CN103989269A - Method for manufacturing photocatalysis self-cleaning mask - Google Patents
Method for manufacturing photocatalysis self-cleaning mask Download PDFInfo
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- CN103989269A CN103989269A CN201410219837.5A CN201410219837A CN103989269A CN 103989269 A CN103989269 A CN 103989269A CN 201410219837 A CN201410219837 A CN 201410219837A CN 103989269 A CN103989269 A CN 103989269A
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Abstract
The invention provides a method for manufacturing a photocatalysis self-cleaning mask. The method is characterized by including the specific steps of firstly, preparing TiO2/SiO2 mixed sol; secondly, removing impurities on the mask, cleaning the mask, and conducting radio frequency plasma preprocessing on the mask; thirdly, soaking the mask where radio frequency plasma preprocessing is conducted in the TiO2/SiO2 mixed sol, conducting the twice-soaking and twice-rolling process, drying the mask for three minutes to eight minutes at the temperature of 70 DEG C to 90 DEG C, curing the mask for one minute to five minutes at the temperature of 100 DEG C to 150 DEG C, cleaning the mask through deionized water, drying the mask under the natural condition, and obtaining the photocatalysis self-cleaning mask. The photocatalysis self-cleaning mask manufactured through the method is good in self-cleaning effect and durable in effect. The method can be applied to industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of photocatalytic self-cleaning mouth mask, belong to finishing field after weaving face fabric.
Background technology
Since entering 21st century, the mankind's industrial civilization is able to fast development, and the problem of environmental pollution causing is thus increasingly severe.The today of becoming increasingly prosperous and developing in economy, oneself becomes a direct threat human survival and focal issue anxious to be resolved problem of environmental pollution.And along with the development of World Economics, personnel transfer is unprecedentedly frequent, the various diseases possibility that particularly communicate illness occurs and day sharp increase, have large area outburst when some burst diseases, how to prevent various burst diseases to become the significant problem that the mankind face.Except perfecting national community health Healthy System and improving the common people's health consciousness, it is very necessary adopting convenient and practical protection tool.Wearing mouth mask is exactly a kind of traditional, easy to use and effective safeguard procedures.Common mouth mask is generally made with degreasing cotton gauze or nonwoven, and it is by the most dust granules that suspend in human body self-absorbing filtering mode blocks air.But for than the less dust granule of gauze hole dimension and germ, the protective benefits of common mouth mask is often very low.And the skin of mouth mask is often gathering the dirt such as dust, bacterium in a lot of outside airs, and nexine is stopping bacterium, the saliva breathed out, therefore, two sides can not be used alternatingly, otherwise the dirt that skin can be infected with sucks human body in the time being directly close to face, and becomes the infection sources.Therefore, give that common mouth mask is given dust-break, anti-to kill many safeguard functions such as bacterium and virus be the research topic that has important practical usage.
Since Fujishima in 1972 and Honda etc. find the TiO of raying
2on can carry out lasting water redox reaction and produce after hydrogen, semiconductor catalysis comes into one's own, and has been unfolded research widely.Along with the development of Photocatalitic Technique of Semiconductor, its application also constantly expand, by first for sewage disposal, the appearance of self-cleaned by photocatalyst glass, pottery, textile finally, photocatalyst technology has slowly been come into people's life.
Photocatalyst is that a class is with TiO
2for the general name of the semi-conducting material with photocatalysis performance of representative.The semi-conducting material that can be used as at present photochemical catalyst mainly contains TiO
2, CdS, ZnO, WO
3, Fe
2o
3, SnO
2deng compound, but due to TiO
2advantages such as relatively other semi-conducting materials have that photocatalytic activity is high, good stability, price are low and enjoy favor.Photocatalyst can produce similar photosynthetic catalytic reaction under the irradiation of sunshine or fluorescent lamp, and airborne oxygen and hydrone are excited, and forms extremely strong hydroxyl radical free radical (OH) and the ultra-oxygen anion free radical (O of oxidability
2-).The extremely strong free radical of these oxidizing forces can kill the aerial bacterium that swims, and organic pollution is constantly degraded into water and carbon dioxide etc., thereby reaches environment purification and keep the clean and not contaminated object of material self.Photocatalyst technology is applied to field of textiles, and it is significant for energy-conserving and environment-protective that exploitation has the textile of environmental protection self-cleaning performance.
Due to TiO
2photocatalysis can only utilize wavelength to be less than the ultraviolet light of 400nm, and this part light only accounts for 3%~5% of daylight luminous energy, and temporal evolution is obvious.This has greatly restricted efficiency and the application of photocatalytic self-cleaning material, and SiO
2have good network structure, be difficult for assembling, preparation method is simple, and refractive index is low, and can improve TiO
2photocatalysis efficiency, therefore we utilize sol-gel process to prepare TiO
2-SiO
2laminated film, by controlling TiO
2with SiO
2the factor such as the molecular weight of adding proportion, pore creating material and addition, solvent (ethanol) consumption, make the laminated film of preparation both there is SiO
2lower refractive index, preferably heat endurance and mechanical stability, there is again TiO
2photocatalysis performance and hydrophilicity preferably.
In the last few years, along with air quality runs down, the haze weather phenomenon frequency of occurrences was more and more higher, and they invade in human respiratory tract and the lobe of the lung when people have no to take precautions against, thereby give rise to diseases.And the research of the Chinese government to photocatalytic product and application thereof are also very paid attention to,, in " 12 " plan, national nanometer plan and " 863 " in the works, nano-photo catalytic is all listed in important research project.A kind ofly there is efficient anti-soil, antibacterial automatically cleaning mouth mask taking nano-photo catalytic as mechanism so be necessary to develop, for the intrusion and the transmission of disease that reduce harmful particle in air do effective protective action.
Summary of the invention
The object of the invention is to develop one and there is photocatalytic self-cleaning effect, energy dust-break, the anti-mouth mask that kills many safeguard functions such as bacterium and virus.
In order to achieve the above object, the invention provides a kind of preparation method of photocatalytic self-cleaning mouth mask, it is characterized in that, concrete steps comprise:
The first step: preparation TiO
2/ SiO
2mixed sols;
Second step: by mouth mask decontamination, clean, then mouth mask is carried out to radio frequency plasma pretreatment;
The 3rd step: pretreated radio frequency plasma mouth mask is immersed in to TiO
2/ SiO
2in mixed sols, adopt two to soak two roll process, then dry after 3-8 minute at 70-90 DEG C, at 100-150 DEG C, solidify 1-5 minute; Dry under field conditions (factors) with putting after washed with de-ionized water, obtain photocatalytic self-cleaning mouth mask.
Preferably, in the described first step, TiO
2/ SiO
2the preparation method of mixed sols comprises:
Step 1: the tetraisopropyl titanate that is 30-99% by mass fraction, ethyl orthosilicate and absolute ethyl alcohol mix, and stir 0.5-3 hour under room temperature, obtain A solution;
Step 2: the HCl that is 10-70% by mass fraction, absolute ethyl alcohol and deionized water are mixed, makes pH value for 2-6, stirs 0.5-3 hour under room temperature, obtains B solution;
Step 3: the B solution that step 2 is obtained is added drop-wise in the A solution that step 1 prepares, and stirs 1.0-3 hour; Adding molecular weight is the PEG of 1-4KDa, is heated to 40-80 DEG C and stir 1.0-3 hour, and ageing 2-24 hour, obtains TiO
2/ SiO
2mixed sols.
The volume ratio of tetraisopropyl titanate, ethyl orthosilicate and absolute ethyl alcohol that more preferably, in described step 1, mass fraction is 30-99% is 1: (1.0~6.0): (10~60).
The volume ratio of HCl, ethanol and deionized water that more preferably, the mass fraction in described step 2 is 10-70% is 0.1: (1.0~3.0): 15~80.
More preferably, the volume ratio of the absolute ethyl alcohol in described step 1 and step 2 is (1-4): 1.
More preferably, the ratio of the cumulative volume of the absolute ethyl alcohol in addition and step 1 and the step 2 of the PEG in described step 3 is lg: 10-15ml.
Preferably, in the described first step, TiO
2/ SiO
2the preparation method of mixed sols comprises:
Step 1: the tetraisopropyl titanate that is 30-99% by mass fraction and absolute ethyl alcohol mix, and stir 0.5-3 hour under room temperature, obtain C solution;
Step 2: ethyl orthosilicate is added in the mixed solution of ethanol and deionized water under stirring, and then adding mass fraction is the HCl of 10-70%, makes pH value for 2-4, and at room temperature ultrasonic processing acidifying 0.5-1h, obtains D solution;
Step 3: C solution is added drop-wise in D solution, ultrasonic processing 1-3 hour, aged at room temperature 2-24 hour, obtains TiO
2/ SiO
2mixed sols.
More preferably, the tetraisopropyl titanate that the mass fraction in described step 1 is 30-99% and the volume ratio of absolute ethyl alcohol are 1: (2-5).
More preferably, in ethanol in described step 2 and the mixed solution of deionized water, the volume ratio of ethanol and deionized water is 1: (0.01-0.03), the volume ratio of the mixed solution of ethyl orthosilicate and ethanol and deionized water is 1: (2-4).
More preferably, the volume ratio of described C solution and D solution is 1: (1.5-3).
Preferably, the cleaning in described second step comprises with nonionic detergent cleaning, uses afterwards washed with de-ionized water.
More preferably, described nonionic detergent is 3% (owf) Sandoclean PC or Kieralon OL, and scavenging period is 0.5-1 hour, cleans and carries out under ul-trasonic irradiation with nonionic detergent.
More preferably, described use washed with de-ionized water is carried out under ul-trasonic irradiation, and scavenging period is 0.5-3 hour.
Preferably, in described second step, the pretreated treatment conditions of radio frequency plasma are: adopt the low-temp low-pressure glow discharge plasma of 12.56MHZ discharge frequency to carry out discharge process to material.Wherein, pressure 20-45Pa, discharge power 50-100W, processing time 1-10 minute.
Preferably, two pressure that soak milling train in two roll process in described the 3rd step are 3-5kg/cm
2, rotating speed is 3-6rpm.
Compared with prior art, the invention has the beneficial effects as follows:
1, mouth mask of the present invention first passes through Cement Composite Treated by Plasma, makes its surface etching to a certain degree, produces active group, then carries out functional-coated arrangement, is conducive to the combination of fabric and functional finishing agent, improves the cross-linking reaction between finishing agent and fabric.
2, use TiO
2/ SiO
2the synergy of mixed sols, makes the laminated film of preparation both have SiO
2lower refractive index, preferably heat endurance and mechanical stability, there is again TiO
2preferably photocatalysis performance and hydrophilicity, significantly improves the automatically cleaning efficiency of mouth mask under different illumination conditions.
3, add PEG as pore creating material, the Detitanium-ore-type that makes to exist in whole film smaller szie and high dispersive is received crystalline substance, therefore has higher photocatalytic activity.
4, the prepared automatically cleaning mouth mask of preparation method of the present invention, automatically cleaning is effective, and effect is lasting.Preparation method is applicable to suitability for industrialized production.
Brief description of the drawings
Fig. 1-1 is SEM figure before mouth mask coating,
Fig. 1-2 is SEM figure after mouth mask coating;
Fig. 2 is the photocatalytic self-cleaning fabric situation that different time decomposes coffee stain under high light in the embodiment of the present invention 1
Fig. 3 is the photocatalytic self-cleaning fabric situation that different time decomposes coffee stain under high light in the embodiment of the present invention 2
Fig. 4 is the contact angle (under the ultraviolet light of 254nm after illumination 3h) of photocatalytic self-cleaning fabric and water in the embodiment of the present invention 1
Fig. 5 is the contact angle (under the ultraviolet light of 254nm after illumination 3h) of photocatalytic self-cleaning fabric and water in the embodiment of the present invention 2
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that, after having read content of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
A preparation method for photocatalytic self-cleaning mouth mask, concrete steps are:
(1) prepare TiO
2/ SiO
2mixed sols:
As shown in Figure 1, the tetraisopropyl titanate that is 97% by 2ml mass fraction and 10ml absolute ethyl alcohol mix, and the mixing speed with 800rmp under room temperature stirs 0.5 hour.
5ml ethyl orthosilicate is added in the mixed solution of 10ml ethanol and 1ml deionized water under stirring, and then adding mass fraction is 10% HCL0.2ml, and making pH is 2, at room temperature ultrasonic processing acidifying 30 minutes.Its reaction equation is as follows:
1) hydrolysis
Si(OC
2H
5)
4+4H
2O→Si(OH)
4+4C
2H
5OH
2) polymerisation
The tetraisopropyl titanate that is dissolved in absolute ethyl alcohol is added drop-wise in the teos solution of previous step preparation to ultrasonic processing 30min with the speed of 1 drop/sec.By the TiO of gained
2-SiO
2colloidal sol aged at room temperature 24 hours.
Its concrete reaction is as follows:
1) hydrolysis
Ti{OCH(C
2H
3)
2}
4+nH
2O→Ti{OCH(C
2H
3)
2}
4-n(OH)
n+n(C
2H
3)
2CHOH(n=1,2,3,4)
2) polymerisation
{(C
2H
3)
2CHO}
3Ti-OH+HO-Ti{OCH(C
2H
3)
2}
3→H
2O+{(C
2H
3)
2CHO}
3Ti-O-Ti{OCH(C
2H
3)
2}
3
{(C
2H
3)
2CHO}
3Ti-OCH(C
2H
3)
2+HO-Ti{OCH(C
2H
3)
2}
3→{(C
2H
3)
2CHO}
3Ti-O-Ti{OCH(C
2H
3)
2}
3+(C
2H
3)
2CHOH
3) later stage of sol-process, the TiO of generation
2the intermolecular further polycondensation of colloidal sol, and slough H
2o molecule or alcohol molecule, be just configured to the gel of network state.
(2) mouth mask pretreatment
By 17.5 × 9cm, grammes per square metre is the mouth mask decontamination of 200g/, cleans 30 minutes with nonionic detergent 3% (owf) Sandoclean PC at 40 DEG C under ul-trasonic irradiation, then under ul-trasonic irradiation, cleans 0.5 hour by deionized water.Then with RF plasma processing device pretreatment mouth mask, the pretreated treatment conditions of radio frequency plasma are: adopt the low-temp low-pressure glow discharge plasma of 12.56MHZ discharge frequency to carry out discharge process to material.Wherein, pressure 25Pa, discharge power 100W, 3 minutes processing times.
(3) colloidal sol arranges
As Figure 1-1, be SEM figure before mouth mask coating, mouth mask after treatment is immersed in TiO
2/ SiO
2in mixed sols, adopt two to soak two roll process, the pressure of milling train is 3kg/cm
2, rotating speed is 6rpm, then, after 5 minutes, solidifies 3 minutes in 120 DEG C, baking oven at 80 DEG C of oven dryings, dry under field conditions (factors) with putting after washed with de-ionized water, obtains photocatalytic self-cleaning mouth mask.As shown in Figure 1-2, be SEM figure after mouth mask coating.
Coffee being sprinkled upon on the photocatalytic self-cleaning mouth mask of gained, as shown in Figure 2, is the photocatalytic self-cleaning fabric situation that different time decomposes coffee stain under high light.As shown in Figure 4, be the contact angle of photocatalytic self-cleaning fabric and water in the embodiment of the present invention 1 (under the ultraviolet light of 254nm after illumination 3h).
Embodiment 2
(1) prepare TiO
2/ SiO
2mixed sols
The tetraisopropyl titanate that is 95% by 2ml mass fraction, 10ml ethyl orthosilicate and 40ml absolute ethyl alcohol mix, and the mixing speed with 800rmp under room temperature stirs one hour, is called A solution; The HCl that is 37% by 0.5ml mass fraction, 20ml ethanol, 3ml deionized water are mixed, and making pH value is 3, and the mixing speed with 800rmp under room temperature stirs 0.5 hour, is called B solution.And then with the speed of 3 drops/sec, B solution is slowly joined in A solution, stir 1 hour, then to add 5g molecular weight be the PEG of 4000KDa, be heated to 60 DEG C, to stir 1 hour, ageing 2 hours, obtains TiO
2/ SiO
2mixed sols.
(2) mouth mask pretreatment
By 17.5 × 9cm, grammes per square metre is the mouth mask decontamination of 200g/, cleans 30 minutes with nonionic detergent 3% (owf) Sandoclean PC under hyperacoustic effect at 40 DEG C, then under ul-trasonic irradiation, cleans 0.5 hour by deionized water.Then with RF plasma processing device pretreatment mouth mask, the pretreated treatment conditions of radio frequency plasma are: adopt the low-temp low-pressure glow discharge plasma of 12.56MHZ discharge frequency to carry out discharge process to material.Wherein, pressure 25Pa, discharge power 100W, 4 minutes processing times.
(3) colloidal sol arranges
Mouth mask after treatment is immersed in TiO
2/ SiO
2in mixed sols, adopt two to soak two roll process, the pressure of milling train is 3kg/cm
2, rotating speed is 6rpm, then, after 5 minutes, solidifies 3 minutes in 120 DEG C, baking oven at 80 DEG C of oven dryings, dry under field conditions (factors) with putting after washed with de-ionized water, obtains photocatalytic self-cleaning mouth mask.
Coffee being sprinkled upon on the photocatalytic self-cleaning mouth mask of gained, as shown in Figure 3, is the photocatalytic self-cleaning fabric situation that different time decomposes coffee stain under high light.As shown in Figure 5, be the contact angle of photocatalytic self-cleaning fabric and water in the embodiment of the present invention 1 (under the ultraviolet light of 254nm after illumination 3h).Fig. 5 shows, in 483ms, contact angle is reduced to rapidly 2 °, and water droplet is absorbed by fabric very soon.
Claims (10)
1. a preparation method for photocatalytic self-cleaning mouth mask, is characterized in that, concrete steps comprise:
The first step: preparation TiO
2/ SiO
2mixed sols;
Second step: by mouth mask decontamination, clean, then mouth mask is carried out to radio frequency plasma pretreatment;
The 3rd step: pretreated radio frequency plasma mouth mask is immersed in to TiO
2/ SiO
2in mixed sols, adopt two to soak two roll process, then dry after 3-8 minute at 70-90 DEG C, at 100-150 DEG C, solidify 1-5 minute; Dry under field conditions (factors) with putting after washed with de-ionized water, obtain photocatalytic self-cleaning mouth mask.
2. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 1, is characterized in that, in the described first step, and TiO
2/ SiO
2the preparation method of mixed sols comprises:
Step 1: the tetraisopropyl titanate that is 30-99% by mass fraction, ethyl orthosilicate and absolute ethyl alcohol mix, and stir 0.5-2 hour under room temperature, obtain A solution;
Step 2: the HCl that is 10-70% by mass fraction, absolute ethyl alcohol and deionized water are mixed, makes pH value for 2-6, stirs 0.5-3 hour under room temperature, obtains B solution;
Step 3: the B solution that step 2 is obtained is added drop-wise in the A solution that step 1 prepares, and stirs 1.0-3 hour; Adding molecular weight is the PEG of 1000-4000KDa, is heated to 40-80 DEG C and stir 1.0-3 hour, and ageing 2-24 hour, obtains TiO
2/ SiO
2mixed sols.
3. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 2, it is characterized in that, the volume ratio of tetraisopropyl titanate, ethyl orthosilicate and absolute ethyl alcohol that in described step 1, mass fraction is 30-99% is 1: (1.0-6.0): (10-60).
4. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 2, it is characterized in that, the volume ratio of HCl, ethanol and deionized water that the mass fraction in described step 2 is 10-70% is 0.1: (1.0-3.0): (15-80).
5. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 2, is characterized in that, the volume ratio of the absolute ethyl alcohol in described step 1 and step 2 is (1-4): 1.
6. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 2, is characterized in that, the ratio of the cumulative volume of the absolute ethyl alcohol in addition and step 1 and the step 2 of the PEG in described step 3 is 1g:10-15ml.
7. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 1, is characterized in that, in the described first step, and TiO
2/ SiO
2the preparation method of mixed sols comprises:
Step 1: metatitanic acid four isopropyl alcohols that are 30-99% by mass fraction and absolute ethyl alcohol mix, and stir 0.5-3 hour under room temperature, obtain C solution;
Step 2: ethyl orthosilicate is added in the mixed solution of ethanol and deionized water under stirring, and then adding mass fraction is the HCl of 10-70%, makes pH value for 2-4, and at room temperature ultrasonic processing acidifying 0.5-3 hour, obtains D solution;
Step 3: C solution is added drop-wise in D solution, ultrasonic processing 1-3 hour, aged at room temperature 2-24 hour, obtains TiO
2/ SiO
2mixed sols.
8. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 1, is characterized in that, the cleaning in described second step comprises with nonionic detergent cleaning, uses afterwards washed with de-ionized water.
9. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 1, it is characterized in that, in described second step, the pretreated treatment conditions of radio frequency plasma are: adopt the low-temp low-pressure glow discharge plasma of 12.56MHZ discharge frequency to carry out discharge process to material, wherein, pressure 20-45Pa, discharge power 50-100W, processing time 1-10 minute.
10. the preparation method of photocatalytic self-cleaning mouth mask as claimed in claim 1, is characterized in that, two pressure that soak milling train in two roll process in described the 3rd step are 3~5kg/cm
2, rotating speed is 3~6rpm.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105286134A (en) * | 2015-12-07 | 2016-02-03 | 刘博纯 | Method for preparing photocatalytic mouth mask |
WO2020097880A1 (en) * | 2018-11-15 | 2020-05-22 | 中国科学院大连化学物理研究所 | Macromolecular ultraviolet absorbent, preparation method therefor and application thereof |
CN111658798A (en) * | 2020-06-15 | 2020-09-15 | 安徽静斯德科技有限公司 | Mask disinfection and sterilization method based on plasma |
CN112195648A (en) * | 2020-08-28 | 2021-01-08 | 无锡市宇寿医疗器械有限公司 | Photocatalytic self-cleaning non-woven fabric, preparation method and mask prepared from same |
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CN2652434Y (en) * | 2003-09-10 | 2004-11-03 | 武汉理工大学 | Optical catalytic elecronic mask with high adsorptive property |
CN2696665Y (en) * | 2004-04-29 | 2005-05-04 | 天津理工学院 | Nano antiseptic mouthpiece |
WO2007078412A1 (en) * | 2005-12-21 | 2007-07-12 | Kimberly-Clark Worldwide, Inc. | Germicidal surface-covering assembly |
CN101810373A (en) * | 2009-10-12 | 2010-08-25 | 上海伯欧环保科技发展有限公司 | Photocatalyst antiseptic mask and manufacturing process thereof |
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CN2652434Y (en) * | 2003-09-10 | 2004-11-03 | 武汉理工大学 | Optical catalytic elecronic mask with high adsorptive property |
CN2696665Y (en) * | 2004-04-29 | 2005-05-04 | 天津理工学院 | Nano antiseptic mouthpiece |
WO2007078412A1 (en) * | 2005-12-21 | 2007-07-12 | Kimberly-Clark Worldwide, Inc. | Germicidal surface-covering assembly |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105286134A (en) * | 2015-12-07 | 2016-02-03 | 刘博纯 | Method for preparing photocatalytic mouth mask |
WO2020097880A1 (en) * | 2018-11-15 | 2020-05-22 | 中国科学院大连化学物理研究所 | Macromolecular ultraviolet absorbent, preparation method therefor and application thereof |
CN111658798A (en) * | 2020-06-15 | 2020-09-15 | 安徽静斯德科技有限公司 | Mask disinfection and sterilization method based on plasma |
CN112195648A (en) * | 2020-08-28 | 2021-01-08 | 无锡市宇寿医疗器械有限公司 | Photocatalytic self-cleaning non-woven fabric, preparation method and mask prepared from same |
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