CN111359319B - Nano metal aerogel sterilization filter material, preparation method thereof and protective mask - Google Patents
Nano metal aerogel sterilization filter material, preparation method thereof and protective mask Download PDFInfo
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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
- B01D46/0001—Making filtering elements
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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
- A41D31/30—Antimicrobial, e.g. antibacterial
- A41D31/305—Antimicrobial, e.g. antibacterial using layered materials
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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
- B01D46/0028—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions provided with antibacterial or antifungal means
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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
- B01D46/0032—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions using electrostatic forces to remove particles, e.g. electret filters
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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
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
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Abstract
The invention provides a nano metal aerogel sterilization filter material, a preparation method thereof and a protective mask, wherein the nano metal aerogel sterilization filter material comprises a nano metal aerogel layer and a conductive electrode, and the conductive electrode is electrically connected with the nano metal aerogel; the interior of the nano metal aerogel layer comprises a three-dimensional nano network consisting of metal nanowires with a sterilization function. The nano metal aerogel sterilization filter material has the advantages of large specific surface area and strong activity, and a nanowire network in the nano metal aerogel sterilization filter material can directly form a large amount of sterilization metal ions under the action of air and water vapor exhaled by a human body, so that the nano metal aerogel sterilization filter material has excellent sterilization performance; the conductive capability is strong, the power supply can be connected to load a strong electrostatic field or a directional electric field, the adsorption capability and killing effect on micro-nano particles, bacteria and viruses are improved, and the micro-nano particles, bacteria and viruses can be repeatedly utilized; meanwhile, the air purifier has small network gaps and low space density, ensures free circulation of air, slows down blockage of particle pollutants, and prolongs the service life.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a nano metal aerogel sterilization filter material, a preparation method thereof and a protective mask.
Background
With the progress of environmental technology and biotechnology, people gradually recognize the toxic action and threat of dust, fine particulate matters, bacteria, fungi, mold, virus and other atmospheric floating matters and microorganisms to the health, and the public worry about air pollution (such as PM2.5 standard exceeding) and respiratory infectious disease outbreak which occurs at times. The use of air filtering materials and protective masks is an effective method for isolating/preventing pollutants in the air and protecting the health of the user, and a large amount of practical applications are obtained in life at present, and particularly in the prevention and treatment work of novel coronary pneumonia in 2020, the protective masks and related air filtering equipment become important strategic materials for protecting first-line medical care personnel and controlling epidemic propagation.
The existing air filtering material and protective mask in the market are generally of a multilayer structure and mainly comprise a rough filtering surface consisting of non-woven fabrics, gauze or steel meshes, a deodorizing layer consisting of adsorbing materials such as activated carbon and the like, and a filtering core consisting of PP (polypropylene) filter paper, composite PP/PET (polypropylene/polyethylene terephthalate) filter paper, melt-blown glass fibers, melt-blown fiber cloth and the like. The materials have very remarkable effects on isolating fine particulate matters (PM 2.5 and the like) in the air, eliminating peculiar smell and the like, but cannot block the circulation of small-sized pathogens due to large gap size (1-5 microns); meanwhile, bacteria and viruses are isolated by using a fine-gap filtering material or by means of electrostatic adsorption, the mask is easy to block due to accumulation of particles and water vapor, the service life is shortened, the breathing is difficult and the like, and particularly, the mask does not have the bacteria and virus killing capacity, and the continuous use can cause enrichment and even penetration of pathogens in the filtering layer, so that the protection effect is lost, and effective protection can be realized only by frequent replacement. Therefore, the development of an air filtering material and a protective mask with high-efficiency antibacterial and antiviral capabilities and long service life has become a key problem to be solved urgently.
The nano silver is an excellent sterilizing material. Under the action of water molecules in air and human exhaled air, silver oxide on the surface of the nano silver is activated and decomposed to form silver ions, so that the synthesis of cell walls can be effectively interfered, cell membranes can be damaged, the synthesis of proteins can be inhibited, the replication of nucleic acid (DNA, RNA and DNA transcription mRNA) can be interfered, and the silver ions can be dissociated again after pathogens die, so that the processes can be repeatedly completed, and the effects of lasting sterilization and virus resistance can be achieved. And the adsorption and killing of bacteria and viruses can be completed by means of the action of a strong electrostatic field and a directional electric field, so that the antibacterial and antiviral functions are realized, for example, the inactivation of the avian coronavirus under the action of the electric field is confirmed in 2006 by Shanghai traffic university. However, the nanosilver-based filtration and purification materials disclosed in the prior patents tend to have significant limitations. For example, a nano silver layer prepared by directly spraying nano silver particles or nano silver wires and the like is often thin in thickness and sparse in structure, and cannot be guaranteed to be in full contact with pathogens; excessive coating of nano silver and nano silver wires can lead to reduced flexibility of the material and cause dyspnea; the nano-silver composite material prepared by taking the activated carbon, the nano-fiber and the like as the loading matrix is easy to precipitate and fall off in the using process, so that the sterilization function is reduced, the nano-silver composite material can be inhaled by a human body, adverse health effects are generated, and even heavy metal poisoning is caused. On the other hand, since static electricity is difficult to store and the conductivity of the commonly used filter fibers is not good, a high voltage must be applied to obtain a stable electrostatic field or a directional electric field, the required equipment requirement is high and the common users are easily injured, and the method for realizing the antibacterial and antiviral performances by applying the strong electrostatic field and the directional electric field is not widely applied. Therefore, it is necessary to develop a novel filter material or method for realizing a filter material and a protective mask having both antibacterial and antiviral functions and a long service life.
Disclosure of Invention
Aiming at the technical problems, the invention discloses a nano metal aerogel sterilization filter material, a preparation method thereof and a protective mask, which have better filtering and sterilization capabilities and longer service life.
In contrast, the technical scheme adopted by the invention is as follows:
a nano metal aerogel sterilization filter material comprises a nano metal aerogel layer and a conductive electrode, wherein the conductive electrode is electrically connected with the nano metal aerogel;
the interior of the nano metal aerogel layer comprises a three-dimensional nano network consisting of metal nanowires with a sterilization function.
The nano metal aerogel sterilization filter material can be in the form of a filter screen or a filter membrane and the like, and can be used for air filtration sterilization.
In the technical scheme, the three-dimensional nanowire network is a necessary condition for ensuring gas circulation and isolating micro/nano-sized particles, and an electrostatic field or a directional electric field can be formed in the filter screen under the action of a low-voltage power supply by utilizing the high conductivity and the conductive electrode of the nano metal aerogel, so that the adsorption capacity and the antibacterial and antiviral capacities are improved.
By adopting the technical scheme, the conductive electrode is connected with the power supply, wherein the metal nanowire with the sterilization function has the sterilization effect, and simultaneously loads an electrostatic field or a directional electric field, so that the adsorption can be further enhanced, and the better sterilization effect is achieved; the technical scheme of the invention gives consideration to the functions of nano metal sterilization and electric field coupling, enhances the sterilization effect, and is not passive filtration in the prior art.
Furthermore, the size of the space between the metal nanowires is 50nm-10 μm, so that the metal nanowires can be fully contacted with pollutants in the air, meanwhile, the proper diameter of the nanowires and the space between the nanowires are necessary conditions for ensuring air permeability, particle blocking capability, full contact with pathogens, avoiding gap blockage and prolonging service life, and the sufficient sterilization is also ensured while ensuring air circulation, namely air permeability.
As a further improvement of the invention, the diameter of the metal nanowire is 20-1000 nm.
As a further improvement of the invention, the surface of the nano metal aerogel layer is provided with a supporting layer and a moisture absorption layer.
As a further improvement of the invention, the thickness of the nano metal aerogel layer is 0.1-10 mm.
As a further improvement of the present invention, the metal nanowires include at least one of Ag, Cu @ Ag (silver clad copper core-shell structure) metal nanowires or other metal nanowires.
As a further improvement of the present invention, the interior or surface of the nano metal aerogel layer may be filled with nano metal particles, activated carbon, carbon nanotubes, or graphene. Furthermore, the crosslinking degree and the structural stability can be improved by means of treatment methods such as hot pressing, electrification, irradiation and the like. By adopting the technical scheme, the adsorption, filtration, antibacterial and antiviral capabilities of the nano metal aerogel can be further improved, and the electric field load and the cleaning resistance capability are improved.
As a further improvement of the invention, the conductive electrode is a built-in wire, a conductive sheet or a metal columnar electrode connected with the nano metal aerogel. Further, the metal columnar electrode penetrates through the nano metal aerogel.
The invention also discloses a preparation method of the nano metal aerogel sterilizing and filtering material, which comprises the following steps:
step S1, preparing nano metal aerogel;
step S2, cleaning and surface treating the nano metal gel, drying and cutting the nano metal gel into a nano metal aerogel film;
and step S3, adopting non-woven fabrics or absorbent cotton gauze as an upper surface layer and a lower surface layer, and attaching and fixing the non-woven fabrics or the absorbent cotton gauze with the nano metal aerogel film and the conductive electrode obtained in the step S2 to obtain the nano metal aerogel sterilizing and filtering material.
As a further improvement of the present invention, the nano metal aerogel in step S1 is prepared by the following steps:
step S11, adding an active material matrix into a solvent for mixing to obtain a three-dimensional growth active agent;
step S12, melting the needed metal precursor and surfactant into solvent, adding the three-dimensional growth activator obtained in step S1, mixing uniformly, and putting into a closed reaction mold for chemical reduction reaction;
step S13, heating the reaction mould of step S12, and continuously reacting to obtain a nano metal gel structure which has the same shape with the mould and contains a solvent inside;
and S14, taking out the nano metal gel tissue obtained in the step S13, cleaning to remove residual solvent, free nanowire monomer and active agent, and drying to finally obtain the nano metal aerogel with a three-dimensional structure.
According to the technical scheme, the growth mode of the nanowire can be adjusted through the three-dimensional growth active agent, so that a nanowire metal network with a three-dimensional cross-linked structure is formed, and the nanowire metal network is a necessary condition for preparing the pure metal aerogel. The active material matrix may be dissolved in a solvent or may be formed into a suspension.
By adopting the technical scheme, the nano metal aerogel is directly prepared by a chemical synthesis, cleaning and drying method without the steps of dispersing, suspending, freezing or high-energy photocuring and the like, is completely different from the existing aerogel forming principle, and has the advantages of simple preparation process, convenient processing and lower manufacturing cost.
In addition, in material performance, because the nano metal nano wire is directly prepared by using a chemical synthesis method, compared with the aerogel prepared by a suspension and freezing method in the prior art, the nano metal nano wire has higher space density, smaller pore diameter and difficult agglomeration, so the nano metal nano wire has better uniformity, conductivity and filterability, can ensure the full contact with bacteria, viruses and the like, and simultaneously has better deformability and strain recovery characteristics because the inside is an interlaced nano silver wire structure, has better usability and is difficult to directly collapse into a compact film due to the action of external force.
As a further improvement of the present invention, in step S11, the active material matrix is one or a mixture of more of a polymer material such as lignin, cellulose, amino acid, paraffin, and a decomposition product of the above material.
As a further improvement of the present invention, the solvent in the three-dimensional growth activator is the same as the solvent used in the reaction in step S2, so that the growth of the nanowires is not affected. Further, the solvent is an organic solvent such as acetone, ethanol or polyhydric alcohol.
As a further improvement of the invention, the mass ratio of the solvent in the three-dimensional growth active agent is not less than 70%. By adopting the technical scheme, the agglomeration of active substances and the formation of nanowire agglomerates and holes in the growth process of the aerogel can be effectively avoided.
As a further improvement of the present invention, in step S11, the active material matrix is washed and activated and then added to the solvent.
As a further improvement of the present invention, in step S11, the mixing is performed by heating, stirring, ball milling, or the like.
As a further improvement of the present invention, in step S11, the active material matrix is washed and activated and then added to a solvent for dissolution. The dissolution is dissolution or dispersion by means of heating, stirring, ball milling, or the like.
As a further improvement of the present invention, in step S12, the metal precursor is a corresponding salt or organic compound required for preparing metal nanowires of Ag, Cu, Ni, or Au, and the surfactant is a corresponding common surfactant such as PVP, hydrazine hydrate, or glucose.
Further, the mixing mode is electromagnetic or mechanical stirring, and the stirring speed is 100-400 rpm, so as to ensure the stability of nucleation and inhibit the overgrowth of crystal nuclei.
Further, the closed reaction mold is a mold with an internal cavity made of polytetrafluoroethylene, stainless steel or other materials which do not react with the solvent physically and chemically.
As a further improvement of the invention, the depth of the inner cavity of the closed reaction mould<50 mm. This is because the growth of aerogels and nanowires is often influenced by the oxidation process, and even with deeper cavities, larger size aerogels cannot be obtained, only when other oxidants such as H are added2O2、O3、Fe3+When the reactivity is improved, a deeper cavity can be used.
Further, the metal gel structure obtained in step S13 is a jelly-like block, and the internal structure thereof is a continuous network structure of mutually cross-linked foam nanowires.
As a further improvement of the present invention, in step S14, the cleaning is performed by soaking and continuous solvent replacement. Furthermore, in the replacement process, the solvent completely submerges the metal aerogel tissue, deionized water-acetone/ethanol-deionized water or a single solvent is sequentially used in the replacement process, the replacement speed of the solvent is 1-50 ml/min, and the replacement time is 0.5-24 h. The solvent replacement speed is too fast, the damage of the gel structure is easy to cause, the cleaning of the interior of the gel cannot be realized if the replacement speed is too slow, and 0.5h is the shortest replacement time required for ensuring the cleaning effect under the condition of high replacement speed.
As a further improvement of the present invention, in step S14, supercritical drying or ultralow temperature N is adopted2Drying is carried out in a freezing and vacuum freeze drying mode. The pure metal aerogel obtained by adopting the technical scheme of the invention has a three-dimensional structure and is a foam-shaped flexible block material completely formed by crosslinking nano wires. The drying method can avoid collapse or damage of the aerogel network structure caused by the surface tension of the liquid.
The reaction, cleaning and drying method has simple process flow and low requirements on environment and equipment, can ensure that the three-dimensional growth process of the nanowire is performed quickly and fully to form a gel tissue, can effectively remove incompletely-reacted precursors, surfactants, organic solvents and the like, and can avoid collapse or damage of the aerogel structure due to the action of liquid surface tension in the drying process.
The invention also discloses a nano metal aerogel sterilization protective mask which comprises the nano metal aerogel sterilization filter material, an upper support base fabric, a lower support base fabric, a fixing component and a power supply module, wherein the upper surface and the lower surface of the nano metal aerogel sterilization filter material are respectively connected with the upper support base fabric and the lower support base fabric, two sides of the nano metal aerogel sterilization filter material are connected with the fixing component, and the power supply module is electrically connected with the conductive electrode. By adopting the technical scheme, the portability and the usability of the protective mask can be ensured, and the electrostatic field or the directional electric field can be conveniently applied.
As a further development of the invention, the fastening means is a tightening strap, a metal bracket or a mask shell.
As a further improvement of the present invention, the power supply module is a battery. Furthermore, the power supply module is a button cell, a thin film battery, a flexible battery or other small power supplies.
As a further improvement of the invention, the power supply module is integrated on the surface of the mask or a fixing component.
As a further improvement of the invention, the upper supporting base fabric and the lower supporting base fabric are single-layer or multi-layer non-woven fabrics or absorbent cotton gauze. Furthermore, the surface of the upper support base cloth or the lower support base cloth is provided with an activated carbon deodorization layer or a melt-blown filter layer and the like. Further, the mask body or the fixing member may be provided with an active air supply and exhaust device, such as a breather valve. By adopting the technical scheme, the adsorption, filtration and deodorization capabilities of the protective mask can be further enhanced, and the active air supply and exhaust device can further enhance the air circulation and ensure smooth breathing.
The nano metal aerogel sterilization protective mask is prepared by the following steps: the nanometer metal aerogel sterilization filter material is sewn/attached to the upper support base cloth and the lower support base cloth, then the two sides of the nanometer metal aerogel sterilization filter material are fixed to the fixing component, the power supply module is connected with the conductive electrode, and the nanometer metal aerogel sterilization protective mask is obtained.
The nanometer metal aerogel sterilization filter material and the nanometer metal aerogel sterilization protective mask have the advantages of simple manufacturing process flow, low requirements on environment and equipment, controllable structure of the nanometer metal aerogel, and capability of directly processing to obtain the filter unit with a specific size and a specific space density, so that the filter screen and the protective mask can be quickly manufactured in a mounting manner; meanwhile, the obtained nano metal aerogel in the filter screen and the protective mask has the characteristics of low density, small network gap, good structure and environment stability and the like, and has the characteristics of excellent electric field loading capacity, sterilization and antivirus capacity and the like, and has obvious application advantages.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the nano metal aerogel sterilization filter material adopting the technical scheme of the invention has large specific surface area and strong activity, and the dense nanowire network in the nano metal aerogel sterilization filter material can directly form a large amount of silver ions under the action of air and water vapor exhaled by human body, thereby realizing excellent sterilization and antivirus performance; the conductive capability is good, a power supply can be switched on to load a strong electrostatic field or a directional electric field, and the adsorption capability and killing effect on micro-nano particles, bacteria and viruses are further improved; the temperature adaptability is strong, the structural stability is good, the deformation requirement of daily use can be met, and ultrasonic cleaning can be carried out under different environmental conditions so as to kill residual pathogens, remove adsorbed or blocked pollutants and realize recycling; meanwhile, the network gap is small but the space density is low, so that more paths can be provided, the free circulation of air is ensured, the blockage of particle pollutants is relieved, and the service life is prolonged.
Second, the existing silver nanowires or nanoparticles cannot directly form a three-dimensional network structure by coating or sintering, and tend to be heavy and exhibit significant rigidity or brittleness when having a large thickness, and are easily broken or dropped. The nano metal aerogel sterilization filter material has a three-dimensional nanowire network structure, and when the thickness is thicker (the nano metal aerogel sterilization filter material has the three-dimensional nanowire network structure)>30 mm) still has a very low density of (<10 mg/cm3) Excellent flexibility and good structural stability and processability, can withstand ultrasound, vibration and large amplitudes (strain rate)>70 percent) of plastic deformation, can be rapidly cut in batches, is not easy to disperse and fall off, and has obvious material performance and processing advantages.
Thirdly, the technical scheme of the invention is based on three-dimensional growth and spontaneous crosslinking of the nanowire material, the sterilization and filtration unit with any shape, size, thickness and spatial density can be obtained only by adjusting the structure of the die and simply cleaning and drying, secondary processing can be carried out by means of a cutting process, the preparation process is simple, the cost and requirements of materials and equipment are low, and large-scale industrial production can be realized.
Drawings
FIG. 1 is a typical macro-morphology and microstructure of the nano-metallic aerogel of the present invention; wherein (a) is an appearance map of the cut nano metal aerogel block and the cut nano metal aerogel film, and (b) is a microstructure map of the nano metal aerogel.
Fig. 2 is a schematic structural diagram of a nano silver wire aerogel sterilization filter screen obtained in embodiment 1 of the present invention.
Fig. 3 is a schematic structural diagram of a nano copper wire aerogel bactericidal protective mask obtained in embodiment 2 of the present invention; wherein (a) is the front view of the protective mask, and (b) is the side view of the protective mask.
The reference numerals include: 1-silver nanowire aerogel film, 2-moisture absorption layer, 3-non-woven fabrics, 4-copper post electrode, 5-copper nanowire aerogel film, 6-copper sheet electrode, 7-absorbent cotton gauze, 8-copper nanowire aerogel sterilization filter screen, 9-active carbon deodorization layer, 10-non-woven fabrics, 11-tightening belt, 12-metal support, 13-button cell.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
Example 1
A nano silver wire aerogel sterilization filter screen is prepared by the following steps:
(1) the hydrolysis product (2 g) of lignin and cellulose is used as a three-dimensional growth active agent, PVP (3.5g) is used as a surfactant and a reducing agent, silver nitrate (3 g) is used as a precursor, ethylene glycol (100 ml) is used as a solvent, a 304 stainless steel reaction kettle is used as a container, liquid phase reduction reaction is induced under the condition of 140 ℃, and the nano silver wire gel structure is prepared, wherein the whole thickness is 30 mm, the diameter of a nano wire is 20 nm, and the average size of gaps among the nano wires is about 100 nm.
(2) Washing the obtained nano silver wire gel tissue with sodium chloride solution (1M), removing residual reaction reagent and free nano wire monomer in the nano silver wire gel tissue, and passing through CO2And obtaining the nano silver wire aerogel by using a supercritical drying technology, and cutting by using a low-power laser to obtain the nano silver wire aerogel film with the thickness of 0.1 mm. Wherein, the macroscopic morphology and the microstructure of the nano silver wire aerogel are shown in figure 1.
(3) The absorbent cotton gauze is selected as the moisture absorption layer 2, the non-woven fabric 3 is selected as the supporting layer to prepare the upper supporting surface and the lower supporting surface, the upper supporting surface and the lower supporting surface are attached to the nano silver wire aerogel film 1, and then 4-6 copper column electrodes 4 penetrate through the whole structure to be fixed, so that the nano metal aerogel sterilization filter screen is obtained, as shown in figure 2.
The nano silver wire aerogel sterilization filter screen obtained in the embodiment has extremely small gap size and strong conductivity, has a remarkable physical barrier effect on micro-nano particle pollutants, bacteria, mold, viruses and other pollutants in the air, and can release a large amount of silver ions to actively kill pathogens; after an external power supply is switched on, an electrostatic field or a directional electric field can be loaded, so that the adsorption effect on pollutants and the killing effect on pathogens are enhanced, and the filter has very high filtering efficiency; on the other hand, the nanowire network in the filter screen has lower space density, strong air circulation capacity, difficult complete blockage and long service life, and can be recycled by means of methods such as high-temperature sterilization, ultrasonic cleaning and the like, so that the filter screen material has obvious application and performance advantages compared with the existing filter screen material.
Example 2
A nano copper wire aerogel sterilization protective mask comprises the following preparation methods:
(1) the preparation method comprises the steps of taking partial hydrolysate (1.5 g) of glutamic acid and alanine as a three-dimensional growth activator, copper nitrate (0.1mol/L, 10 ml) as a precursor, hydrazine hydrate (35 wt.%, 0.25 ml) as a reducing agent and ethylenediamine (1.5 ml) as a surfactant, adding the mixture into sodium hydroxide (15 mol/L, 200 ml) solution, and inducing liquid-phase reduction reaction in a polytetrafluoroethylene reaction tank at 175 ℃ to prepare the nano copper wire gel structure, wherein the whole thickness of the nano copper wire gel structure is 25 mm, the diameter of a nano wire is 250 nm, and the average size of gaps among the nano wires is about 2 microns.
(2) Sodium citrate (2.5 g) is used as a surfactant and a reducing agent, silver nitrate (3 g) is used as a precursor, ethylene glycol (100 ml) is used as a solvent, a glass reaction kettle is used for preparing nano silver particles at 160 ℃, a reaction reagent is mechanically stirred in the liquid phase reduction process, the rotating speed is 150 rpm, and the reaction time is 3.5 hours.
(3) Washing the obtained nano copper wire gel tissue and nano silver particles by using ethanol and a sodium sulfate solution (1M), and placing the nano copper wire gel tissue and the nano silver particles in deionized water to form nano copper wire hydrogel and nano silver suspension; uniformly mixing the two, filling the nano-silver particles in gaps among the nano-copper wire networks by a solvent replacement method, and combining a freeze drying technology to obtain the nano-copper wire aerogel with the nano-silver particles on the surface; and then, heating at 100 ℃ for 30 minutes to promote the sintering of the nano silver particles on the copper wire network, and cutting by using a low-voltage electron beam to obtain a nano copper wire aerogel film with the thickness of 2 mm.
(4) Placing the nano copper wire aerogel film 5 and the copper sheet electrode 6 between two layers of absorbent cotton gauze 7, and attaching and fixing to obtain a nano copper wire aerogel sterilization filter screen 8, as shown in fig. 3;
(5) the obtained nano copper wire aerogel sterilization filter screen 8 and the active carbon deodorization layer 9 are attached between two layers of non-woven fabrics 10 or other skin-friendly fabrics, a tightening belt 11 and a metal support 12 are installed by sewing and bonding, and a copper sheet electrode 6 in the filter screen is connected with a button cell 13 interface preset on the metal support, so that the nano copper wire aerogel sterilization protective mask with the active adsorption sterilization function is formed, as shown in fig. 3.
The nano copper wire aerogel sterilization protective mask obtained in the embodiment has weak physical barrier capability, and active adsorption and sterilization of pathogens such as bacteria and viruses are realized mainly by means of nano silver particles on a nano copper wire network and a loaded electrostatic field. Compared with the nano silver wire aerogel sterilization filter screen obtained in the embodiment 1, the protective mask uses a thicker copper wire network with larger space between wires as a sterilization filter unit. Because copper is easy to oxidize compared with silver in sterilization and antivirus performance, the air filtering capacity, the antibacterial and antivirus capacity and the service life of the protective mask are reduced, but the protective mask has strong air circulation capacity, low preparation cost and convenient use, thereby being suitable for daily protection work with lower requirements on antibacterial and antivirus.
Comparative example 1
The utility model provides a protective facial mask that contains nanometer silver and chitosan comprises the cover body and frenulum, its characterized in that, the cover body comprises 5 layers of gauze material: the first layer is a cotton wool layer, the second layer and the third layer are gauze functional layers containing nano silver and chitosan, the fourth layer is a cotton wool layer, and the fifth layer is a non-woven fabric layer, wherein the particle size of the nano silver is 2-80 nm, the thickness of the functional layer material is 0.2-2mm, and the porosity is more than 80%.
Under the process conditions of the embodiment, the nano silver particles are difficult to uniformly coat, and are easy to react with hydrogen sulfide, sulfur dioxide and the like in the air to form Ag due to small size2S, thereby losing the sterilization ability; meanwhile, the nano silver particles are easy to fall off from the fibers, so that the nano silver particles enter a human body along with airflow and generate toxic action. In summary, the embodiments 1 to 2 have significant performance and safety advantages over the comparative example.
Comparative example 2
A kind of nanometer silver wire airstrainer, including upper and lower two-layer supporting network, the intermediate layer is the filtration membrane of nanometer silver wire, and the nanometer silver wire is glued with the nanometer silver particle, its preparation method includes the following steps:
1) growing a nano silver wire by a chemical method, adding nano silver particles, and mixing the nano silver particles with a special coating liquid to prepare nano silver wire ink;
2) printing or coating nano silver ink on a supporting net;
3) carrying out heat treatment on the nano silver wire filtering membrane by adopting an oven at about 200 ℃ or strong light irradiation;
4) after thermosetting to form a film, a multi-layer net-shaped woven three-dimensional structure is formed.
5) And (4) attaching and fixing the upper and lower supporting nets to form the nano silver wire air filter screen.
Under the process condition of the embodiment, the nano silver wires and the nano particle ink are sintered into a multi-layer network woven three-dimensional structure in a multi-printing and high-temperature sintering mode. However, the process of this embodiment is complex, and multiple printing and curing are required after nanowire synthesis to form the filter membrane; the nano-wire ink is generally high in viscosity, the thickness and the air circulation capacity after printing are difficult to control, and when the viscosity is reduced, the concentration of the nano-silver wire needs to be reduced, so that the size of a gap is increased easily, and the sufficient contact between the nano-silver and a pathogen cannot be ensured; nanowires and nanoparticles in the ink are prone to agglomeration during printing, so that protective "gaps" appear; the plane sintered body is easily obtained by a multilayer printing and sintering method, and a three-dimensional structure is difficult to form, so that the rigidity and the brittleness of the obtained printing structure are higher, the damage or the fracture is easy to occur, and the antibacterial and antiviral capabilities are lost; meanwhile, because the support cloth has extremely poor conductivity, the air filter screen cannot be loaded with an electrostatic field or a directional electric field, and stronger adsorption, antibacterial and antiviral capabilities are realized. In summary, the present invention has significant process and performance advantages over this embodiment.
Comparative example 3
A nano silver wire aerogel sterilization filter screen is prepared by the following steps:
(1) taking hydrolysate (2 g) of lignin and cellulose as a three-dimensional growth active agent, PVP (4g) as a surfactant and a reducing agent, silver nitrate (3.5g) as a precursor, ethylene glycol (200 ml) as a solvent and a 304 stainless steel reaction kettle as a container, inducing a liquid phase reduction reaction at 140 ℃ to prepare the nano silver wire gel structure, wherein the whole thickness of the nano silver wire gel structure is 60 mm, the diameter of the nano wire is 50nm, and the average size of gaps among the nano wires is about 350 nm.
(2) Washing the obtained nano silver wire gel tissue with sodium sulfate solution (1M), removing residual reaction reagent and free nano wire monomer in the nano silver wire gel tissue, and passing through CO2And obtaining the nano silver wire aerogel by using a supercritical drying technology, and cutting by using a low-power laser to obtain the nano silver wire aerogel film with the thickness of 5 mm.
(3) The nano metal aerogel sterilization filter screen is obtained by adopting the step (3) of the embodiment 1.
This example uses more solvent and higher surfactant concentration, the void size of the resulting silver nanowire aerogel network is larger, and although the air flow is better, because of insufficient contact with viruses or bacteria in the air, a thicker film must be used to ensure a certain bactericidal effect, and the cost is higher instead.
Comparative example 4
A nano silver wire aerogel sterilization filter screen is prepared by the following steps:
(1) the hydrolysis product (4g) of lignin and cellulose is used as a three-dimensional growth active agent, PVP (3.5g) is used as a surfactant and a reducing agent, silver nitrate (4g) is used as a precursor, ethylene glycol (70 ml) is used as a solvent, a 304 stainless steel reaction kettle is used as a container, liquid phase reduction reaction is induced under the condition of 165 ℃, and the nano silver wire gel structure is prepared, wherein the whole thickness is 20 mm, the diameter of a nano wire is 30 nm, and the average size of gaps among the nano wires is only about 50 nm.
(2) Washing the obtained nano silver wire gel tissue with a mixed solution of sodium chloride (1M) and sodium bromide (1M), removing residual reaction reagent and free nanowire monomer in the nano silver wire gel tissue, and passing through CO2And obtaining the nano silver wire aerogel by using a supercritical drying technology, and cutting by using a low-power laser to obtain the nano silver wire aerogel film with the thickness of 0.03 mm.
(3) The nano silver wire aerogel sterilization filter screen is obtained by adopting the step (3) of the embodiment 1.
The comparative example uses more three-dimensional growth active agents and precursors, so that the diameter of the obtained silver nanowire is larger, the space interweaving effect is stronger, the size of a gap is smaller, the aerogel material can ensure full sterilization under the condition of not loading an electrostatic field, but the air circulation is not smooth due to too small gaps, and the normal use cannot be ensured even if the thickness is reduced.
Comparative example 5
A nano silver wire aerogel sterilization filter screen is prepared by the following steps:
(1) the hydrolysis product (2 g) of lignin and cellulose is used as a three-dimensional growth active agent, PVP (3.5g) is used as a surfactant and a reducing agent, silver nitrate (3 g) is used as a precursor, ethylene glycol (100 ml) is used as a solvent, a 304 stainless steel reaction kettle is used as a container, liquid phase reduction reaction is induced under the condition of 165 ℃, and the nano silver wire gel structure is prepared, wherein the whole thickness is 30 mm, the diameter of a nano wire is 30 nm, and the average size of gaps among the nano wires is about 150 nm.
(2) By CO2And obtaining the nano silver wire aerogel by using a supercritical drying technology, and cutting by using a low-power laser to obtain the nano silver wire aerogel film with the thickness of 0.1 mm.
(3) The nano silver wire aerogel sterilization filter screen is obtained by adopting the step (3) of the embodiment 1.
The nano silver wire aerogel obtained in the embodiment has a large amount of residual PVP coating layers on the surface, the contact resistance between the nano silver wires is extremely large, so the electric conductivity is poor, only 150-300S/m is provided, due to the partial pressure and power consumption of the PVP layer, the button battery is high in consumption speed, due sterilization and adsorption effects can be obtained only by increasing the voltage to 15-30V, the using effect is poor, skin damage is easy to cause, and therefore the embodiment is not practical.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (9)
1. A nano metal aerogel sterilization and filtration material is characterized in that: the nano-metal aerogel layer is electrically connected with the conductive electrode; the interior of the nano metal aerogel layer comprises a three-dimensional nano network consisting of metal nanowires with a sterilization function;
the nano metal aerogel is prepared by the following steps:
step S11, adding an active material matrix into a solvent for mixing to obtain a three-dimensional growth active agent;
step S12, melting the needed metal precursor and surfactant into solvent, adding the three-dimensional growth activator obtained in step S11, mixing uniformly, and putting into a closed reaction mold for chemical reduction reaction;
step S13, heating the reaction mould of step S12, and continuously reacting to obtain a nano metal gel structure which has the same shape with the mould and contains a solvent inside;
step S14, taking out the nano metal gel tissue obtained in the step S13, cleaning to remove residual solvent, free nanowire monomer and active agent, and drying to finally obtain the nano metal aerogel with a three-dimensional structure;
in step S11, the active material matrix is one or a mixture of lignin, cellulose, amino acids, paraffin materials, and decomposition products of the foregoing materials.
2. The nano-metallic aerogel sterilizing filter material as claimed in claim 1, wherein: the size of the space between the metal nanowires is 50nm-10 mu m, and the diameter of the metal nanowires is 20-1000 nm.
3. The nano-metallic aerogel sterilizing filter material as claimed in claim 2, wherein: the surface of the nano metal aerogel layer is provided with a supporting layer and a moisture absorption layer; the thickness of the nano metal aerogel layer is 0.1-10 mm.
4. The nano-metallic aerogel sterilizing filter material as claimed in claim 2, wherein: the metal nanowires comprise at least one of Ag, Cu and Cu @ Ag metal nanowires.
5. The nano-metal aerogel sterilizing and filtering material as claimed in any one of claims 1 to 4, wherein: the interior or the surface of the nano metal aerogel layer is filled with nano metal particles, activated carbon, carbon nano tubes or graphene.
6. The nano-metallic aerogel sterilizing filter material of claim 5, wherein: the conductive electrode is a built-in wire, a conductive sheet or a metal columnar electrode connected with the nano metal aerogel.
7. The method for preparing nano-metal aerogel sterilizing and filtering material as claimed in any one of claims 1 to 6, wherein the method comprises the following steps: which comprises the following steps:
step S1, preparing nano metal aerogel;
step S2, cleaning and surface treating the nano metal gel, drying and cutting the nano metal gel into a nano metal aerogel film;
and step S3, adopting non-woven fabrics or absorbent cotton gauze as an upper surface layer and a lower surface layer, and attaching and fixing the non-woven fabrics or the absorbent cotton gauze with the nano metal aerogel film and the conductive electrode obtained in the step S2 to obtain the nano metal aerogel sterilizing and filtering material.
8. The method for preparing nano-metallic aerogel sterilizing filter material according to claim 7, wherein the method comprises the following steps:
the mass ratio of the solvent in the three-dimensional growth activator is not less than 70 percent; the solvent is acetone, ethanol or polyalcohol; in step S11, the active material matrix is washed and activated and then added to a solvent;
in step S12, the metal precursor and the surfactant are corresponding reaction reagents required for preparing Ag or Cu nanowires;
in step S14, the cleaning is performed by soaking and continuous solvent replacement; in the replacement process, the solvent completely submerges the metal aerogel tissue, deionized water-acetone or ethanol-deionized water or a single solvent is used in the replacement process in sequence, the replacement speed of the solvent is 1-50 ml/min, and the replacement time is 0.5-24 h.
9. A protective mask is characterized in that: the nano metal aerogel sterilization filter material comprises the nano metal aerogel sterilization filter material, an upper support base fabric, a lower support base fabric, a fixing component and a power supply module, wherein the upper surface and the lower surface of the nano metal aerogel sterilization filter material are respectively connected with the upper support base fabric and the lower support base fabric, two sides of the nano metal aerogel sterilization filter material are connected with the fixing component, and the power supply module is electrically connected with a conductive electrode.
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| TW202216936A (en) * | 2020-10-27 | 2022-05-01 | 梁詠淇 | Filter pad |
| KR102301735B1 (en) * | 2020-12-07 | 2021-09-13 | (주)신화케이엔엘 | Sterilization mask |
| CN113802371A (en) * | 2021-09-01 | 2021-12-17 | 深圳清华大学研究院 | Antibacterial and antiviral non-woven fabric and preparation method and application thereof |
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