CN114907771B - Sterilization type coating precursor and preparation method and application thereof - Google Patents
Sterilization type coating precursor and preparation method and application thereof Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 94
- 239000002243 precursor Substances 0.000 title claims abstract description 36
- 238000004659 sterilization and disinfection Methods 0.000 title claims abstract description 33
- 230000001954 sterilising effect Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 59
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- 238000000034 method Methods 0.000 claims abstract description 26
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 239000002114 nanocomposite Substances 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
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- 239000000243 solution Substances 0.000 claims description 24
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 22
- BNCPSJBACSAPHV-UHFFFAOYSA-N (2-oxo-1h-pyrimidin-6-yl)urea Chemical compound NC(=O)NC=1C=CNC(=O)N=1 BNCPSJBACSAPHV-UHFFFAOYSA-N 0.000 claims description 18
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- JORAUNFTUVJTNG-BSTBCYLQSA-N n-[(2s)-4-amino-1-[[(2s,3r)-1-[[(2s)-4-amino-1-oxo-1-[[(3s,6s,9s,12s,15r,18s,21s)-6,9,18-tris(2-aminoethyl)-3-[(1r)-1-hydroxyethyl]-12,15-bis(2-methylpropyl)-2,5,8,11,14,17,20-heptaoxo-1,4,7,10,13,16,19-heptazacyclotricos-21-yl]amino]butan-2-yl]amino]-3-h Chemical compound CC(C)CCCCC(=O)N[C@@H](CCN)C(=O)N[C@H]([C@@H](C)O)CN[C@@H](CCN)C(=O)N[C@H]1CCNC(=O)[C@H]([C@@H](C)O)NC(=O)[C@H](CCN)NC(=O)[C@H](CCN)NC(=O)[C@H](CC(C)C)NC(=O)[C@@H](CC(C)C)NC(=O)[C@H](CCN)NC1=O.CCC(C)CCCCC(=O)N[C@@H](CCN)C(=O)N[C@H]([C@@H](C)O)CN[C@@H](CCN)C(=O)N[C@H]1CCNC(=O)[C@H]([C@@H](C)O)NC(=O)[C@H](CCN)NC(=O)[C@H](CCN)NC(=O)[C@H](CC(C)C)NC(=O)[C@@H](CC(C)C)NC(=O)[C@H](CCN)NC1=O JORAUNFTUVJTNG-BSTBCYLQSA-N 0.000 description 1
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- XDJYMJULXQKGMM-UHFFFAOYSA-N polymyxin E1 Natural products CCC(C)CCCCC(=O)NC(CCN)C(=O)NC(C(C)O)C(=O)NC(CCN)C(=O)NC1CCNC(=O)C(C(C)O)NC(=O)C(CCN)NC(=O)C(CCN)NC(=O)C(CC(C)C)NC(=O)C(CC(C)C)NC(=O)C(CCN)NC1=O XDJYMJULXQKGMM-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention provides a sterilization type coating precursor and a preparation method and application thereof. The preparation method comprises the following steps: silica-coated metal nanoparticlesRice grain GNRs @ SiO 2 Carboxylation treatment to obtain carboxylated GNRs @ SiO 2 (ii) a UPy-PDMS modified carboxylated GNRs @ SiO 2 Obtaining GNRs @ SiO 2 -PDMS-UPy; mixing GNRs @ SiO 2 -mixing PDMS-UPy with UPy-PDMS-UPy to obtain a sterile coating precursor. The coating precursor of the present invention is pressed on a substrate to obtain a nanocomposite coating having excellent sterilization efficiency. The present invention also provides a simple and effective sterilization process using the above-described sterilization-type coating precursor.
Description
Technical Field
The invention relates to a preparation method of a composite coating, in particular to a press-ready sterilization type nano composite coating, and belongs to the technical field of coating materials.
Background
The air transmission and the contact transmission are important modes for the transmission of pathogenic microorganisms between the environment and a host, and the application of the antibacterial and antiviral coating can effectively block the transmission path of the pathogenic microorganisms, thereby realizing the control and the prevention of infectious diseases. The currently widely used antibacterial and antiviral coatings mainly rely on chemical or biological inactivation mechanisms, have high cost and poor durability, and have insufficient performance in practical application (CN 104004392B). Meanwhile, chemical or biological inactivation components used in the coating not only bring certain environmental pollution risks, but also may cause the spread of drug-resistant bacteria after long-term use. Therefore, the coating based on physical killing mechanisms such as biomolecule heat inactivation and the like is prepared, a convenient use method and an ultra-fast action mechanism are endowed, the vacancy of the conventional disinfection strategy at present can be filled, and the control and prevention of pathogenic microorganisms and infectious diseases are enhanced.
Disclosure of Invention
In order to solve the problems of the prior art, it is an object of the present invention to provide a coating having excellent sterilization properties.
In order to achieve the above technical object, the present invention firstly provides a method for preparing a sterilization-type coating precursor, the method comprising:
for silicon dioxide coated metal nanoparticles GNRs @ SiO 2 Performing carboxylation treatment to obtain carboxylChemically GNRs @ SiO 2 ；
Modified carboxylated GNRs @ SiO with ureido pyrimidone mono-terminated polydimethylsiloxane UPy-PDMS at 20-40 DEG C 2 Obtaining GNRs @ SiO 2 -PDMS-UPy；
Coupling GNRs @ SiO 2 -PDMS-UPy is mixed with ureidopyrimidone bis-blocked polydimethylsiloxane UPy-PDMS-UPy to obtain a sterile coating precursor; wherein, GNRs @ SiO 2 Mass ratio of PDMS-UPy to UPy-PDMS-UPy is 1-1.
The preparation method of the sterilization type coating precursor of the invention specifically comprises the following steps:
preparation of silica-coated Metal nanoparticle rods GNRs @ SiO 2 From GNRs @ SiO 2 Carboxylation treatment to obtain carboxylated GNRs @ SiO 2 ；
Preparing ureido pyrimidone single-end-capped polydimethylsiloxane UPy-PDMS and ureido pyrimidone double-end-capped polydimethylsiloxane UPy-PDMS-UPy;
UPy-PDMS modified carboxylated GNRs @ SiO 2 Obtaining GNRs @ SiO 2 -PDMS-UPy；
Coupling GNRs @ SiO 2 -mixing PDMS-UPy with UPy-PDMS-UPy to obtain a sterile coating precursor.
In the preparation method of the invention, the preparation method comprises the steps of preparing the metal nano-particles covered by silicon dioxide, GNRs @ SiO 2 Step (2). In one embodiment of the present invention, GNRs @ SiO 2 The adopted metal is gold nanorods, molybdenum disulfide nanoparticles or ferroferric oxide nanoparticles; preferably gold nanorods.
Taking a gold nanorod as an example, the gold nanorod wrapped by silicon dioxide is prepared according to the following steps:
10mL of 0.1mol/L cetyltrimethylammonium bromide (CTAB) and 250. Mu.L of 0.01mol/L chloroauric acid (HAuCl) 4 ) The aqueous solutions were mixed and then 600. Mu.L of 0.01mol/L sodium borohydride was added to give a brownish yellow solution, which was finally stirred for 5 minutes and left to stand at 25 ℃ for 3 hours to give a seed solution. In addition, to 30mL of a 0.1mol/L CTAB solution, 1.2mL of 0.01 was addedmol/L HAuCl 4 An aqueous solution, and then 160. Mu.L of a 0.01mol/L silver nitrate solution and 240. Mu.L of ascorbic acid were rapidly added thereto to obtain a growth solution. Subsequently, 60. Mu.L of the seed solution was added to the growth solution and mixed well, and left to stand for 24 hours to obtain a GNRs solution. Finally, the GNRs were obtained by centrifugation at 12000 rpm for 15 minutes and three water washes.
After the GNRs were dispersed in 10mL of water, 10. Mu.L of 0.1mol/L sodium hydroxide was added. Subsequently, 100. Mu.L of ethyl orthosilicate (10% by mass) dissolved in methanol was added and reacted for 12 hours with stirring at normal temperature. After the reaction, centrifugation was carried out at 12000 rpm for 15 minutes and the precipitate was washed with water and ethanol three times each to give GNRs @ SiO 2 。
In the preparation method of the invention, the preparation method comprises the following steps of coating silicon dioxide with metal nano particles GNRs @ SiO 2 A step of performing carboxylation treatment.
15mg of GNRs @ SiO 2 Dispersed in 10mL of ethanol, and reacted with 0.5mL of 3-Aminopropyltriethoxysilane (APTMS) and 50. Mu.L of acetic acid for 12 hours. Repeated washing of APTMS-modified GNRs @ SiO with deionized water 2 To remove excess APTMS. Finally, a solution of succinic acid (10% by mass) in dimethylformamide was added thereto and reacted for 12 hours under a nitrogen atmosphere. Centrifuging at 12000 rpm for 15 min and washing with water to precipitate three times to obtain carboxylated GNRs @ SiO 2 。
The preparation method comprises the step of respectively preparing ureido pyrimidone mono-terminated polydimethylsiloxane UPy-PDMS and ureido pyrimidone di-terminated polydimethylsiloxane UPy-PDMS-UPy.
Wherein, 4' -dicyclohexylmethane diisocyanate is connected with ureido pyrimidone (UPy) to obtain UPy-NCO, then the UPy-NCO reacts with amino double-end-capped polydimethylsiloxane (with different molecular weights), and UPy single-end-capped PDMS (UPy-PDMS) and UPy double-end-capped PDMS (UPy-PDMS-UPy) are prepared by regulating and controlling the feeding molar ratio of reactants (UPy-NCO: PDMS). Wherein the charging molar ratio for preparing UPy-PDMS is 1.
In the inventionThe preparation method comprises the step of modifying carboxylated GNRs @ SiO by an amidation reaction through UPy-PDMS 2 Preparation of GNRs @ SiO 2 -PDMS-UPy.
In one embodiment of the present invention, GNRs @ SiO 2 The preparation method of the PDMS-UPy comprises the following steps:
carboxylation of GNRs @ SiO 2 Dispersing in DMSO, adding excessive activating agent, and activating for 30-120 min to obtain mixed solution; wherein, carboxylated GNRs @ SiO 2 The mixing ratio with DMSO was 30.2mg: (10-200) mL;
adding DMSO solution containing 100mg-1000mg UPy-PDMS dropwise into the mixed solution, stirring vigorously at 50-1000 rpm for 12-36 hr (preferably 24 hr), centrifuging, washing, precipitating, and vacuum drying to obtain GNRs @ SiO 2 -PDMS-UPy。
In one embodiment of the present invention, the DMSO solution containing 100mg to 1000mg of UPy-PDMS is not particularly limited, as long as it contains UPy-PDMS, and the amount of DMSO is determined by one skilled in the art.
In one embodiment of the present invention, the activating agent used comprises one or a combination of two or more of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, dicyclohexylcarbodiimide, N' -diisopropylcarbodiimide and N-hydroxysuccinimide.
In one embodiment of the present invention, UPy-PDMS modified carboxylated GNRs @ SiO with different molecular weights is used 2 . Wherein, the difference of the molecular weight of PDMS in UPy-PDMS with different molecular weight leads to the difference of the molecular weight of UPy-PDMS, and the molecular weight of UPy is fixed. The PDMS in the UPy-PDMS with different molecular weights is one or the combination of more than two of PDMS with the number average molecular weight of 100-10000. The PDMS in UPy-PDMS with different molecular weight is preferably one or the combination of more than two of PDMS with the number average molecular weight of 870-3000.
In one embodiment of the present invention, carboxylated GNRs @ SiO 2 And the mass ratio of UPy-PDMS is 1.
In the inventionIn one embodiment, GNRs @ SiO is prepared 2 When PDMS-UPy is adopted, the rotation speed of centrifugation is 1000-20000 rpm, and the time of centrifugation is 10-60 min. After centrifugation, the precipitate was washed repeatedly with chloroform and water.
In the preparation method of the invention, GNRs @ SiO 2 -a step of mixing PDMS-UPy and UPy-PDMS-UPy to prepare a sterile coating precursor.
In one embodiment of the present invention, GNRs @ SiO 2 -mixing PDMS-UPy with UPy-PDMS-UPy, comprising the steps of:
mixing GNRs @ SiO 2 And ultrasonically dispersing PDMS-UPy and UPy-PDMS-UPy in DMSO respectively to obtain respective dispersion liquid, mixing the two dispersion liquids, violently stirring at the rotating speed of 50-1000 rpm for 1-10 hours, centrifuging, washing and vacuum drying to obtain the sterile coating precursor.
In one embodiment of the present invention, GNRs @ SiO 2 The mixing mass ratio of PDMS-UPy to UPy-PDMS-UPy is 12:0.01-1000.GNRs @ SiO 2 -the mixing ratio of PDMS-UPy to DMSO is 12mg: (10-200) mL; the mixing ratio of UPy-PDMS-UPy to DMSO is (0.01-1000) mg: (10-200) mL.
In one embodiment of the present invention, the number average molecular weight of PDMS in the UPy-PDMS-UPy as a cross-linking agent (CLs) is 3000 or 5000.
In one embodiment of the invention, the dispersion is mixed and centrifuged at a speed of 50 to 20000 rpm for a period of 5 to 60 minutes. The pellet after centrifugation was washed repeatedly with water to remove residual DMSO.
The invention also provides a sterilized coating precursor prepared by the preparation method of the sterilized coating precursor.
The invention also provides a press-and-play nanocomposite coating obtained by pressing the biocidal coating precursor of the invention onto a substrate surface.
In one embodiment of the invention, 2mg to 100mg of the sterilization-type coating precursor is pressed onto a substrate at a pressure of 1KPa to 100KPa to produce a coating having a thickness of 50 microns to 200 microns. Wherein, the substrate can be medical gloves, fabrics, glassware, plastics or metals, etc.
After the press-ready nano composite coating is irradiated for 6 seconds under the infrared light with the wavelength of 808 nanometers and the power of 0.5 watt/square centimeter, the sterilization efficiency exceeds 99.9 percent, and after the infrared light is irradiated for 6 seconds again, the sterilization efficiency can be improved to 99.9999 percent.
The present invention also provides a method of sterilization by the sterile coating precursor of the invention.
In one embodiment of the present invention, the sterilization method comprises the steps of:
the sterilization-type coating precursor of the present invention is pressed against a substrate to be sterilized to form a coating, and the coating is irradiated by infrared light to complete sterilization of the substrate.
In one embodiment of the invention, the sterilization treatment is carried out by pressing 2mg to 100mg of the sterilization-type coating precursor at a pressure of 1KPa to 100KPa against the substrate to be sterilized to produce a coating having a thickness of 50 microns to 200 microns.
According to the sterilization method, the sterilization type coating precursor is pressed on the substrate, after the substrate is irradiated for 6 seconds under the infrared light with the wavelength of 808 nanometers and the power of 0.5 watt/square centimeter, the sterilization efficiency exceeds 99.9%, and after the substrate is irradiated for 6 seconds again, the sterilization efficiency can be improved to 99.9999%.
The sterilization type coating precursor and the pressing ready-to-use nano composite coating can realize rapid sterilization under the assistance of photo-thermal. Compared with other traditional antibacterial and antiviral coatings, the coating has the advantages of simple material synthesis route, low raw material price, convenient preparation method, good photo-thermal disinfection effect and obvious advantages.
The preparation method of the sterilization type coating precursor has the advantages of simple synthetic route, low raw material price, convenient preparation method, good photo-thermal disinfection effect of the formed coating and wide market application prospect.
Drawings
FIG. 1a is a diagram of GNRs @ SiO of example 1 of the present invention 2 PDMS-UPy and UImage of powder and coating after Py-PDMS-UPy mixing.
FIG. 1b shows GnRs @ SiO after pressing in example 1 of the present invention 2 Rheological test curves of PDMS-UPy.
FIG. 2a shows GNRs @ SiO of example 1 of the present invention 2 Strain scans (0.1 hz,25 ℃) of PDMS-UPy after forming coatings with crosslinkers of different molecular weights.
FIG. 2b shows GNRs @ SiO of example 1 of the present invention 2 Modulus profile of PDMS-UPy after 15KPa compression.
FIG. 2c is a graph of GNRs @ SiO in example 1 of the present invention 2 Adhesion distribution of PDMS-UPy after 15KPa pressing.
FIG. 3a is a graph showing the temperature change and cooling profile of the coating on the glass substrate and glass of example 1 of the present invention under 60 seconds of near infrared irradiation.
FIG. 3b is a graph of the change in surface temperature of the coating of example 1 of the present invention over five 6 second light ramp-cool cycles.
Fig. 3c shows the results of the experiment of the coating of example 1 against five drug-resistant bacteria, wherein the sterilization efficiency is repeated after 6 seconds of irradiation with near infrared light (0.5 w/cm, 808 nm).
FIG. 3d shows the sterilization efficiency after another 6 seconds of irradiation of the coating of example 1 according to the invention.
Fig. 4a is a schematic view of the preparation of a press-and-play nanocomposite coating according to example 1 of the invention.
FIG. 4b is a graph of the strain tolerance of the coating of example 1 of the present invention to finger bending.
FIG. 4c shows that the coating of example 1 of the present invention can withstand the impact of water flow, and black arrows indicate the coating.
FIG. 4d shows that the coating of example 1 of the present invention is not damaged in normal use.
Fig. 4e shows the coating of example 1 of the invention after 40 cycles of the stick-peel test on a standard tape Elcometer 99.
FIG. 4f is an image of the temperature change of the outside of the glove at the coated finger after 6 seconds of near infrared illumination and the temperature change of the inside of the glove at the finger of example 1 of the present invention.
FIG. 4g is a graph of the temperature change of the outside of the glove at the fingers after 6 seconds of NIR irradiation and the temperature change of the inside of the glove at the fingers for a coating of example 1 in accordance with the present invention.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The embodiment provides a press-and-play nanocomposite coating, which is realized by the following specific steps:
30.2mg of carboxylated GNRs @ SiO 2 Dispersed in 20ml of DMSO and then activated for 60 minutes by adding 139mg of an activating agent (100 mg of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 39mg of N-hydroxysuccinimide). After activation, the solution containing 500mgUPy-PDMS x (x represents the number average molecular weight of PDMS; x is 870) was added dropwise to the above solution, followed by vigorous stirring for 24 hours. After the reaction was completed, the above product was centrifuged at 12000 rpm for 30 minutes, and the precipitate was repeatedly washed with chloroform and water. Finally the product obtained is dried in vacuum to obtain GNRs @ SiO 2 -PDMS-UPy。
12mg of GNRs @ SiO 2 PDMS-UPy and 97mgUPy-PDMS as a cross-linking agent x UPy (x represents the number average molecular weight of PDMS; x is 5000) is dispersed by sonication in 20mL of DMSO, respectively. They were then mixed and stirred vigorously for 5 hours. The homogeneously mixed product was centrifuged at 3000 rpm for 15 minutes, and the precipitate obtained after centrifugation was washed with water several times to remove residual DMSO. Finally, the above product was vacuum dried to obtain a precursor powder.
The powder allows for the rapid preparation of coatings of about 70 microns thickness on various surfaces (e.g., medical gloves) at 15 KPa.
Wherein, the gold nanorods wrapped by silicon dioxide GNRs @ SiO 2 The preparation method comprises the following steps:
10mL of 0.1mol/L hexadecyl groupTrimethyl Ammonium Bromide (CTAB) with 250. Mu.L of 0.01mol/L chloroauric acid (HAuCl) 4 ) The aqueous solutions were mixed and 600. Mu.L of 0.01mol/L sodium borohydride was added to give a brown-yellow solution which was finally stirred for 5 minutes and left to stand at 25 ℃ for 3 hours to give a seed solution. In addition, 1.2mL of 0.01mol/L HAuCl was added to 30mL of 0.1mol/L CTAB solution 4 An aqueous solution, and then 160. Mu.L of a 0.01mol/L silver nitrate solution and 240. Mu.L of ascorbic acid were rapidly added thereto to obtain a growth solution. Subsequently, 60. Mu.L of the seed solution was added to the growth solution and mixed well, and left to stand for 24 hours to obtain a GNRs solution. Finally, centrifugation was carried out at 12000 rpm for 15 minutes and the pellet was washed three times with water to obtain GNRs.
After the GNRs were dispersed in 10mL of water, 10. Mu.L of 0.1mol/L sodium hydroxide was added. Subsequently, 100. Mu.L of ethyl orthosilicate (10% by mass) dissolved in methanol was added and reacted for 12 hours with stirring at normal temperature. After the reaction, centrifugation was carried out at 12000 rpm for 15 minutes and the precipitate was washed with water and ethanol three times each to give GNRs @ SiO 2 。
Silicon dioxide coated metal nanoparticles GNRs @ SiO 2 And (3) performing carboxylation treatment.
15mg of GNRs @ SiO 2 Dispersed in 10mL of ethanol, and then reacted with 0.5mL of 3-Aminopropyltriethoxysilane (APTMS) and 50. Mu.L of acetic acid for 12 hours. Then repeatedly washing APTMS modified GNRs @ SiO by deionized water 2 To remove excess APTMS. Finally, a solution of succinic acid (10% by mass) in dimethylformamide was added and reacted for 12 hours under nitrogen. Centrifuging at 12000 rpm for 15 min and washing with water to precipitate three times to obtain carboxylated GNRs @ SiO 2 。
Connecting 4,4' -dicyclohexylmethane diisocyanate with ureido pyrimidone (UPy) to obtain UPy-NCO, reacting with amino double-terminated polydimethylsiloxane with different molecular weights, and preparing UPy single-terminated PDMS (UPy-PDMS) and UPy double-terminated PDMS (UPy-PDMS-UPy) by regulating and controlling the feeding molar ratio of reactants (UPy-NCO: PDMS). Wherein the charging molar ratio for preparing UPy-PDMS is 1.
All figures below show the results for example 1 of the present invention, except that in FIG. 1b, FIG. 2b and FIG. 2c only GNRs @ SiO were tested 2 PDMS-UPy (PDMS number average molecular weight 870) and FIG. 2a compares GNRs @ SiO 2 PDMS-UPy with different molecular weight crosslinkers in a mass ratio of 1 to 8, all the figures below show GNRs @ SiO 2 And (3) uniformly mixing PDMS-UPy (the PDMS number average molecular weight is 870) and UPy-PDMS-UPy (the PDMS number average molecular weight is 5000) at a mass ratio of 1.
Figure 1a shows an image of a powder and a coating that can be rapidly prepared on the surface by pressing the precursor powder, while the coating can be recovered from the powder after ultrasonic pulverization in acetone. TEM picture shows GNRs @ SiO 2 And the micro-morphology of the powder. The scale bar is 100 nm.
FIG. 1b shows GnRs @ SiO after pressing 2 Rheological testing of PDMS-UPy, indicating GNRs @ SiO 2 The PDMS-UPy interaction is destroyed at 1% strain (0.1Hz, 25 ℃) and recovers after removal of the strain (0.1Hz, 50 ℃), thus exhibiting repairability.
The strain sweep of FIG. 2a (0.1 Hz,25 ℃) shows: crosslinkers (CLs) of different molecular weights can modulate the mechanical properties of the coating. In which GNRs @ SiO without CLs 2 PDMS-UPy has the highest storage modulus, but its strain tolerance is the weakest; while the coatings incorporating a 5000 molecular weight crosslinker (CLs-5000) had the best strain tolerance and higher storage modulus, and were suitable for coating applications.
FIGS. 2b and 2c show GNRs @ SiO without CLs 2 -modulus and adhesion profile of PDMS-UPy press-formed coating at 15 KPa; the inset is an image of the modulus and adhesion obtained by atomic force microscopy (area: 5 μm. Times.5 μm). The graph shows that the coating produced after pressing has a high hardness and a high adhesion.
Fig. 3a shows the temperature change of the coating on the glass substrate and the glass under 60 seconds of near infrared light irradiation (808 nm, 0.5 w/cm) and the cooling process thereof, indicating that the coating has excellent photothermal effect.
Fig. 3b shows the temperature change of the coating after five cycles of 6 seconds of light exposure, temperature ramp-cool, indicating that the coating has good light stability.
Fig. 3c shows that for five drug-resistant bacteria, the repeated sterilization efficiency is over 99.9% after 6 seconds of irradiation by near infrared light (0.5 w/cm, 808 nm). Wherein the MRSA is methicillin-resistant Staphylococcus aureus; CREC is carbapenem-resistant E.coli; CRAP is carbapenem-resistant acinetobacter; CRKP is carbapenem-resistant Klebsiella pneumoniae; CCRKP is carbapenem-and colistin-resistant Klebsiella pneumoniae.
Figure 3d shows that the sterilization efficiency can be increased to 99.9999% after 6 seconds of re-irradiation.
Figure 4a gives a schematic representation of the preparation of a press-and-play nanocomposite coating.
Figure 4b shows the strain tolerance of the coating to finger bending. The specific implementation was to press 6.5mg of the precursor powder at 15KPa onto the glove to form a coating. When the finger joint is flexed, the coating can tolerate the stretching of the finger joint and still adhere to the glove without breaking or falling off.
Fig. 4c shows that the coating can withstand the impact of a water stream (2bar, 10 minutes) and the black arrows indicate the coating. The specific implementation was to press 6.5mg of the precursor powder at 15KPa to form the coating at each finger. The water pressure was then adjusted to 2bar and the resulting coating was subjected to water impingement for 10 minutes, and it was found that the coating remained adhered to the glove without being damaged or falling off.
Figure 4d shows that the coating is not damaged in normal use. The specific implementation was to press 6.5mg of the precursor powder at 15KPa to form the coating at each finger. Then, the coated fingers were handled normally by taking the beaker and putting it in water, and it could be found that there was no coating left on the beaker and the coating remained adhered to the glove.
Figure 4e shows that the coating remains intact after 40 cycles of the stick-peel test of a standard tape Elcometer 99. A specific operation is to roll a 1 kg weight on a tape and then peel it off.
Figure 4f shows the temperature change image of the outside of the glove at the finger after 6 seconds of near infrared light (808 nm, 0.5 watts per square centimeter) exposure and the temperature change image of the inside of the glove at the finger, indicating that the coated glove achieved efficient sterilization within 6 seconds after being contaminated and that the fingers inside the glove maintained a comfortable temperature.
Fig. 4g shows the temperature profile of the outside of the glove at the fingers after 6 seconds of near infrared irradiation and the temperature profile of the inside of the glove at the fingers. Indicating that the outside of the glove is highly sterilizable before and after 6 seconds of light exposure while the inside of the glove maintains a relatively comfortable temperature range for the fingers.
Claims (21)
1. A method of preparing a sterilization-type coating precursor, wherein the method of preparing comprises:
for silicon dioxide coated metal nanoparticles GNRs @ SiO 2 Carboxylation treatment to obtain carboxylated GNRs @ SiO 2 ；
Modified carboxylated GNRs @ SiO by ureido pyrimidone mono-terminated polydimethylsiloxane UPy-PDMS at 20-40 DEG C 2 Obtaining GNRs @ SiO 2 -PDMS-UPy；
Mixing GNRs @ SiO 2 -PDMS-UPy is mixed with ureidopyrimidone bis-blocked polydimethylsiloxane UPy-PDMS-UPy to obtain a sterile coating precursor; GNRs @ SiO 2 -the mass ratio of PDMS-UPy to UPy-PDMS-UPy is 1-1;
wherein, GNRs @ SiO is prepared 2 PDMS-UPy, according to the following steps:
carboxylation of GNRs @ SiO 2 Dispersing in DMSO, adding excessive activating agent, and activating for 30-120 min to obtain mixed solution; among them, carboxylated GNRs @ SiO 2 The mixing ratio with DMSO was 30.2mg: (10-200) mL; the activating agent comprises one or the combination of more than two of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, dicyclohexylcarbodiimide, N' -diisopropylcarbodiimide and N-hydroxysuccinimide;
will contain 100mg-1000The DMSO solution of mgUPy-PDMS is dripped into the mixed solution, stirred for 12-36 hours at the rotating speed of 50-1000 r/min, and then centrifuged, washed, precipitated and vacuum dried to obtain the GNRs @ SiO 2 -PDMS-UPy。
2. The method of claim 1, wherein the UPy-PDMS is UPy-PDMS of different molecular weights.
3. The method according to claim 2, wherein the PDMS of the UPy-PDMS having different molecular weights is one or a combination of two or more of PDMS having a number average molecular weight of 100-10000.
4. The method according to claim 3, wherein the PDMS of the UPy-PDMS having different molecular weights is one or a combination of two or more of PDMS having a number average molecular weight of 870-3000.
5. The process according to claim 1, wherein the carboxylated GNRs @ SiO 2 And the mass ratio of UPy-PDMS is 1.
6. The process according to claim 5, wherein the carboxylated GNRs @ SiO 2 And the mass ratio of UPy-PDMS is 1.
7. The method for preparing claim 1, wherein the rotation speed of the centrifugation is 1000 rpm to 20000 rpm, and the time of the centrifugation is 10min to 60min.
8. The process according to claim 1, wherein GNRs @ SiO 2 -PDMS-UPy when mixed with UPy-PDMS-UPy, comprising the steps of:
mixing GNRs @ SiO 2 Ultrasonic dispersing PDMS-UPy and UPy-PDMS-UPy in DMSO to obtain respective dispersion, mixing the dispersions, stirring at 50-1000 rpm for 1-10 hr, centrifuging, washing, and vacuum dryingDrying to obtain a sterile coating precursor;
GNRs@SiO 2 the mixing mass ratio of PDMS-UPy to UPy-PDMS-UPy is 12:0.01-1000.
9. The method of claim 8, wherein GNRs @ SiO 2 -the mixing ratio of PDMS-UPy to DMSO is 12mg: (10-200) mL.
10. The preparation method of claim 8, wherein the mixing ratio of UPy-PDMS-UPy to DMSO is (0.01-1000) mg: (10-200) mL.
11. The method of claim 8, wherein the number average molecular weight of the PDMS used in UPy-PDMS-UPy is 3000 or 5000.
12. The method of claim 8, wherein the centrifugation is performed at a speed of 50 rpm to 20000 rpm for a period of 5 minutes to 60 minutes.
13. The method of claim 1, wherein the gnrs @ sio 2 The adopted metal is gold nanorod, molybdenum disulfide nano particle or ferroferric oxide nano particle.
14. The method of claim 13, wherein the gnrs @ sio 2 The adopted metal is gold nanorods.
15. A sterilized coating precursor prepared by the method of any one of claims 1 to 14.
16. A press-and-play nanocomposite coating obtained by pressing the sterilized coating precursor of claim 15 on a substrate.
17. The press-to-use nanocomposite coating according to claim 16, wherein 2mg to 100mg of the sterilized coating precursor is pressed onto a substrate at a pressure of 1KPa to 100KPa to produce a coating having a thickness of 50 microns to 200 microns, i.e. the press-to-use nanocomposite coating.
18. The press-to-use nanocomposite coating according to claim 16, wherein said substrate is a medical glove, a fabric, a glassware, a plastic, or a metal.
19. A method of sterilization by the sterilization-type coating precursor of claim 15.
20. Sterilization process according to claim 19, wherein it comprises the following steps:
and pressing the sterilizing coating precursor on a substrate to be sterilized to form a coating, and irradiating the coating for 6 seconds under the infrared light with the wavelength of 808 nanometers and the power of 0.5 watt/square centimeter to finish the sterilization treatment.
21. Sterilization process according to claim 20, wherein 2mg-100mg of the sterilization-type coating precursor is pressed at a pressure of 1KPa-100KPa on a substrate to be sterilized, producing a coating with a thickness of 50-200 microns.
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