CN115110308B - External heat and internal cold Janus antibacterial material with light responsiveness and preparation method thereof - Google Patents
External heat and internal cold Janus antibacterial material with light responsiveness and preparation method thereof Download PDFInfo
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 52
- 230000004043 responsiveness Effects 0.000 title claims abstract description 18
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- 239000002096 quantum dot Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 26
- 230000000694 effects Effects 0.000 claims abstract description 20
- 238000004729 solvothermal method Methods 0.000 claims abstract description 20
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
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- 238000000576 coating method Methods 0.000 claims abstract description 7
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- 239000004743 Polypropylene Substances 0.000 claims description 28
- 229920001155 polypropylene Polymers 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
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- KETXQNLMOUVTQB-UHFFFAOYSA-N 2,3,7,8,12,13,17,18-octaethylporphyrin;platinum Chemical compound [Pt].C=1C(C(=C2CC)CC)=NC2=CC(C(=C2CC)CC)=NC2=CC(C(=C2CC)CC)=NC2=CC2=NC=1C(CC)=C2CC KETXQNLMOUVTQB-UHFFFAOYSA-N 0.000 claims description 3
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- 239000002184 metal Substances 0.000 claims description 3
- FCNCGHJSNVOIKE-UHFFFAOYSA-N 9,10-diphenylanthracene Chemical compound C1=CC=CC=C1C(C1=CC=CC=C11)=C(C=CC=C2)C2=C1C1=CC=CC=C1 FCNCGHJSNVOIKE-UHFFFAOYSA-N 0.000 claims description 2
- 241000192125 Firmicutes Species 0.000 claims description 2
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- 229920001131 Pulp (paper) Polymers 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
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- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 claims description 2
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 claims description 2
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 2
- CTWKPPTYPMKFQL-UHFFFAOYSA-N platinum 5,10,15,20-tetraphenyl-21,23-dihydroporphyrin Chemical compound [Pt].c1cc2nc1c(-c1ccccc1)c1ccc([nH]1)c(-c1ccccc1)c1ccc(n1)c(-c1ccccc1)c1ccc([nH]1)c2-c1ccccc1 CTWKPPTYPMKFQL-UHFFFAOYSA-N 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
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- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
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- 229910004613 CdTe Inorganic materials 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 8
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- 239000006185 dispersion Substances 0.000 description 6
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- 239000007788 liquid Substances 0.000 description 6
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- 239000011259 mixed solution Substances 0.000 description 5
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 4
- 238000003331 infrared imaging Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 241000194019 Streptococcus mutans Species 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
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- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical class C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 2
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- 229910004573 CdF 2 Inorganic materials 0.000 description 1
- 229910017768 LaF 3 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
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- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/52—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with selenium, tellurium, polonium or their compounds; with sulfur, dithionites or compounds containing sulfur and halogens, with or without oxygen; by sulfohalogenation with chlorosulfonic acid; by sulfohalogenation with a mixture of sulfur dioxide and free halogens
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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Abstract
The invention discloses an external heat and internal cold Janus antibacterial material with light responsiveness and a preparation method thereof, wherein the preparation method comprises the following steps: synthesizing nano particles or quantum dots with photo-thermal effect by adopting a solvothermal method; synthesizing an up-conversion material with a light cooling effect by adopting a solvothermal method; and adopting methods of spraying, sputtering, depositing and the like to respectively cover the photo-thermal material and the photo-cooling material on the two sides of the protective material in a coating mode, so as to construct the antibacterial protective material with the Janus structure. According to the invention, the Janus structure is constructed by synchronously introducing the photo-thermal functional material and the photo-cooling functional material, so that photo-thermal sterilization of the protective articles is realized, the photo-cooling effect is utilized, the thermal effect of the contact surface of the protective articles and human bodies is reduced to the greatest extent, the skin-friendly performance and the use experience of the antibacterial protective articles are improved, and the practical application requirements of the medical protective materials are met.
Description
Technical Field
The invention relates to a preparation method of an external heat and internal cold Janus antibacterial material with light responsiveness, belonging to the technical field of preparation of photothermal antibacterial functional materials and biomedical protective materials.
Background
The novel material with excellent antibacterial property has very important market demand and huge market value in the field of life health, can effectively ensure life safety and prevents the increment and secondary propagation of bacteria. The photo-thermal sterilization is an emerging technology, can convert light energy into local heat energy by utilizing the band gap specificity of a photo-thermal functional material, further kills bacteria, has the advantages of low energy consumption, environmental friendliness, high safety and the like, and is expected to realize remote accurate sterilization of protective articles. The photo-thermal functional materials currently used for improving the antibacterial performance of the protective material comprise carbon nanotubes (CN 111000566A), silver nanoparticles, gold nanoparticles (CN 113332484A) and the like, and all have excellent antibacterial performance. However, under the condition of illumination, although the photothermal antibacterial functional material can effectively kill bacteria, there are still some problems, such as the increase of the temperature of the protective material itself, so that the skin-friendly property of the protective material itself is reduced, and the use experience of the protective material on the contact surface with the human body is poor. Therefore, the development of Janus antibacterial functional materials with external heat and internal cold can effectively promote the actual industrialized application of photo-thermal antibacterial materials
The physical cooling of the up-conversion material can be effectively realized by utilizing the anti-Stokes fluorescence cooling effect of the up-conversion material, and the method has heuristic significance for the development of external heat and internal cooling type materials. CN109564056a discloses a double-or multi-layer device or arrangement for optical anti-stokes cooling of an object surface, exploiting active cooling independent of the coherent nature of the radiation, which enables the use of incoherent solar radiation as an active cooling input energy source. The invention designs an external heat and internal cold Janus antibacterial protective material by utilizing the anti-Stokes cooling effect of the up-conversion material and combining a photo-thermal functional material, so that one surface of the Janus antibacterial protective material has excellent antibacterial performance, and the other surface of the Janus antibacterial protective material still maintains skin-friendly performance, and has important significance for realizing practical application of the photo-thermal antibacterial protective material in the early days.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an external heat and internal cold Janus antibacterial material with light responsiveness and a preparation method thereof.
The invention adopts the following technical scheme to realize the purposes:
1. solvent thermal method for synthesizing nano particles or quantum dots with photo-thermal effect
Dispersing a source material of the nano particles in a solvent with a certain concentration (0.01-0.1 mmol/mL) by adopting a solvothermal method, and magnetically stirring for 5-20 min; after being uniformly mixed, the mixture undergoes solvothermal reaction for 0.1 to 720 minutes at the temperature of 50 to 210 ℃; cooling to room temperature after the reaction is finished, centrifuging at 5000-18000 rpm, and vacuum drying at 40-100 ℃ to obtain the required nano particles or quantum dots.
Wherein the nanoparticle or QDs with photothermal effect is selected from purple phosphorus, black phosphorus, graphene oxide, graphite alkyne, carbon nanotube, au nanoparticle, ag nanoparticle, ti 3 C 2 T x Nanoplatelets, ti 2 CT x Nanosheets, V 2 CT x Nanoplatelets, nb 2 CT x Nanoplatelets, mo 2 CT x Nanosheets, cr 2 CT x Nanoplatelets, hf 2 CT x Nanoplatelets, ti 3 CNT x One or two or three of nano-sheets, bi QDs, se QDs, sb QDs, te QDs, agS QDs, snS nano-sheets, snSe nano-sheets, snTe nano-sheets, cdS QDs/nano-sheets, cdSe QDs/nano-sheets, cdTe QDs/nano-sheets, pbS QDs/nano-sheets, pbSe QDs/nano-sheets, pbTe QDs/nano-sheets, znS QDs/nano-sheets, znSe QDs/nano-sheets and ZnTe QDs/nano-sheets.
The solvent is one or two of ethanol, ethyl acetate, isopropanol, n-butanol, tert-butanol, toluene, n-hexane, petroleum ether, dichloromethane and deionized water.
2. Solvent thermal method for synthesizing up-conversion material with light cooling effect
Uniformly dispersing a source material in a solvent according to a certain concentration (0.01-0.1 mmol/mL) by adopting a solvothermal method; after being uniformly mixed, the mixture is subjected to solvothermal reaction for 0.1 to 720 minutes at the temperature of 50 to 450 ℃; cooling to room temperature after the reaction is finished, centrifuging at 5000-18000 rpm, and vacuum drying at 40-100 ℃ to obtain the material with the light cooling effect.
The up-conversion material with the light cooling effect is one or two or three of rare earth up-conversion material, semiconductor double quantum dot system and organic molecular system.
The rare earth up-conversion material is composed of a host material including fluoride (GdF) 3 、YF 3 、LaF 3 、LiYF 4 、BaF 2 、NaYF 4 、LiLuF 4 Etc.), rare earth oxide (Y 2 O 3 、ZrO 2 、Gd 2 O 2 、NaY(WO 4 ) 2 、Nd 2 (WO 4 ) 3 、YVO 4 Etc.), oxyfluoride (SiO 2 -Al 2 O 3 -PbF 2 -CdF 2 Etc.), halides (LaCl) 3 、Cs 3 Lu 2 Br 9 Etc., oxyhalideObject (YOCl) 3 Etc.), sulfur-containing compound (Y) 2 O 2 S、La 2 O 2 S、Ca 2 O 3 -La 2 S 3 Etc.); sensitizer ions comprising Yb 3+ And Nd 3+ The method comprises the steps of carrying out a first treatment on the surface of the Activator ions include Er 3+ 、Tm 3+ 、Ho 3+ The method comprises the steps of carrying out a first treatment on the surface of the Doped metal cations include Ba 2+ 、Bi 3+ 、Li + 、Na + 、Ca 2 + 、Sr 2+ Etc.
The semiconductor double-quantum dot system comprises an absorber, a potential barrier and a luminous body, wherein the absorber comprises one or two of CdS, cdSe, cdSe (Te), cdTe, pbS, pbSe, pbSe (Te), pbTe, znS, znSe, znSe (Te), znTe, snS, snSe, snSe (Te) and SnTe; the potential barrier comprises one or two or three of CdS, cdSe, cdSe (Te), cdTe, pbS, pbSe, pbSe (Te), pbTe, znS, znSe, znSe (Te), znTe, snS, snSe, snSe (Te) and SnTe; the illuminant includes one or two of CdS, cdSe, cdSe (Te), cdTe, pbS, pbSe, pbSe (Te), pbTe, znS, znSe, znSe (Te), znTe, snS, snSe, snSe (Te), and SnTe.
The organic molecular system comprises energy donor molecules and acceptor molecules, wherein the donor molecules comprise platinum (II) -octaethylporphyrin (PtOEP), palladium (II) -octaethylporphyrin (PdOEP), 5,10,15, 20-tetraphenylporphyrin palladium (PdPP), 5,10,15, 20-tetraphenylporphyrin platinum (PtTPP), pdTTP, palladium tetraphenylporphyrin (PdTPBP), platinum tetraphenylporphyrin (PtTPBP), TPTBTBPPt, pdMesoIX, pdPh 4 One or two of the TBPs; the acceptor molecule comprises one or two of 9, 10-diphenyl anthracene (DPA), BODIPY, perylene, 9, 10-diphenyl anthracene-2-sodium sulfonate (DPAS) and 2-chloro-9, 10-xylyl anthracene (DTACl).
The solvent is one or two of ethanol, ethyl acetate, isopropanol, n-butanol, tert-butanol, toluene, n-hexane, petroleum ether, dichloromethane and deionized water.
3. Synthesis of Janus protective material with external heat and internal cooling
And adopting methods of spraying, spin coating, depositing and the like to respectively cover the photo-thermal material and the photo-cooling material on the two sides of the protective material in a coating mode to construct the antibacterial protective material with the Janus structure.
Wherein the solvent is one or two of ethanol, ethyl acetate, isopropanol, n-butanol, tert-butanol, toluene, n-hexane, petroleum ether, dichloromethane and deionized water.
The concentration of the photo-thermal material and the photo-cooling material in the solvent is 0.5-500 mg mL -1 。
The protective material substrate is one or two or three of polypropylene melt-blown cloth, polypropylene non-woven cloth, polyethylene melt-blown cloth, polypropylene spun-bonded cloth, spun-laced cloth compounded by polyester fiber and wood pulp, high polymer coated fabric, polyethylene non-woven cloth, polypropylene spun-bonded-melt-blown composite non-woven cloth, polyethylene spun-bonded-melt-blown-spun-bonded composite non-woven cloth, polypropylene-polyethylene melt-blown cloth and polypropylene-polyethylene blended non-woven cloth.
The Janus antibacterial protective material has the photo-thermal antibacterial performance that bacteria attached to the surface can be killed rapidly under the illumination condition, and the inhibition rate of gram-positive bacteria and gram-negative bacteria can reach more than 90%;
the Janus antibacterial protective material has the light cooling performance that the temperature difference of more than 5 ℃ exists between the inner layer and the outer layer attached with the up-conversion light cooling material while the outer layer is subjected to light-heat antibacterial.
In summary, the preparation method of the external heat and internal cold Janus antibacterial material with light responsiveness has the following advantages compared with the prior art:
1. the Janus medical protective material prepared by the invention has a double Janus structure in microcompositions and functions, wherein one surface of the Janus medical protective material is composed of a nano material with a photo-thermal effect, and the other surface of the Janus medical protective material is composed of an up-conversion material with a photo-cooling effect.
2. The Janus antibacterial functional material prepared by the invention has one surface composed of the nano material with the photo-thermal effect, and the other surface composed of the up-conversion material with the photo-cold effect, so that the photo-thermal antibacterial performance, the skin-friendly performance and the comfort of the inside can be considered under the illumination condition, the use experience of the protective material is greatly improved while the photo-thermal antibacterial effect is high, and the actual requirements of the biomedical technical field are met.
Drawings
FIG. 1 is an infrared imaging picture of the photo-thermal side of Janus polypropylene meltblown web prepared in example 1, with an optical density of 0.1W cm -2 The irradiation time was 2min.
FIG. 2 is an infrared imaging picture of a photo-cooled surface of Janus polypropylene melt-blown cloth prepared in example 1, having an optical density of 0.1W cm -2 The irradiation time was 2min.
FIG. 3 shows a photo-thermal antibacterial test of Streptococcus mutans by Janus polypropylene melt-blown cloth prepared in example 1, wherein the left side shows colony growth on the surface of the medium after irradiation with light, and the right side shows colony growth on the surface of the medium without irradiation with light, and the optical density is 0.1W cm -2 The irradiation time was 2min.
Detailed Description
The preparation method and the performance of the external heat and internal cold Janus antibacterial material with light responsiveness are further described below through specific examples.
Example 1
SnCl is added 2 ·2H 2 O and thioacetamide at 1:1 in the molar ratio, respectively dispersing uniformly in isopropanol, and magnetically stirring for 20min; then SnCl is added 2 ·2H 2 Uniformly mixing the dispersion liquid of O and thioacetamide, and magnetically stirring for 30min; transferring the mixed solution into a polytetrafluoroethylene reaction kettle liner, and performing solvothermal reaction for 12h at 160 ℃; and (3) after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing for three times by using distilled water and absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain the SnS nano-sheets.
Uniformly mixing 0.05g of CdO, 3.5g of tri-n-octylphosphino, 0.3g of octadecylphosphonic acid, 2.0g of trioctylphosphine and selenium simple substance by adopting a solvothermal method, and reacting for 5min at 370 ℃; cooling to room temperature after the reaction is finished, and fully washing at 10000rpm to obtain the CdSe quantum dot. The same method is adopted to obtain a CdTe@CdS@CdSe double-quantum dot system.
And dispersing the SnS nanosheets, the photo-thermal materials and the CdTe@CdS@CdSe quantum dots in isopropanol with the concentration of 1.0mg/mL, and respectively spraying the two materials on two sides of the polypropylene melt-blown cloth by adopting a pressure spray gun to obtain the external heat and internal cooling protective material with a Janus structure.
Example 2
PbCl is added 2 ·2H 2 O and thioacetamide at 1:1 in the molar ratio, respectively dispersing uniformly in isopropanol, and magnetically stirring for 20min; pbCl is then added 2 ·2H 2 Uniformly mixing the dispersion liquid of O and thioacetamide, and magnetically stirring for 30min; transferring the mixed solution into a polytetrafluoroethylene reaction kettle liner, and performing solvothermal reaction for 12h at 160 ℃; and (3) after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing for three times by using distilled water and absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain the PbS nano-sheet.
Uniformly mixing 0.05g of CdO, 3.5g of tri-n-octylphosphino, 0.3g of octadecylphosphonic acid, 2.0g of trioctylphosphine and selenium simple substance by adopting a solvothermal method, and reacting for 5min at 370 ℃; cooling to room temperature after the reaction is finished, and fully washing at 10000rpm to obtain the CdSe quantum dot. The same method is adopted to obtain a CdTe@CdS@CdSe double-quantum dot system.
Dispersing PbS nano-sheets, photo-thermal materials and CdTe@CdS@CdSe quantum dots in isopropanol with the concentration of 1.0mg/mL, and respectively spraying the two materials on two sides of polypropylene melt-blown cloth by adopting a pressure spray gun to obtain the external-heat and internal-cooling protective material with a Janus structure.
Example 3
SnCl is added 2 ·2H 2 O and thioacetamide at 1:1 in the molar ratio, respectively dispersing uniformly in isopropanol, and magnetically stirring for 20min; then SnCl is added 2 ·2H 2 Uniformly mixing the dispersion liquid of O and thioacetamide, and magnetically stirring for 30min; transferring the mixed solution into a polytetrafluoroethylene reaction kettle liner, and performing solvothermal reaction for 12h at 160 ℃; and (3) after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing for three times by using distilled water and absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain the SnS nano-sheets.
Uniformly mixing 0.05g of PbO, 3.5g of tri-n-octylphosphino, 0.3g of octadecylphosphonic acid, 2.0g of trioctylphosphine and selenium simple substance by adopting a solvothermal method, and reacting for 5min at 370 ℃; and cooling to room temperature after the reaction is finished, and fully washing at 10000rpm to obtain the PbSe quantum dots. By adopting the same method, a PbTe@PbS@PbSe double-quantum dot system is obtained.
And dispersing the SnS nanosheets, the photo-thermal materials and the PbTe@PbS@PbSe quantum dots in isopropanol with the concentration of 1.0mg/mL, and respectively spraying the two materials on two sides of polypropylene melt-blown cloth by adopting a pressure spray gun to obtain the external heat and internal cooling protective material with a Janus structure.
Example 4
SnCl is added 2 ·2H 2 O and thioacetamide at 1:1 in the molar ratio, respectively dispersing uniformly in isopropanol, and magnetically stirring for 20min; then SnCl is added 2 ·2H 2 Uniformly mixing the dispersion liquid of O and thioacetamide, and magnetically stirring for 30min; transferring the mixed solution into a polytetrafluoroethylene reaction kettle liner, and performing solvothermal reaction for 12h at 160 ℃; and (3) after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing for three times by using distilled water and absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain the SnS nano-sheets.
Uniformly mixing 0.05g of PbO, 3.5g of tri-n-octylphosphino, 0.3g of octadecylphosphonic acid, 2.0g of trioctylphosphine and selenium simple substance by adopting a solvothermal method, and reacting for 5min at 370 ℃; and cooling to room temperature after the reaction is finished, and fully washing at 10000rpm to obtain the PbSe quantum dots. By adopting the same method, a PbTe@PbS@PbSe double-quantum dot system is obtained.
And dispersing the SnS nanosheets, the photo-thermal materials and the PbTe@PbS@PbSe quantum dots in isopropanol with the concentration of 1.0mg/mL, and respectively spin-coating the two materials on two sides of polypropylene melt-blown cloth by adopting a spin-coating method to obtain the external heat and internal cooling protective material with a Janus structure.
Example 5
PbCl is added 2 ·2H 2 O and thioacetamide at 1:1 in the molar ratio, respectively dispersing uniformly in isopropanol, and magnetically stirring for 20min; pbCl is then added 2 ·2H 2 Uniformly mixing the dispersion liquid of O and thioacetamide, and magnetically stirring for 30min; transferring the mixed solutionTransferring the mixture into a polytetrafluoroethylene reaction kettle liner, and performing solvothermal reaction for 12 hours at 160 ℃; and (3) after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing for three times by using distilled water and absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain the PbS nano-sheet.
Uniformly mixing 0.05g of CdO, 3.5g of tri-n-octylphosphino, 0.3g of octadecylphosphonic acid, 2.0g of trioctylphosphine and selenium simple substance by adopting a solvothermal method, and reacting for 5min at 370 ℃; cooling to room temperature after the reaction is finished, and fully washing at 10000rpm to obtain the CdSe quantum dot. The same method is adopted to obtain a CdTe@CdS@CdSe double-quantum dot system.
Dispersing PbS nano-sheets, photo-thermal materials and CdTe@CdS@CdSe quantum dots in isopropanol with the concentration of 1.0mg/mL, and respectively spin-coating the two materials on two sides of polypropylene melt-blown cloth by adopting a spin-coating method to obtain the external heat and internal cooling protective material with a Janus structure.
Example 6
SnCl is added 2 ·2H 2 O and thioacetamide at 1:1 in the molar ratio, respectively dispersing uniformly in isopropanol, and magnetically stirring for 20min; then SnCl is added 2 ·2H 2 Uniformly mixing the dispersion liquid of O and thioacetamide, and magnetically stirring for 30min; transferring the mixed solution into a polytetrafluoroethylene reaction kettle liner, and performing solvothermal reaction for 12h at 160 ℃; and (3) after the reaction kettle is naturally cooled to room temperature, respectively centrifugally washing for three times by using distilled water and absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain the SnS nano-sheets.
Uniformly mixing 0.05g of CdO, 3.5g of tri-n-octylphosphino, 0.3g of octadecylphosphonic acid, 2.0g of trioctylphosphine and selenium simple substance by adopting a solvothermal method, and reacting for 5min at 370 ℃; cooling to room temperature after the reaction is finished, and fully washing at 10000rpm to obtain the CdSe quantum dot. The same method is adopted to obtain a CdTe@CdS@CdSe double-quantum dot system.
And dispersing the SnS nanosheets, the photo-thermal material and the CdTe@CdS@CdSe quantum dots in isopropanol with the concentration of 1.0mg/mL, and respectively spin-coating the two materials on two sides of the polypropylene melt-blown fabric by adopting a spin-coating method to obtain the external heat and internal cooling protective material with a Janus structure.
Performance evaluation was performed on the external hot and internal cold Janus polypropylene melt-blown cloth prepared in example 1:
1. evaluation of photo-thermal and photo-cooling properties of photo-thermal antibacterial Janus polypropylene meltblown cloth
The testing method comprises the following steps: adopting a 350W short-arc xenon lamp to simulate solar irradiation Janus polypropylene melt-blown cloth, wherein the energy density is 0.1-1.0W cm -2 The irradiation distance is 25cm; the change of the surface temperature of the super-hydrophobic sponge along with the irradiation time is recorded by using a ST 9450A+ type thermal imager of a sigma instrument, and the distance between the thermal imager and the sample is set to be 25cm.
FIG. 1 is an infrared imaging picture of the photo-thermal side of Janus polypropylene meltblown web prepared in example 1, with an optical density of 0.1W cm -2 The irradiation time was 2min.
FIG. 2 is an infrared imaging picture of a photo-cooled surface of Janus polypropylene melt-blown cloth prepared in example 1, having an optical density of 0.1W cm -2 The irradiation time was 2min.
2. Evaluation of antibacterial Property of Janus Polypropylene meltblown
The testing method comprises the following steps: 1) 1mL of 10 7 CFU mL -1 Dripping a concentration streptococcus mutans culture solution on the surface of the sterilized Janus polypropylene melt-blown cloth, and culturing for 3 hours at 37 ℃; 2) Washing the surface of the sample with sterilized water for 3 times; 3) Immersing the washed sample in 4mL of sterilized water, and performing ultrasonic treatment for 1min; 4) Taking 100 mu L of the ultrasonic solution, coating the solution on an agar plate, and culturing the solution in an environment of 37 ℃ for 24 hours; 5) Colonies on agar plates were photographed and counted.
Photothermal antibacterial experiment: after the above step 2), the reaction mixture was heated at 0.1W cm -2 The irradiation is carried out under the simulated sunlight for 1min, and the steps 3) to 5) are repeated.
FIG. 3 shows a photo-thermal antibacterial test of Janus antibacterial polypropylene melt-blown cloth prepared in example 1 on Streptococcus mutans, wherein the left side shows colony growth on the surface of the medium after illumination, and the right side shows colony growth on the surface of the medium without illumination. As can be seen from comparison, the Janus polypropylene melt-blown cloth surface after the light treatment is aseptic and colony growth exists on the Janus polypropylene melt-blown cloth surface without the light treatment, which proves that the Janus polypropylene melt-blown cloth prepared in the example 1 has excellent photo-thermal antibacterial capability.
Claims (10)
1. The external heat and internal cold Janus antibacterial material with the light responsiveness is characterized by having a microstructure and light responsiveness with different double surfaces, wherein one surface is coated with a light-heat functional material and has a light-heat antibacterial effect, and the other surface is coated with an up-conversion material and has an anti-Stokes fluorescent cooling effect.
2. A preparation method of an external heat and internal cold Janus antibacterial material with light responsiveness is characterized in that a solvothermal method is adopted to synthesize nano particles or QDs (quantum dots) with light-heat effect, namely a light-heat material; synthesizing an up-conversion material with a light cooling effect, namely a light cooling material by adopting a solvothermal method; and (3) respectively coating the photo-thermal material and the photo-cooling material on two sides of the protective material in a coating mode by adopting a spraying, spin coating or deposition method to construct the antibacterial protective material with a Janus structure.
3. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 2, which is characterized in that: the nanoparticle or QDs with photothermal effect is selected from purple phosphorus, black phosphorus, graphene oxide, graphite alkyne, carbon nanotube, au nanoparticle, ag nanoparticle, ti 3 C 2 T x Nanoplatelets, ti 2 CT x Nanosheets, V 2 CT x Nanoplatelets, nb 2 CT x Nanoplatelets, mo 2 CT x Nanosheets, cr 2 CT x Nanoplatelets, hf 2 CT x Nanoplatelets, ti 3 CNT x One or two or three of nano-sheets, bi QDs, se QDs, sb QDs, te QDs, agS QDs, snS nano-sheets, snSe nano-sheets, snTe nano-sheets, cdS QDs/nano-sheets, cdSe QDs/nano-sheets, cdTe QDs/nano-sheets, pbS QDs/nano-sheets, pbSe QDs/nano-sheets, pbTe QDs/nano-sheets, znS QDs/nano-sheets, znSe QDs/nano-sheets and ZnTe QDs/nano-sheets.
4. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 2, which is characterized in that: the up-conversion material with the light cooling effect is one or two or three of a rare earth up-conversion material, a semiconductor double-quantum dot system and an organic molecular system.
5. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 4, which is characterized in that: the rare earth up-conversion material consists of a matrix material, sensitizer ions, activator ions and doped metal cations, wherein the matrix material comprises fluoride, rare earth oxide, oxyfluoride, halide, oxyhalide and sulfur-containing compound; sensitizer ions comprising Yb 3+ And Nd 3+ The method comprises the steps of carrying out a first treatment on the surface of the Activator ions include Er 3+ 、Tm 3+ 、Ho 3+ The method comprises the steps of carrying out a first treatment on the surface of the Doped metal cations include Ba 2+ 、Bi 3+ 、Li + 、Na + 、Ca 2+ 、Sr 2+ 。
6. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 4, which is characterized in that: the semiconductor double-quantum dot system comprises an absorber, a potential barrier and a luminophor, wherein the absorber comprises one or two of CdS, cdSe, cdSe (Te), cdTe, pbS, pbSe, pbSe (Te), pbTe, znS, znSe, znSe (Te), znTe, snS, snSe, snSe (Te) and SnTe; the potential barrier comprises one or two or three of CdS, cdSe, cdSe (Te), cdTe, pbS, pbSe, pbSe (Te), pbTe, znS, znSe, znSe (Te), znTe, snS, snSe, snSe (Te) and SnTe; the illuminant includes one or two of CdS, cdSe, cdSe (Te), cdTe, pbS, pbSe, pbSe (Te), pbTe, znS, znSe, znSe (Te), znTe, snS, snSe, snSe (Te), and SnTe.
7. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 4, which is characterized in that: the organic molecular system comprises an energy donor molecule and a receptor molecule, wherein the donor molecule comprises platinum (II) -octaethylporphyrin (PtO)EP), palladium (II) -octaethylporphyrin (PdOEP), 5,10,15, 20-tetraphenylporphyrin palladium (PdPP), 5,10,15, 20-tetraphenylporphyrin platinum (PtTPP), pdTTP, palladium tetraphenylporphyrin (PdTMBP), platinum tetraphenylporphyrin (PtTPBP), TPTBTBPPt, pdMesoIX, pdPh 4 One or two of the TBPs; the acceptor molecule comprises one or two of 9, 10-diphenyl anthracene (DPA), BODIPY, perylene, 9, 10-diphenyl anthracene-2-sodium sulfonate (DPAS) and 2-chloro-9, 10-xylyl anthracene (DTACl).
8. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 2, which is characterized in that: the photo-thermal material and the photo-cooling material are respectively attached to the two sides of the protective material in the form of a coating, and the solvent required for forming the coating is one or two of ethanol, ethyl acetate, isopropanol, n-butanol, tertiary butanol, toluene, n-hexane, petroleum ether, methylene dichloride and deionized water; the concentration of the photo-thermal material and the photo-cooling material in the solvent is 0.5-500 mg mL -1 。
9. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 2, which is characterized in that: the substrate of the protective material is one or two or three of polypropylene melt-blown cloth, polypropylene non-woven cloth, polyethylene melt-blown cloth, polypropylene spun-bonded cloth, spun-laced cloth compounded by polyester fiber and wood pulp, high polymer coated fabric, polyethylene non-woven cloth, polypropylene spun-bonded-melt-blown composite non-woven cloth, polyethylene spun-bonded-melt-blown-spun-bonded composite non-woven cloth, polypropylene-polyethylene melt-blown cloth and polypropylene-polyethylene blended non-woven cloth.
10. The method for preparing the external heat and internal cold Janus antibacterial material with light responsiveness as claimed in claim 2, which is characterized in that: the Janus antibacterial protective material has the photo-thermal antibacterial performance that bacteria attached to the surface can be killed rapidly under the illumination condition, and the inhibition rate of gram-positive bacteria and gram-negative bacteria can reach more than 90%;
the Janus antibacterial protective material has the light cooling performance that the temperature difference of more than 5 ℃ exists between the inner layer and the outer layer attached with the up-conversion light cooling material while the outer layer is subjected to light-heat antibacterial.
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