of the photocatalyst melt-blown non-woven fabric, and covering the nose bridge strip by the non-woven fabric; placing two ear belts at the left and right ends of the outer layer of the photocatalyst melt-blown non-woven fabric respectively; then hot pressing to obtain the antibacterial active carbon mask.
The invention has the beneficial effects that:
(1) the antibacterial activated carbon mask is prepared by combining the outer layer with photocatalytic degradation, the copper-doped activated carbon filtering inner layer and the skin-friendly spunlace non-woven fabric surface layer, the preparation process is simple, the functional layers are good in matching performance, the filtering efficiency on particles is high, and the mask has stable long-term service performance.
(2) The biomass waste is comprehensively utilized, the waste bamboo is used as a precursor of the activated carbon, the copper nitrate trihydrate is used as a mild modifier and a functional agent, and a structure regulator is added, so that the performance of the copper-doped activated carbon is obviously improved, and the filtering efficiency of the antibacterial activated carbon mask is further improved.
(3) The composite nano antibacterial agent prepared from graphene oxide, ferric chloride and bacterial cellulose is added on the outer layer of the photocatalyst melt-blown non-woven fabric, so that the antibacterial performance of the non-woven fabric layer is effectively improved.
Drawings
FIG. 1 is a field emission scanning electron microscope image of the activated carbon prepared by the invention, wherein A is example 1, B is example 2, C is example 3, D is example 4, E is comparative example 1, and F is comparative example 2.
Fig. 2 is a graph showing the change of the filtering efficiency of the masks according to the present invention in the simulated human breathing environment, which is prepared in example 4 and comparative example 3, with time.
Detailed Description
Part of the raw materials used in the invention are introduced:
melt-blown nonwoven fabric having a grammage of 40g/m2。
Pure cotton spunlaced nonwoven fabric with gram weight of 100g/m2。
The waste bamboo stalks were collected from Wuhan City.
KN95 melt-blown nonwoven fabric with a grammage of 50g/m2。
Example 1
A preparation method of an antibacterial activated carbon mask comprises the following steps: according to the preparation method of the common mask, the photocatalyst melt-blown non-woven fabric outer layer, the activated carbon melt-blown non-woven fabric inner layer and the pure cotton spunlace non-woven fabric surface layer are cut into the specifications with the upper and lower heights of 95mm and the left and right widths of 175mm, and the photocatalyst melt-blown non-woven fabric outer layer, the activated carbon melt-blown non-woven fabric inner layer and the pure cotton spunlace non-woven fabric surface layer are sequentially stacked from top to bottom; placing the nose bridge strip at the position, which is 8mm away from the upper sideline and is centered left and right, of the outer layer of the photocatalyst melt-blown non-woven fabric, and covering the nose bridge strip by the non-woven fabric; placing two ear belts at the left end and the right end of the outer layer of the photocatalyst melt-blown non-woven fabric respectively, wherein the distance between the two ear belts is 5mm from the upper side line and the lower side line; and then carrying out hot pressing to obtain the antibacterial activated carbon mask.
The preparation method of the photocatalyst melt-blown non-woven fabric outer layer comprises the following steps:
s1, adding 0.5g of hexadecyl trimethyl ammonium bromide into 25g of absolute ethyl alcohol at 25 ℃, stirring at the speed of 300r/min for 5min to obtain a clear solution, adding 5g of tetrabutyl titanate, and continuously stirring for 10min to obtain a light yellow solution I; then 1g of glacial acetic acid and 2g of water are added into the light yellow solution I; stirring at 60 deg.C for 6h, aging for 24h to obtain milky white gel; calcining the milky white gel at 550 ℃ for 3h, naturally cooling to 25 ℃, and then crushing and sieving to obtain 325-mesh titanium dioxide powder;
s2, adding 5g of nickel nitrate hexahydrate into 150g of water, and stirring to form a solution II; adding 10g of the titanium dioxide powder obtained in the step S1 into the solution II, dispersing for 30min at the ultrasonic power of 80W and the frequency of 50kHz, and then soaking for 12 h; after filtration, drying the insoluble substances at 120 ℃ for 2h, then calcining at 550 ℃ for 3h, naturally cooling to 25 ℃, and crushing and sieving to obtain 325-mesh titanium dioxide powder to obtain nickel-doped titanium dioxide powder;
s3, dispersing 5g of the nickel-doped titanium dioxide powder obtained in the step S2, 0.2g of sodium dodecyl benzene sulfonate and 150g of water for 30min under the dispersion condition of 1500r/min of a high-speed dispersion machine to obtain a coating liquid, and thus obtaining the coating liquid; spraying the coating liquid on one surface of the melt-blown non-woven fabric in an airless spraying manner, wherein the coating weight is 8g/m in terms of nickel-doped titanium dioxide powder2Drying at 60 deg.C for 3 h; and obtaining the photocatalyst melt-blown non-woven fabric outer layer.
The preparation method of the activated carbon melt-blown non-woven fabric inner layer comprises the following steps:
(1) cleaning waste bamboo stalks, and drying at 90 ℃ for 6 hours; then crushing and sieving to obtain 325-mesh bamboo powder;
(2) adding 2g of copper nitrate trihydrate into 150g of water, and stirring at the rotating speed of 300r/min for 5min to form a solution A; adding 5g of the bamboo powder obtained in the step (1) into the solution A, and soaking for 12 hours; filtering, and drying the insoluble substance at 80 deg.C for 6 hr; heating to 700 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2h, naturally cooling to 25 ℃, washing the powder with water and acetone for three times respectively, drying at 60 ℃ for 6h, crushing and sieving to obtain 325-mesh copper-doped activated carbon;
(3) dispersing 5g of the copper-doped activated carbon obtained in the step (2), 0.2g of sodium dodecyl benzene sulfonate and 150g of water for 30min under the dispersion condition of a high-speed dispersion machine at 1500r/min to obtain a coating liquid; spraying the coating liquid on both sides of the melt-blown non-woven fabric in an airless spraying manner, wherein the coating weight is 50g/m in terms of the amount of the copper-doped activated carbon2(ii) a Drying at 60 deg.C for 3h to obtain activated carbon melt-blownNon-woven fabrics;
example 2
The preparation method of the antibacterial activated carbon mask is basically the same as that of the antibacterial activated carbon mask in example 1, and the differences are only that:
the preparation method of the activated carbon melt-blown non-woven fabric inner layer comprises the following steps:
(1) cleaning waste bamboo stalks, and drying at 90 ℃ for 6 hours; then crushing and sieving to obtain 325-mesh bamboo powder;
(2) adding 2g of copper nitrate trihydrate and 0.02g of hexamethylenetetramine into 150g of water, and stirring at the rotating speed of 300r/min for 5min to form a solution A; adding 5g of the bamboo powder obtained in the step (1) into the solution A, and soaking for 12 hours; filtering, and drying the insoluble substance at 80 deg.C for 6 hr; heating to 700 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2h, naturally cooling to 25 ℃, washing the powder with water and acetone for three times respectively, drying at 60 ℃ for 6h, crushing and sieving to obtain 325-mesh copper-doped activated carbon;
(3) dispersing 5g of the copper-doped activated carbon obtained in the step (2), 0.2g of sodium dodecyl benzene sulfonate and 150g of water for 30min under the dispersion condition of a high-speed dispersion machine at 1500r/min to obtain a coating liquid; spraying the coating liquid on both sides of the melt-blown non-woven fabric in an airless spraying manner, wherein the coating weight is 50g/m in terms of the amount of the copper-doped activated carbon2(ii) a Drying at 60 deg.C for 3h to obtain activated carbon melt-blown nonwoven fabric;
example 3
The preparation method of the antibacterial activated carbon mask is basically the same as that of the antibacterial activated carbon mask in example 1, and the differences are only that:
the preparation method of the activated carbon melt-blown non-woven fabric inner layer comprises the following steps:
(1) cleaning waste bamboo stalks, and drying at 90 ℃ for 6 hours; then crushing and sieving to obtain 325-mesh bamboo powder;
(2) adding 2g of copper nitrate trihydrate and 0.02g of 1-butyl-3-methylimidazole bistrifluoromethanesulfonylimide salt into 150g of water, and stirring at the rotating speed of 300r/min for 5min to form a solution A; adding 5g of the bamboo powder obtained in the step (1) into the solution A, and soaking for 12 hours; filtering, and drying the insoluble substance at 80 deg.C for 6 hr; heating to 700 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2h, naturally cooling to 25 ℃, washing the powder with water and acetone for three times respectively, drying at 60 ℃ for 6h, crushing and sieving to obtain 325-mesh copper-doped activated carbon;
(3) dispersing 5g of the copper-doped activated carbon obtained in the step (2), 0.2g of sodium dodecyl benzene sulfonate and 150g of water for 30min under the dispersion condition of a high-speed dispersion machine at 1500r/min to obtain a coating liquid; spraying the coating liquid on both sides of the melt-blown non-woven fabric in an airless spraying manner, wherein the coating weight is 50g/m in terms of the amount of the copper-doped activated carbon2(ii) a Drying at 60 deg.C for 3h to obtain activated carbon melt-blown nonwoven fabric.
Example 4
The preparation method of the antibacterial activated carbon mask is basically the same as that of the antibacterial activated carbon mask in example 1, and the differences are only that:
the preparation method of the activated carbon melt-blown non-woven fabric inner layer comprises the following steps:
(1) cleaning waste bamboo stalks, and drying at 90 ℃ for 6 hours; then crushing and sieving to obtain 325-mesh bamboo powder;
(2) adding 2g of copper nitrate trihydrate, 0.016g of 1-butyl-3-methylimidazole bistrifluoromethanesulfonylimide salt and 0.004g of hexamethylenetetramine into 150g of water, and stirring at the rotating speed of 300r/min for 5min to form a solution A; adding 5g of the bamboo powder obtained in the step (1) into the solution A, and soaking for 12 hours; filtering, and drying the insoluble substance at 80 deg.C for 6 hr; heating to 700 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2h, naturally cooling to 25 ℃, washing the powder with water and acetone for three times respectively, drying at 60 ℃ for 6h, crushing and sieving to obtain 325-mesh copper-doped activated carbon;
(3) dispersing 5g of the copper-doped activated carbon obtained in the step (2), 0.2g of sodium dodecyl benzene sulfonate and 150g of water for 30min under the dispersion condition of a high-speed dispersion machine at 1500r/min to obtain a coating liquid; spraying the coating liquid on both sides of the melt-blown non-woven fabric in an airless spraying manner, wherein the coating weight is 50g/m in terms of the amount of the copper-doped activated carbon2(ii) a Drying at 60 deg.C for 3h to obtain activated carbon melt-blown nonwoven fabric.
Example 5
The preparation method of the antibacterial activated carbon mask is basically the same as that of the antibacterial activated carbon mask in example 4, and the differences are only that:
the preparation method of the photocatalyst melt-blown non-woven fabric outer layer comprises the following steps:
s1, adding 0.5g of hexadecyl trimethyl ammonium bromide into 25g of absolute ethyl alcohol at 25 ℃, stirring at the speed of 300r/min for 5min to obtain a clear solution, adding 5g of tetrabutyl titanate, and continuously stirring for 10min to obtain a light yellow solution I; then 1g of glacial acetic acid and 2g of water are added into the light yellow solution I; stirring at 60 deg.C for 6h, aging for 24h to obtain milky white gel; calcining the milky white gel at 550 ℃ for 3h, naturally cooling to 25 ℃, and then crushing and sieving to obtain 325-mesh titanium dioxide powder;
s2, adding 5g of nickel nitrate hexahydrate into 150g of water, and stirring to form a solution II; adding 10g of the titanium dioxide powder obtained in the step S1 into the solution II, dispersing for 30min at the ultrasonic power of 80W and the frequency of 50kHz, and then soaking for 12 h; after filtration, drying the insoluble substances at 120 ℃ for 2h, then calcining at 550 ℃ for 3h, naturally cooling to 25 ℃, and crushing and sieving to obtain 325-mesh titanium dioxide powder to obtain nickel-doped titanium dioxide powder;
s3, dispersing 5g of the nickel-doped titanium dioxide powder obtained in the step S2, 0.2g of sodium dodecyl benzene sulfonate and 150g of water for 30min under the dispersion condition of 1500r/min of a high-speed dispersion machine, and then mixing with 0.2g of the composite nano antibacterial agent to obtain a coating liquid, thus obtaining the coating liquid; spraying the coating liquid on one surface of the melt-blown non-woven fabric in an airless spraying manner, wherein the coating weight is 8g/m in terms of nickel-doped titanium dioxide powder2Drying at 60 deg.C for 3 h; and obtaining the photocatalyst melt-blown non-woven fabric outer layer.
The preparation method of the composite nano microbial inoculum comprises the following steps:
10g of graphene oxide and 0.6g of FeCl3·6H2Dissolving O in 40mL of ethylene glycol to obtain a mixed solution 1, adding 1.5g of ammonium acetate and 0.8g of bacterial cellulose into the mixed solution 1, performing ultrasonic dispersion for 1h to obtain a mixed solution 2, transferring the mixed solution 2 into a polytetrafluoroethylene-lined high-pressure kettle, reacting for 10h at 180 ℃, filtering after the reaction is finished, collecting filter residues, washing the filter residues respectively with water and absolute ethyl alcohol for 3 times, and then placing the filter residues in a 60-position drying box for drying for 12h to obtain the composite nano antibacterial agent.
Comparative example 1
The preparation method of the antibacterial activated carbon mask is basically the same as that of the antibacterial activated carbon mask in example 1, and the differences are only that:
the preparation method of the activated carbon melt-blown non-woven fabric inner layer comprises the following steps:
(1) cleaning waste bamboo stalks, and drying at 90 ℃ for 6 hours; then crushing and sieving to obtain 325-mesh bamboo powder;
(2) heating bamboo powder to 700 deg.C at a heating rate of 5 deg.C/min in nitrogen atmosphere, maintaining for 2 hr, naturally cooling to 25 deg.C, washing the powder with water and acetone for three times, drying at 60 deg.C for 6 hr, pulverizing, and sieving to obtain 325 mesh active carbon;
(3) dispersing 5g of the activated carbon obtained in the step (2), 0.2g of sodium dodecyl benzene sulfonate and 150g of water for 30min under the dispersion condition of a high-speed dispersion machine 1500r/min to obtain a coating liquid; spraying the coating liquid on both sides of the melt-blown non-woven fabric in an airless spraying manner, wherein the coating weight is 50g/m in terms of the amount of the copper-doped activated carbon2(ii) a Drying at 60 deg.C for 3h to obtain activated carbon melt-blown nonwoven fabric.
Comparative example 2
The preparation method of the antibacterial activated carbon mask is basically the same as that of the antibacterial activated carbon mask in example 1, and the differences are only that: in the preparation of the activated carbon melt-blown non-woven fabric inner layer, KOH activated carbon is used for replacing copper-doped activated carbon in the activated carbon melt-blown non-woven fabric inner layer.
The preparation method of the KOH activated carbon comprises the following steps: cleaning waste bamboo stalks, and drying at 90 ℃ for 6 hours; then crushing and sieving to obtain 325-mesh bamboo powder; mixing 325-mesh bamboo powder with 5 times of KOH by mass at 25 ℃, heating to 750 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and naturally cooling to 25 ℃; the solid was immersed in 2mol/L hydrochloric acid, washed with water to give a supernatant having a pH of 7.0, and the insoluble matter was filtered, dried in an oven at 100 ℃ for 6 hours, and then pulverized and sieved to obtain 325 mesh KOH activated carbon.
Comparative example 3
The preparation method of the antibacterial activated carbon mask is basically the same as that of the antibacterial activated carbon mask in example 1, and the only difference is that: KN95 melt-blown nonwoven fabric is used for replacing the inner layer of the activated carbon melt-blown nonwoven fabric.
Test example 1 structural test of activated carbon
The morphology of the activated carbon materials prepared in examples 1 to 4 and comparative examples 1 to 2 of the present invention was tested by using a field emission scanning electron microscope, and the results are shown in fig. 1. In FIG. 1, example A1, example B2, example C3, example D4, comparative example E1, and comparative example F2. It can be seen that the direct calcination of activated carbon from bamboo powder of comparative example 1 (fig. 1E) and the KOH-activated carbon of comparative example 2 (fig. 1F) have a significant etching of the bamboo structure by KOH activation, and the KOH-activated bamboo powder has a large amount of irregular pore structures, which significantly increases the specific surface area of the activated carbon. Example 1 copper nitrate trihydrate added the copper doped activated carbon (figure 1A) prepared with a similar overall structure to that of comparative example 1, with randomly distributed, distinct spherical particles (XRD analysis shows copper or cuprous oxide) present on the surface, indicating that the copper nitrate trihydrate, when added, is reduced in situ to lower valence copper species at high temperature, embedded in the activated carbon surface. Examples 2 to 4 are similar to example 1 in their entirety except that the particles (copper or cuprous oxide by XRD analysis) on the surface have different shapes and sizes. Example 2 (fig. 1B) copper-doped activated carbon prepared by adding copper nitrate trihydrate and hexamethylenetetramine, the copper species on the surface of the activated carbon are obviously refined and widely dispersed on the surface of the activated carbon; example 3 (fig. 1C) copper-doped activated carbon prepared by adding copper nitrate trihydrate, 1-butyl-3-methylimidazolium bistrifluoromethylsulfonimide salt, the copper species become coarse and distributed in clusters on the activated carbon surface; example 4 (fig. 1D) copper-doped activated carbon prepared by adding copper nitrate trihydrate, 1-butyl-3-methylimidazolium bistrifluoromethanesulfonimide salt, hexamethylenetetramine, copper species are dispersed most uniformly without significant agglomeration and the presence of large particles. These results indicate that hexamethylenetetramine and 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt have a great influence on the morphology of copper species in copper-doped activated carbon. This is probably because hexamethylenetetramine and 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt enhance the action of bamboo powder in a liquid phase environment and copper ions, hexamethylenetetramine is added to refine in-situ generated copper species, and 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt can properly disperse copper species on the surface and promote decomposition to form a coarse structure; the combined action of the hexamethylenetetramine and the 1-butyl-3-methylimidazole bistrifluoromethanesulfonylimide salt ensures that the copper species on the surface of the activated carbon has uniform structure and appearance and rougher surface.
Specific surface area tests were performed using a nitrogen adsorption test to determine the specific surface areas of the activated carbon materials prepared in examples 1 to 4 of the present invention and comparative examples 1 to 2, and the results are shown in table 1.
TABLE 1 specific surface area results for activated carbon materials
From the results of comparative example 1 and example 1, it is seen that the addition of copper nitrate trihydrate increases the surface area of the activated carbon and the pore size structure, and the specific surface areas of comparative examples 2 to 4 are further increased, which indicates that the addition of hexamethylenetetramine and 1-butyl-3-methylimidazole bistrifluoromethane sulfimide salt can enhance the decomposition of bamboo powder and introduce the pore structure, and the combination of hexamethylenetetramine and 1-butyl-3-methylimidazole bistrifluoromethane sulfimide salt has stronger etching effect on bamboo powder. Although the activated carbon prepared by KOH activation in the comparative example has the highest specific surface area, the pore diameter is concentrated in micropores, and the activated carbon is easy to adsorb micro impurities and lose activity, so that the activated carbon is not suitable for preparing a PM 2.5-proof mask.
Test example 2 mask Performance test
PM2.5 contacted in life is mainly non-oily particulate matters such as dust with different sizes, and smaller particles can enter alveoli to influence the health of human bodies. Therefore, the non-oily particulate matter filtration efficiency is an important index of the PM 2.5-proof mask. The invention uses an automatic filter material tester, and uses NaCl aerogel to simulate PM2.5 under the condition of 85L +/-1L/min air flow, so as to test the filtering efficiency and the respiratory resistance of the mask; the NaCl aerogel used has a particle size distribution with a median particle number diameter of 0.075 μm +/-0.020 μm, a geometric standard deviation within 1.86, and a concentration of less than 200mg/m3. The results of the filtration efficiency of the mask are shown in table 2.
TABLE 2 filtration efficiency of the mask
As can be seen from the results of table 2, the filtration efficiency of the activated carbon prepared by direct carbonization of bamboo powder in comparative example 1 and activated carbon prepared by KOH activation in comparative example 2 as the filtration inner layer material of the mask was limited and not met the standards. Comparative example 3 the filtration efficiency reached 96.7% using KN95 melt blown nonwoven fabric as the inner filtration layer. Comparative example 4 when copper-doped activated carbon prepared from copper nitrate trihydrate, 1-butyl-3-methylimidazolium bistrifluoromethylsulfonyl imide salt, and hexamethylenetetramine was used as a material for the inner filtration layer, the filtration efficiency was 97.3%. The reason for this is probably that the addition of 1-butyl-3-methylimidazole bistrifluoromethylsulfonyl imide salt and hexamethylenetetramine promotes the decomposition of carbon matrix to increase the specific surface area of the activated carbon, so that the copper species on the surface of the activated carbon has uniform structure and appearance and rougher surface, the copper-doped activated carbon has larger pore diameter and more binding sites, and particles can be effectively adsorbed.
The inner layer of the melt-blown filtering layer of the mask used in the market captures air dust particles by utilizing the electrostatic force effect of electric charges, and when the mask is used, the moisture consumption electric charges can not avoid causing the failure of the capturing effect of the functional layer and the frequent replacement of the mask. The long-term service performance test of the monitoring mask is very important. The human oral cavity breathing environment that this test utilized constant temperature and humidity case simulation puts into the gauze mask under the setting temperature is 37 ℃, relative humidity is 80% environment, takes out gauze mask test filtration performance every 2h, tests 8h in succession, records the filtration efficiency of every time quantum. The results are shown in FIG. 2.
The results in fig. 2 show that the mask prepared in example 4 of the present invention has no significant decrease in filtration efficiency in 8h of simulated use, and the sustained filtration effect of the inner layer of filter material is significantly better than that of KN95 meltblown. These results indicate that the mask prepared in example 4 of the present invention has good filtering efficiency and long-term use.
Test example 3 antibacterial Effect test
The outer layers of the photocatalyst melt-blown non-woven fabrics prepared in the examples 4 and 5 are subjected to a sterilization rate test with reference to GB15979-2002 hygienic Standard for Disposable sanitary products appendix C product sterilization performance, bacteriostatic performance and stability test method, the action time is 5min, the specific test data is shown in Table 3, wherein Escherichia coli is purchased from China Industrial microbial strain preservation management center, and the strain number is CICC 10899; staphylococcus aureus was purchased from China center for Industrial culture Collection of microorganisms with the strain number CICC 21600.
TABLE 3 test results of outer layer sterilization rate of photocatalyst melt-blown non-woven fabric
As is clear from the data in Table 3, graphene oxide and FeCl were added3·6H2The sterilization rate of the photocatalyst melt-blown non-woven fabric outer layer of the composite nano antibacterial agent prepared from O and bacterial cellulose is obviously higher than that of the photocatalyst melt-blown non-woven fabric without adding graphene oxide and FeCl3·6H2O, the photocatalyst melt-blown non-woven fabric outer layer of the composite nano antibacterial agent prepared from the bacterial cellulose possibly causes that the composite nano antibacterial agent is adsorbed on the surface of bacteria, the permeability of cell walls of the bacteria is changed, the cell structure of the bacteria is damaged, substances in the cells flow out, and the bacteria lose the metabolism capability to achieve the sterilization effect.
Claims (10)
1. A preparation method of an antibacterial activated carbon mask comprises sequentially stacking a photocatalyst melt-blown non-woven fabric outer layer, an activated carbon melt-blown non-woven fabric inner layer and a pure cotton spunlace non-woven fabric surface layer from top to bottom; placing the nose bridge strip in the middle of the upper end of the outer layer of the photocatalyst melt-blown non-woven fabric, and covering the nose bridge strip by the non-woven fabric; placing two ear belts at the left and right ends of the outer layer of the photocatalyst melt-blown non-woven fabric respectively; then hot pressing is carried out to obtain the product; the method is characterized in that: the photocatalyst melt-blown non-woven fabric is characterized in that a composite nano antibacterial agent prepared from graphene oxide, ferric chloride and bacterial cellulose is added in the outer layer of the photocatalyst melt-blown non-woven fabric.
2. The method for preparing an antibacterial activated carbon mask according to claim 1, wherein the step of preparing the photocatalyst melt-blown non-woven fabric outer layer comprises the following steps:
s1, stirring and mixing cetyl trimethyl ammonium bromide, absolute ethyl alcohol and tetrabutyl titanate uniformly to obtain a light yellow solution I; then adding glacial acetic acid and water dropwise into the light yellow solution I; stirring and aging at 50-70 ℃ to obtain milky white gel; calcining the milky white gel at 450-550 ℃ for 3-5 h, naturally cooling, crushing and sieving to obtain titanium dioxide powder;
s2, adding nickel nitrate hexahydrate into water, and stirring to form a solution II; adding the titanium dioxide powder obtained in the step S1 into the solution II for ultrasonic dispersion, and then soaking for 10-15 h; filtering, drying the insoluble substance, calcining at 450-550 ℃ for 3-5 h, naturally cooling, crushing and sieving to obtain titanium dioxide powder, and obtaining nickel-doped titanium dioxide powder;
s3, uniformly dispersing the nickel-doped titanium dioxide powder obtained in the step S2, sodium dodecyl benzene sulfonate and water, and then mixing the uniformly dispersed titanium dioxide powder with the composite nano antibacterial agent to obtain a coating liquid; coating a coating liquid on one surface of the melt-blown non-woven fabric, wherein the coating amount is 6-8 g/m in terms of the amount of nickel-doped titanium dioxide powder2(ii) a Drying; and obtaining the photocatalyst melt-blown non-woven fabric outer layer.
3. The method for preparing an antibacterial activated carbon mask according to claim 1, wherein the method for preparing the activated carbon melt-blown non-woven fabric inner layer comprises the following steps:
(1) preparing bamboo powder;
(2) soaking bamboo powder in copper nitrate solution; after filtering, drying the insoluble substances, and then calcining the insoluble substances under inert gas to obtain copper-doped activated carbon;
(3) and mixing the copper-doped activated carbon with the dispersion liquid to obtain a coating liquid, and coating the coating liquid on the melt-blown non-woven fabric to obtain the activated carbon melt-blown non-woven fabric.
4. The method for preparing an antibacterial activated carbon mask according to claim 3, wherein the method for preparing the activated carbon melt-blown non-woven fabric inner layer comprises the following steps:
(1) cleaning waste bamboo stalks, and drying at 80-120 ℃ for 6-8 h; then crushing to obtain bamboo powder;
(2) adding 2-5 parts by weight of copper nitrate trihydrate and 0.02-0.05 part by weight of structure regulator into 100-150 parts by weight of water, and stirring to form a solution II; adding 5-10 parts by weight of the bamboo powder obtained in the step (1) into the solution II, and soaking for 12-15 hours; filtering, and drying the insoluble substances at the temperature of 60-80 ℃ for 6-8 h; calcining for 2-5 h at 650-850 ℃ in an inert gas atmosphere, naturally cooling to 20-30 ℃, washing the powder with water and acetone for three times respectively, drying for 6-8 h at 60-80 ℃, and crushing and sieving to obtain 300-500-mesh copper-doped activated carbon;
(3) dispersing 5-10 parts by weight of the copper-doped activated carbon obtained in the step (2), 0.2-0.5 part by weight of sodium dodecyl benzene sulfonate and 100-150 parts by weight of water to obtain a coating liquid; coating the coating liquid on two sides of the melt-blown non-woven fabric, wherein the coating amount is 30-60 g/m in terms of the amount of the copper-doped activated carbon2(ii) a And drying to obtain the activated carbon melt-blown non-woven fabric.
5. The method of manufacturing an antibacterial activated carbon mask according to claim 4, wherein the bamboo powder in step (1) has a mesh size of 300 to 500 mesh.
6. The method of manufacturing an antibacterial activated carbon mask according to claim 4, wherein the structure modifier in the step (2) is at least one of 1-ethyl-3-methylimidazolium chloride salt, 1-butyl-3-methylimidazolium bistrifluoromethylsulfonimide salt, 1-butyl-2, 3-dimethylimidazolium hexafluorophosphate, hexamethylenetetramine, and ethylenediamine.
7. The method for preparing an antibacterial activated carbon mask according to claim 4, wherein the structure regulator in the step (2) is 1-butyl-3-methylimidazolium bistrifluoromethylsulfonyl imide salt and hexamethylenetetramine in a mass ratio of (2-4): 1 are mixed to obtain the product.
8. The method for preparing an antibacterial activated carbon mask according to claim 4, wherein the temperature rise rate of the calcination in the step (2) is 2-10 ℃/min.
9. The method for preparing an antibacterial activated carbon mask according to claim 1 or 2, wherein the method for preparing the composite nano antibacterial agent comprises the following steps: 10-15g of graphene oxide and 0.5-0.8g of FeCl3·6H2Dissolving O in 30-50mL of ethylene glycol to obtain a mixed solution 1, adding 1.5-2g of ammonium acetate and 0.5-1g of bacterial cellulose into the mixed solution 1, performing ultrasonic dispersion for 1-1.5h to obtain a mixed solution 2, transferring the mixed solution 2 into a polytetrafluoroethylene-lined autoclave to react at the temperature of 150 ℃ and 200 ℃ for 10-12h, filtering after the reaction is finished, collecting filter residues, respectively washing the filter residues with water and absolute ethyl alcohol for 3 times, then placing the filter residues in a drying box for 50-70, and drying the filter residues in the drying box for 10-12h to obtain the composite nano antibacterial agent.
10. An antibacterial active carbon mask is characterized in that: prepared by the method of any one of claims 1 to 9.
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| CN206586434U (en) * | 2017-03-17 | 2017-10-27 | 王妍 | Catalyst mouth mask |
| CN108618235A (en) * | 2017-03-17 | 2018-10-09 | 王妍 | catalyst mask |
| CN111374152A (en) * | 2020-03-24 | 2020-07-07 | 高登科学(深圳)有限公司 | Bactericide and preparation method thereof, and air filter, mask, modified emulsion paint and modified concrete |
| CN111481850A (en) * | 2020-05-22 | 2020-08-04 | 深圳三爱美容科技有限公司 | Mask with traditional Chinese medicine tablet for supplying fresh air |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN206586434U (en) * | 2017-03-17 | 2017-10-27 | 王妍 | Catalyst mouth mask |
| CN108618235A (en) * | 2017-03-17 | 2018-10-09 | 王妍 | catalyst mask |
| CN111374152A (en) * | 2020-03-24 | 2020-07-07 | 高登科学(深圳)有限公司 | Bactericide and preparation method thereof, and air filter, mask, modified emulsion paint and modified concrete |
| CN111481850A (en) * | 2020-05-22 | 2020-08-04 | 深圳三爱美容科技有限公司 | Mask with traditional Chinese medicine tablet for supplying fresh air |
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