CN111359317A - Nano-photocatalyst antibacterial filter layer and protection device - Google Patents
Nano-photocatalyst antibacterial filter layer and protection device Download PDFInfo
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- CN111359317A CN111359317A CN202010208930.1A CN202010208930A CN111359317A CN 111359317 A CN111359317 A CN 111359317A CN 202010208930 A CN202010208930 A CN 202010208930A CN 111359317 A CN111359317 A CN 111359317A
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- filter layer
- photocatalyst
- antibacterial filter
- silicon dioxide
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 71
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 82
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 23
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 230000001681 protective effect Effects 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 239000000377 silicon dioxide Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 23
- 239000003822 epoxy resin Substances 0.000 claims description 16
- 229920000647 polyepoxide Polymers 0.000 claims description 16
- 239000011550 stock solution Substances 0.000 claims description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- 238000004132 cross linking Methods 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 230000002209 hydrophobic effect Effects 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- 238000004381 surface treatment Methods 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 10
- 239000011248 coating agent Substances 0.000 abstract description 9
- 239000003344 environmental pollutant Substances 0.000 abstract description 8
- 231100000719 pollutant Toxicity 0.000 abstract description 8
- 244000005700 microbiome Species 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 231100001240 inorganic pollutant Toxicity 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 39
- 239000004745 nonwoven fabric Substances 0.000 description 30
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 17
- 239000000203 mixture Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 9
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 8
- 230000000903 blocking effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 6
- FZMJEGJVKFTGMU-UHFFFAOYSA-N triethoxy(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC FZMJEGJVKFTGMU-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 230000001954 sterilising effect Effects 0.000 description 5
- 238000004659 sterilization and disinfection Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 241000700605 Viruses Species 0.000 description 3
- 230000010065 bacterial adhesion Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000003373 anti-fouling effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- A41D13/1192—Protective face masks, e.g. for surgical use, or for use in foul atmospheres with antimicrobial agent
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/30—Antimicrobial, e.g. antibacterial
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L9/00—Disinfection, sterilisation or deodorisation of air
- A61L9/16—Disinfection, sterilisation or deodorisation of air using physical phenomena
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0272—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255
- B01J31/0274—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255 containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0272—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255
- B01J31/0275—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing elements other than those covered by B01J31/0201 - B01J31/0255 also containing elements or functional groups covered by B01J31/0201 - B01J31/0269
-
- B01J35/23—
-
- B01J35/39—
Abstract
The invention provides a nano photocatalyst antibacterial filter layer for a protective device and the protective device comprising the nano photocatalyst antibacterial filter layer. The nano photocatalyst antibacterial filter layer is formed by coating a treatment liquid comprising nano photocatalyst particles and hydrophobically modified nano silicon dioxide on a non-woven material. The nano photocatalyst antibacterial filter layer enables the protective device to effectively prevent inorganic pollutants and organic microorganisms in the air from adhering, effectively blocks external harmful substances and can sterilize the adhered pollutants.
Description
Technical Field
The invention relates to a nano photocatalyst antibacterial filter layer for a protective device, in particular to a nano photocatalyst antibacterial filter layer containing nano photocatalyst particles and hydrophobic modified nano silicon dioxide and a protective device comprising the nano photocatalyst antibacterial filter layer.
Background
With the rapid development of industrial society, the environmental pollution is becoming more serious, and the atmospheric pollutants mainly comprise harmful gases and particulate matters. Wherein, the particulate matter not only can be inhaled respiratory, and then cause respiratory disease, but also because its surface has adsorbed a large amount of organic pollutant, poisonous heavy metal, bacterium and virus etc. and is more harmful to human health.
The mask is a conventional protection device for adsorbing and blocking fine particles. The general mask is made of non-woven fabrics, the blocking principle is mechanical filtration, and when particles collide with the non-woven fabrics, the particles are blocked layer by layer.
However, after the conventional non-woven fabric mask is worn for a long time, viruses, germs and the like are easily accumulated on the outer surface of the non-woven fabric of the mask, the mask is taken off after being used for two to four hours, and is cleaned, disinfected or discarded in time, otherwise, the function of effective blocking is lost.
Disclosure of Invention
The invention aims to provide a nano photocatalyst antibacterial filter layer, which improves the blocking effect by using nano photocatalyst particles and hydrophobically modified nano silicon dioxide, effectively prevents pollutants and microorganisms in the air from adhering to a mask and has a sterilization effect on the adhered pollutants.
According to one aspect of the present invention, there is provided a nano-photocatalyst antibacterial filter layer for a protective device, comprising nano-photocatalyst particles and hydrophobically modified nano-silica.
Wherein the nano photocatalyst particles are nano titanium dioxide. Preferably, the average particle size of the nano photocatalyst particles is 10-30 nm.
Preferably, the weight ratio of the nano-photocatalyst particles to the nano-silica before hydrophobic modification is 1: 3.
The surface of the hydrophobically modified nano silicon dioxide contains long-chain alkyl.
Preferably, the preparation method of the treatment fluid for forming the nano photocatalyst antibacterial filter layer comprises the following steps:
carrying out surface treatment on the nano silicon dioxide by adopting one or more silane coupling agents containing C14-C18 long-chain alkyl;
under the action of an amine catalyst, a cross-linking agent and the nano-silicon dioxide subjected to surface treatment are subjected to cross-linking reaction to prepare nano-silicon dioxide mixed solution;
adding the nano photocatalyst particles into the nano silicon dioxide mixed solution, and uniformly stirring to obtain a nano photocatalyst stock solution.
Preferably, the weight ratio of the silane coupling agent to the nano silicon dioxide is 0.2-0.33: 1.
Specifically, the amine catalyst is ammonia; the cross-linking agent is epoxy resin; the crosslinking reaction temperature is 15-25 ℃.
The epoxy value of the epoxy resin is 0.41-0.54, and the viscosity is 10-40 Pa.s.
According to another aspect of the invention, a protective device is provided, which comprises an inner nonwoven fabric layer, an outer nonwoven fabric layer and a middle nonwoven fabric layer positioned between the inner nonwoven fabric layer and the outer nonwoven fabric layer, wherein the middle nonwoven fabric layer is provided with the nano-photocatalyst antibacterial filter layer.
Preferably, the protective device is a mask.
The nano photocatalyst antibacterial filter layer can replace a filter layer in a common protective device, has a strong blocking effect, can improve the antibacterial, antifouling and staining-resistant properties of the protective device, and particularly can remarkably enhance the sterilization effect on adhered pollutants.
Detailed Description
The nano photocatalyst antibacterial filter layer for the protective device is formed by coating photocatalyst treatment liquid comprising nano photocatalyst and hydrophobically modified nano silicon dioxide on a non-woven material.
The nano photocatalyst particles used in the invention are preferably nano titanium dioxide, and the average particle size of the nano titanium dioxide is 10-30 nm. The nano-silica used in the present invention is generally spherical, and the average particle diameter may be 7 to 20nm, preferably 15 nm. The weight ratio of the nano photocatalyst particles to the nano silicon dioxide before hydrophobic modification is 1: 3.
Before use, the nano silicon dioxide needs to be subjected to hydrophobic modification so as to have strong hydrophobicity. Preferably, the hydrophobic modified nano-silica is obtained by modifying a silane coupling agent containing C14-C18 long-chain alkyl with nano-silica spheres, and performing catalytic crosslinking reaction with epoxy resin through hydrolysis of the silane coupling agent.
According to one embodiment, the hydrophobically modified nanosilica is preferably prepared by the following process:
in an organic solvent, adopting one or more silane coupling agents containing C14-C18 long-chain alkyl to carry out surface treatment on the nano silicon dioxide;
under the action of amine catalyst, the cross-linking agent and the nano-silicon dioxide after surface treatment are subjected to cross-linking reaction to prepare nano-silicon dioxide mixed solution.
The nano silica may be dispersed in a solvent before the surface treatment with the silane coupling agent. The organic solvent which can be used in the present invention may be one or more of ethanol, isopropanol, acetone, methyl isobutyl ketone, preferably ethanol, isopropanol, or ethanol and isopropanol in any ratio. The weight percentage of the nano silicon dioxide in the dispersion liquid can be 5-10%, and the preferable weight percentage is 6%.
Wherein the weight ratio of the silane coupling agent to the nano silicon dioxide is 0.2-0.33: 1. Preferably, the silane coupling agent containing C14-C18 long-chain alkyl can be one or two of hexadecyl trimethoxy silane and octadecyl triethoxy silane.
Specifically, the amine catalyst may be ammonia. The crosslinking agent can be epoxy resin, the epoxy value of the epoxy resin is preferably 0.41-0.54, and the viscosity is 10-40 Pa.s. Specifically, the epoxy resin may be E44 or E55 epoxy resin. The weight ratio of the amine catalyst to the epoxy resin is 1: 0.7-1.
The crosslinking reaction temperature is 15-50 ℃, the temperature of the reaction process is controlled by using condensed water, and the stirring speed in the reaction process is within the range of 100-300 rpm.
In the preparation method, the silane coupling agent containing long-chain alkyl is adopted to carry out chemical grafting with the nano-silica spheres, and the long-chain alkyl is grafted on the surfaces of the nano-silica spheres through hydrolysis and catalytic crosslinking reaction of the silane coupling agent, so that the nano-silica spheres have strong hydrophobicity. Meanwhile, a catalyst (preferably an amine-containing small molecule reagent) is used for carrying out progressive catalysis on the reaction, and then a cross-linking agent (epoxy resin) is used for carrying out cross-linking on the silica spheres, so that the nano silica spheres are combined together, the binding force among the particles is enhanced, and the adhesive force on the surface of the base material is improved.
Adding the nano photocatalyst particles into the prepared nano silicon dioxide mixed solution, and uniformly stirring to obtain a nano photocatalyst stock solution.
Diluting the nano photocatalyst stock solution prepared by the method by the solvent, preferably by 5-20 times, to obtain the nano photocatalyst treatment solution.
The nano photocatalyst treatment liquid is sprayed on the surface, preferably the front surface and the back surface, of a non-woven material of a protective device, such as a mask, and is dried at the temperature of about 60 ℃ to form the nano photocatalyst antibacterial filter layer. The spraying method of the present invention can adopt the conventional method in the field, for example, an air compressor is adopted to uniformly spray the treating fluid on the front and back surfaces of the non-woven fabric.
The thickness of the nano photocatalyst antibacterial filter layer is preferably 20-40 microns.
The invention provides a protective device, such as a mask, which comprises an inner nonwoven fabric layer, an outer nonwoven fabric layer and a middle nonwoven fabric layer positioned between the inner nonwoven fabric layer and the outer nonwoven fabric layer, wherein the middle nonwoven fabric layer is provided with the nano photocatalyst antibacterial filter layer.
After the nano photocatalyst antibacterial filter layer is coated on a non-woven fabric substrate and dried, the surface has extremely low surface energy and a micro-nano coarse structure, so that the effects of strong hydrophobicity, bacteria prevention, contamination prevention and contaminant permeation prevention can be achieved.
Therefore, the raw materials of the nano filter layer are harmless to human bodies, the nano filter layer can replace a filter layer of a common mask in function, can effectively block pollutants, bacteria, microorganisms and the like in the air from being infected with the mask while filtering the air, and has a photocatalytic effect, so that the nano filter layer can catalyze and decompose the microorganisms such as bacteria, viruses and the like infected with the nano filter layer, and the sterilization effect is realized.
The nano photocatalyst antibacterial filter layer of the invention is adopted to replace the filter layer in the conventional mask, can obtain stronger blocking effect, is more beneficial to antibiosis, antifouling and contamination prevention, and has sterilization effect.
The technical solutions of the present application will be more clearly illustrated by the following examples.
Examples
Example 1
1. Adding 3g of nano-silica spheres with the average particle size of 7nm into 47g of absolute ethyl alcohol, and stirring at 200rpm at room temperature to uniformly disperse the nano-silica spheres in the ethyl alcohol to prepare a dispersion liquid.
2. 0.35g of hexadecyltrimethoxysilane, 0.35g of octadecyltriethoxysilane and 10g of anhydrous ethanol were thoroughly mixed and stirred uniformly at 100 rpm.
3. The mixed solution prepared in the step 2 is added into the dispersion liquid of the step 1, stirred at the rotating speed of 300rpm at room temperature and reacted for 4 hours.
4. 2g of ammonia water was added and the reaction was continued with stirring for 4 h.
5. 1.5g E44 epoxy resin was added and the reaction was continued for 2h with stirring and the reaction temperature was controlled to 15 ℃ with condensed water.
6. And (3) after the reaction is finished, taking out a product, adding 1g of nano titanium dioxide with the average particle size of 20nm into the product, and fully stirring the mixture at room temperature at a rotating speed of 150rpm to uniformly mix the mixture to prepare the nano photocatalyst stock solution.
7. The above nano photocatalyst stock solution is diluted by absolute ethyl alcohol according to the proportion of 1:20 to prepare nano photocatalyst treatment solution.
8. The above treatment liquid was sprayed on both surfaces of the nonwoven fabric using an air compressor and dried at 60 ℃ in a ventilated atmosphere for at least 2 hours to give a coating thickness of 20 μm.
Example 2
1. 3g of nano silica spheres with the average particle size of 7nm are added into 47g of isopropanol, and the mixture is stirred at 200rpm at room temperature to uniformly disperse the nano silica spheres in ethanol, so that a dispersion liquid is prepared.
2. 0.35g of hexadecyltrimethoxysilane, 0.35g of octadecyltriethoxysilane and 10g of isopropanol were thoroughly mixed and stirred uniformly at 100 rpm.
3. The mixed solution of step 2 was added to the dispersion of step 1, stirred at 300rpm at room temperature and reacted for 4 hours.
4. 2g of ammonia water was added and the reaction was continued with stirring for 4 h.
5. 1.5g E44 epoxy resin was added and the reaction was continued for 2h with stirring and the reaction temperature was controlled to 35 ℃ with condensed water.
6. And (3) after the reaction is finished, taking out a product, adding 1g of nano titanium dioxide with the average particle size of 20nm into the product, and fully stirring the mixture at room temperature at a rotating speed of 150rpm to uniformly mix the mixture to prepare the nano photocatalyst stock solution.
7. The above nano photocatalyst stock solution is diluted by absolute ethyl alcohol according to the proportion of 1:20 to prepare nano photocatalyst treatment solution.
8. The above treatment liquid was sprayed on both surfaces of the nonwoven fabric using an air compressor and dried at 60 ℃ in a ventilated atmosphere for at least 2 hours to give a coating thickness of 40 μm.
Example 3
1. 3g of nano silica spheres having an average particle diameter of 7nm were added to 23.5g of absolute ethanol and 23.5g of isopropyl alcohol, and the mixture was stirred at 200rpm at room temperature to uniformly disperse the nano silica spheres in ethanol, thereby obtaining a dispersion.
2. 0.35g of hexadecyltrimethoxysilane, 0.35g of octadecyltriethoxysilane, 5g of anhydrous ethanol and 5g of isopropanol were thoroughly mixed and stirred uniformly at a rotation speed of 100 rpm.
3. The mixed solution of step 2 was added to the dispersion of step 1, stirred at 300rpm at room temperature and reacted for 4 hours.
4. 2g of ammonia water was added and the reaction was continued with stirring for 4 h.
5. 2g E51 epoxy resin was added and the reaction was continued for 2h with stirring and the reaction temperature was controlled to 50 ℃ with condensed water.
6. And (3) after the reaction is finished, taking out a product, adding 1g of nano titanium dioxide with the average particle size of 20nm into the product, and fully stirring the mixture at room temperature at a rotating speed of 150rpm to uniformly mix the mixture to prepare the nano photocatalyst stock solution.
7. The nanometer photocatalyst stock solution is diluted by the product of absolute ethyl alcohol and isopropanol in the proportion of 1:10:10 to prepare the nanometer photocatalyst treatment solution.
8. The above treatment liquid was sprayed on both surfaces of the nonwoven fabric using an air compressor and dried at 60 ℃ in a ventilated atmosphere for at least 2 hours to give a coating having a thickness of 30 μm.
Example 4
1. 3g of nano silica spheres with the average particle size of 7nm are added into 47g of absolute ethyl alcohol, and the mixture is stirred at 200rpm at room temperature, so that the nano silica spheres are uniformly dispersed in the ethyl alcohol.
2. 0.7g of hexadecyltrimethoxysilane and 10g of absolute ethanol were thoroughly mixed and stirred at 100 rpm.
3. The mixed solution prepared in the step 2 is added into the dispersion liquid of the step 1, stirred at the rotating speed of 300rpm at room temperature and reacted for 4 hours.
4. 3g of ammonia water was added and the reaction was continued with stirring for 4 h.
5. 1.5g E44 epoxy resin was added and the reaction was continued for 2h with stirring and the reaction temperature was controlled to 25 ℃ with condensed water.
6. And (3) after the reaction is finished, taking out a product, adding 1g of nano titanium dioxide with the average particle size of 20nm into the product, and fully stirring the mixture at room temperature at a rotating speed of 150rpm to uniformly mix the mixture to prepare the nano photocatalyst stock solution.
7. The above nano photocatalyst stock solution is diluted by absolute ethyl alcohol according to the proportion of 1:20 to prepare nano photocatalyst treatment solution.
8. The above treatment liquid was sprayed on both surfaces of the nonwoven fabric using an air compressor and dried at 60 ℃ in a ventilated atmosphere for at least 2 hours to give a coating having a thickness of 32 μm.
Example 5
1. 3g of nano silica spheres with the average particle size of 13nm are added into 47g of absolute ethyl alcohol, and the mixture is stirred at 200rpm at room temperature, so that the nano silica spheres are uniformly dispersed in the ethyl alcohol.
2. 0.5g of hexadecyltrimethoxysilane, 0.5g of octadecyltriethoxysilane and 10g of anhydrous ethanol were thoroughly mixed and stirred at 100 rpm.
3. Adding the solution in the step 2 into the mixed solution in the step 1, stirring at the rotating speed of 300rpm, and reacting for 4 hours.
4. 3g of ammonia water was added and the reaction was continued with stirring for 4 h.
5. 2g E51 epoxy resin was added and the reaction was continued for 2h with stirring.
6. After the reaction, the product was taken out, and 1g of nano titanium dioxide having an average particle size of 20nm was added thereto, and sufficiently stirred at a rotation speed of 150rpm at room temperature to be uniformly mixed.
7. The above nano photocatalyst stock solution is diluted by absolute ethyl alcohol according to the proportion of 1:20 to prepare nano photocatalyst treatment solution.
8. The above treatment liquid was sprayed on both surfaces of the nonwoven fabric using an air compressor and dried at 60 ℃ in a ventilated atmosphere for at least 2 hours to give a coating having a thickness of 24 μm.
Example 6
1. 3g of nano silica spheres with the diameter of 7nm are added into 47g of absolute ethyl alcohol, and the mixture is stirred at 200rpm at room temperature, so that the nano silica spheres are uniformly dispersed in the ethyl alcohol.
2. 0.35g of hexadecyltrimethoxysilane, 0.35g of octadecyltriethoxysilane and 10g of anhydrous ethanol were thoroughly mixed and stirred uniformly at 100 rpm.
3. Adding the solution in the step 2 into the mixed solution in the step 1, stirring at the rotating speed of 300rpm, and reacting for 4 hours.
4. 2g of ammonia water was added and the reaction was continued with stirring for 4 h.
5. 1.5g E44 epoxy resin was added and the reaction was continued for 2h with stirring.
6. After the reaction, the product was taken out, and 1.5g of nano titanium dioxide having an average particle size of 20nm was added thereto, and sufficiently stirred at a rotation speed of 150rpm at room temperature to be uniformly mixed.
7. The above nano photocatalyst stock solution is diluted by absolute ethyl alcohol according to the proportion of 1:20 to prepare nano photocatalyst treatment solution.
8. The above treatment liquid was sprayed on both surfaces of the nonwoven fabric using an air compressor and dried at 60 ℃ in a ventilated atmosphere for at least 2 hours to give a coating thickness of 35 μm.
Comparative example 1
Drying the common non-woven fabric without special treatment for at least 2h in a ventilation environment at 60 ℃.
Performance detection
Contact angle, roll angle: and (3) testing the contact angle and the rolling angle of the surface of the sample by using a water drop angle tester, taking five different positions of each sample for testing, and calculating an average value.
Bacterial adhesion rate: an equal amount of staphylococcus aureus culture solution is taken, a tested sample (an example and a comparative example) is flushed at an equal flow rate, then the number of colonies remained on the sample in a specified area and the number of colonies on original culture solution are detected by using a full-automatic colony counter, and the bacterial adhesion rate is equal to the number of colonies of the sample/the number of colonies of the culture solution. Five tests were run per sample and the average was calculated.
Mask filtration efficiency: tested according to the method of GB 2626-2006.
For the single-layered nonwoven fabrics having inner and outer coatings prepared according to examples 1 to 5, the contact angle, the rolling angle and the bacterial adhesion rate were measured according to the above methods. The results are shown in table 1 below.
The mask structure with three layers was assembled from the inner and outer layers of the common nonwoven fabric and the nonwoven fabric with the coating prepared according to examples 1 to 5. The resulting mask structure was tested for mask filtration efficiency and the results are shown in table 1 below.
TABLE 1
| Sample (I) | Contact angle | Roll angle | Rate of bacterial adherence | Filtration efficiency of mask |
| Example 1 | 162° | 5° | 2％ | 99％ |
| Example 2 | 157° | 9° | 3％ | 99％ |
| Example 3 | 154° | 7° | 2％ | 98％ |
| Example 4 | 163° | 10° | 2％ | 98％ |
| Example 5 | 155° | 5° | 3％ | 98％ |
| Example 6 | 160° | 10° | 1％ | 97％ |
| Comparative example 1 | ～0° | Is free of | 99％ | 95％ |
As can be seen from the data in the above Table 1, after the treatment solution of the present invention is used to spray-coat a non-woven fabric, the front and back surfaces of the non-woven fabric are uniformly covered with the nano photocatalyst filter layer, and a mask with high blocking effect and sterilization effect can be prepared. The mask filter layer can effectively prevent pollutants and microorganisms in the air from adhering to the mask, block the contamination of external harmful substances, filter the air, kill the adhered pollutants and microorganisms and have a lasting and effective effect.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
Claims (10)
1. A nano photocatalyst antibacterial filter layer for a protective device is characterized by comprising nano photocatalyst particles and hydrophobic modified nano silicon dioxide.
2. The nano-photocatalyst antibacterial filter layer of claim 1, wherein the nano-photocatalyst particles are nano-titania.
3. The nano photocatalyst antibacterial filter layer according to claim 1, wherein the average particle size of the nano photocatalyst particles is 10 to 30nm, and the average particle size of the nano silica before hydrophobic modification is 7 to 20 nm.
4. The nano-photocatalyst antibacterial filter layer of claim 1, wherein the weight ratio of the nano-photocatalyst particles to the nano-silica before hydrophobic modification is 1: 3.
5. The nano-photocatalyst antibacterial filter layer of claim 1, the hydrophobically modified nano-silica surface containing long chain alkyl groups.
6. The nano photocatalyst antibacterial filter layer as claimed in any one of claims 1 to 5, the preparation method of the treatment liquid for forming the nano photocatalyst antibacterial filter layer comprises the steps of:
carrying out surface treatment on the nano silicon dioxide by adopting one or more silane coupling agents containing C14-C18 long-chain alkyl;
under the action of an amine catalyst, a cross-linking agent and the nano-silicon dioxide subjected to surface treatment are subjected to cross-linking reaction to prepare nano-silicon dioxide mixed solution;
adding the nano photocatalyst particles into the nano silicon dioxide mixed solution, and uniformly stirring to obtain a nano photocatalyst stock solution.
7. The nano photocatalyst antibacterial filter layer according to claim 6, wherein the amine catalyst is ammonia water, the cross-linking agent is epoxy resin, and the cross-linking reaction temperature is 15-25 ℃.
8. The nano photocatalyst antibacterial filter layer according to claim 6, wherein the weight ratio of the silane coupling agent to the nano silica is 0.2-0.33: 1.
9. A guard comprising an inner nonwoven layer, an outer nonwoven layer and an intermediate nonwoven layer between the inner and outer nonwoven layers, characterized in that the intermediate nonwoven layer has a nano-photocatalyst antibacterial filter layer according to any one of claims 1 to 8.
10. The protective device of claim 9, which is a mask.
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