CN113088170A - Efficient and durable monoatomic antibacterial and antiviral spray coating and preparation method thereof - Google Patents
Efficient and durable monoatomic antibacterial and antiviral spray coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of antibacterial and antiviral functional coatings, and particularly discloses a high-efficiency and durable monoatomic antibacterial and antiviral spray coating and a preparation method thereof. A high-efficiency and durable single-atom antibacterial and antiviral spray coating is prepared from the following raw materials in percentage by mass: 5-10% of monoatomic antibacterial antiviral catalyst, 2-25% of water-based polyurethane, 1-5% of nonionic dispersant, 1-5% of defoaming agent, 4-5% of organic silicon base material wetting agent, 1-5% of film-forming assistant, 0.5-2% of pH regulator and 20-60% of deionized water. The invention uses the independently developed monoatomic antibacterial and antiviral catalyst, does not need other auxiliary conditions, can kill common bacterial viruses in a broad spectrum, can also quickly and continuously kill super bacteria, has the lasting action time of more than 10 years, does not generate any drug resistance, has the advantages of broad-spectrum antibacterial, high-efficiency disinfection, long-acting mildew resistance, no odor, no toxicity, environmental protection and the like, and can be portably sprayed on application scenes such as walls, floors, sofas and the like.
Description
Technical Field
The application relates to the field of antibacterial and antiviral functional coatings, in particular to a high-efficiency and durable monoatomic antibacterial and antiviral spray coating and a preparation method thereof.
Background
Bacteria (such as escherichia coli, staphylococcus aureus and the like) and viruses (such as enterovirus 71, influenza A H3N2, influenza A H1N1 and the like) are ubiquitous in daily life, and are harmful bacteria and viruses with various and large quantities in nature, so that the life health of people is greatly threatened, and the demand of people on antibacterial and antiviral products is increased. Therefore, the development of broad-spectrum and efficient antibacterial and antiviral spray coatings which can be applied to a plurality of application scenes is the most urgent issue at present.
Disclosure of Invention
In order to overcome the defects in the related art, the application aims to provide a high-efficiency and durable monatomic antibacterial and antiviral spray coating and a preparation method thereof.
In a first aspect, the application provides a high-efficiency and durable monatomic antibacterial and antiviral spray coating, which adopts the following technical scheme:
a high-efficiency and durable single-atom antibacterial and antiviral spray coating is prepared from the following raw materials in percentage by mass: 5-10% of monoatomic antibacterial antiviral catalyst, 2-25% of water-based polyurethane, 1-5% of nonionic dispersant, 1-5% of defoaming agent, 4-5% of organic silicon base material wetting agent, 1-5% of film-forming assistant, 0.5-2% of pH regulator and 20-60% of deionized water.
By adopting the technical scheme, the monoatomic antibacterial antiviral spray coating prepared in the application is a special antibacterial antiviral method prepared by performing surface treatment on the surface of a material, is friendly to human bodies and environment, and has wide application scenes; the monoatomic antibacterial and antiviral spray coating prepared in the application has the advantages of good film forming property, long and lasting antibacterial property and high inoxidizability, greatly prolongs the service life, reduces the manufacturing cost and meets the user requirements.
Preferably, the single-atom antibacterial and antiviral catalyst consists of a carrier and acetylacetone salt; the transition metal of the monatomic antibacterial and antiviral catalyst is anchored in the form of monatomic in the defect sites on the surface of the carrier.
By adopting the technical scheme, the carrier adsorbs bacteria or viruses, and the adsorbed bacteria or viruses are subjected to oxidative degradation by matching with the transition metal to destroy proteins and genetic materials of the bacteria or viruses, so that the bacteria and the viruses can be effectively killed.
Preferably, the mass ratio of the transition metal and the carrier in the monatomic antibacterial and antiviral catalyst is 1:20-1:200, and the transition metal is selected from one or more of Fe, Cu, Zn and Ag.
By adopting the technical scheme, the sterilizing and antiviral functions of the monatomic antibacterial and antiviral catalyst are ensured, and the production cost of the monatomic antibacterial and antiviral catalyst is reduced.
Preferably, the carrier is nano silicon oxide, and the fineness of the nano silicon oxide is 50-200 nm; the acetylacetone salt is selected from one or more of ferric acetylacetonate, copper acetylacetonate, zinc acetylacetonate, and silver acetylacetonate.
By adopting the technical scheme, the dispersion effect of the nano silicon oxide in the system can be ensured, the adsorption effect on viruses and bacteria is further improved, and the overall antibacterial and antiviral effects are improved.
Preferably, the synthesis steps of the monatomic antibacterial and antiviral catalyst are as follows:
s1: preparing a nano silicon oxide carrier by a chemical precipitation method;
s2, preparing a monoatomic antibacterial antiviral catalyst precursor: adding an aqueous solution of acetylacetone salt into a nano-silica carrier, wherein the mass ratio of transition metal to carrier is 1:20-1:200, carrying out ultrasonic treatment on the obtained solution for 30min, and stirring the mixed solution for 12-72 h; heating the obtained mixed solution to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and grinding for 0.1-2 hours to obtain solid powder;
and S3, performing high-temperature activation treatment to obtain the monatomic antibacterial antiviral catalyst.
By adopting the technical scheme, the monoatomic antibacterial and antiviral catalyst with better antibacterial and antiviral effects can be efficiently and stably prepared.
Preferably, the step of S1: preparing a nano silicon oxide carrier by a chemical precipitation method:
s1.1, weighing a certain mass of sodium silicate to prepare an ethanol aqueous solution with a volume ratio of 1 (6-10), and dissolving the sodium silicate in the ethanol aqueous solution to prepare a 0.3-0.5mol/L sodium silicate solution;
s1.2, adding 0.3-1.5g of cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB);
s1.3, preparing 100ml of ammonium chloride solution with the concentration of 1.0-2.0mol/L, stirring the ammonium chloride solution, controlling the temperature at 40 +/-1.5 ℃, and dripping the sodium silicate solution in the S1.1 into the ammonium chloride solution until the pH value reaches 8.5;
s1.4, stirring and reacting for 1-2h, centrifugally washing the obtained precipitate by using an ethanol aqueous solution added with CTAB in S1.2, drying the obtained white powder, calcining at 500 +/-10 ℃ for 3-6h, and grinding until the particle size of the powder is 80-150 nm.
By adopting the technical scheme, the nano silicon oxide carrier can be prepared more stably, the quality of the prepared carrier is ensured, and the antibacterial and antiviral functions of the single-atom antibacterial and antiviral catalyst are further ensured.
Preferably, the preparation of the single-atom antibacterial and antiviral catalyst precursor in S2 comprises the step of adding 10-100g/L of an aqueous solution of an acetylacetone salt into a nano silica carrier in S1 at a dropping speed of 80-120 mu L/S, wherein the mass ratio of a transition metal to the carrier is 1:20-1:200, performing ultrasonic treatment on the obtained solution under the condition of 100kHz for 30min to uniformly disperse the solution, and then stirring the mixed solution for 100-1000r/min for 12-72 h; heating the obtained mixed solution to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and performing ball milling at the rotating speed of 50-600r/min for 0.1-2 hours to obtain solid powder.
By adopting the technical scheme, stable preparation parameters are obtained through experiments, and the monoatomic antibacterial antiviral catalyst precursor can be prepared more stably.
Preferably, the high-temperature activation treatment in S3 is performed to obtain the monatomic antibacterial and antiviral catalyst, the solid powder in S2 is heated for 6-24h under the conditions of air atmosphere and temperature of 200-1000 ℃, cooled to room temperature, and ground for 30-60min at the rotating speed of 50r/min, so that the monatomic antibacterial and antiviral catalyst is obtained.
By adopting the technical scheme, the solid powder obtained in the step S3 is subjected to high-temperature activation treatment, so that the solid powder is subjected to high-temperature in-situ activation, and the antibacterial and antiviral functions of the prepared monatomic catalyst are ensured.
Preferably, the water-based polyurethane is a binder formed by dissolving or dispersing the polyurethane in water, the non-ionic dispersing agent is a Texaco non-ionic wetting dispersing agent BREAK-THRUDA646, the defoaming agent is a non-silicone mineral oil system, the film forming aid is propylene glycol phenyl ether, and the pH regulator is WantVANTEX-T.
By adopting the technical scheme, the single-atom antibacterial and antiviral catalyst can be well fused with a water-based polyurethane system to obtain the spray coating with better antibacterial and antiviral functions.
In a second aspect, the present application provides a method for preparing a high-efficiency and durable monatomic antibacterial and antiviral spray coating.
A preparation method of a high-efficiency and durable monatomic antibacterial and antiviral spray coating comprises the following steps:
s1, weighing the monoatomic antibacterial/antiviral catalyst and the nonionic dispersant according to the proportion, stirring and mixing uniformly, and grinding until the fineness is less than 10 mu m to obtain a component A;
s2, dispersing the component A and the water-based polyurethane at the rotating speed of 400-600r/min for 5-10min to obtain a component B;
and S3, uniformly dispersing the mixture of the component A and the component B, adding accurately weighed deionized water, an organic silicon base material wetting agent, a film forming aid and a defoaming agent, mechanically stirring and dispersing for 10min, adding a pH regulator during the mechanical stirring and regulating the pH value to be 7.1-7.5 to prepare the monatomic antibacterial antiviral spray.
By adopting the technical scheme, the preparation method is simple, easy for batch production and convenient for popularization and application.
In summary, the present application has the following advantages:
1. the monoatomic antibacterial and antiviral spray coating prepared by the method does not need other auxiliary conditions, can kill common bacteria and viruses in a broad spectrum, and can also quickly and continuously kill bacteria generating drug resistance, namely superbacteria.
2. The monoatomic antibacterial and antiviral spray coating prepared by the method can last for more than 10 years, does not generate any drug resistance, and has the advantages of broad-spectrum antibacterial, efficient disinfection, long-acting mildew resistance, no odor, no toxicity, environmental friendliness. Can be portably sprayed on various application scenes such as wall surfaces, ground surfaces, sofas and the like.
3. The monoatomic antibacterial antiviral spray coating prepared by the method can be portably sprayed on various application scenes such as walls, floors and sofas.
4. The preparation method is simple, easy to carry out batch production and convenient to popularize and apply.
Drawings
FIG. 1 is a transmission electron microscope photograph for correcting spherical aberration of the monoatomic antibacterial/antiviral catalyst according to preparation example 1 of the present application.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples.
Raw materials
Preparation example
Preparation example 1
The preparation of the single-atom antibacterial antiviral catalyst comprises the following steps:
s1 preparation of the nano-silica carrier by a chemical precipitation method:
s1.1, preparing an ethanol water solution with a volume ratio of 1:8, weighing sodium silicate, dissolving the sodium silicate in the ethanol water solution, and preparing a 0.4mol/L sodium silicate solution;
s1.2, and adding 0.5g of cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) into the sodium silicate solution;
s1.3, preparing 100ml of ammonium chloride solution with the concentration of 1.5mol/L, placing the prepared ammonium chloride solution on a constant-temperature magnetic stirrer, controlling the stirring speed to be 500rpm, controlling the temperature to be 40 ℃, dripping the sodium silicate solution in the S1.2 into the ammonium chloride solution at the speed of 100 mu L/S until the pH value is 8.5, continuing stirring and reacting for 1h, centrifugally washing the obtained precipitate by using ethanol water solution added with CTAB, wherein the ethanol water solution of CTAB is 0.1mol/L ethanol water solution of CTAB, and the ethanol water solution is ethanol water solution with the volume ratio of 1: 8;
s1.4, drying the obtained white powder in an oven at 100 ℃, calcining the white powder for 4 hours in a muffle furnace at 500 ℃, and grinding the white powder in a planetary ball mill until the granularity is 100nm to obtain a nano silicon oxide carrier;
s2, adding 20g/L of ferric acetylacetonate water solution into the nano silicon oxide carrier in S1.4 at a dropping speed of 100 mu L/S, wherein the mass ratio of the transition metal to the carrier is 1:20, carrying out ultrasonic treatment on the obtained solution for 30min under the condition of 100kHz to uniformly disperse, and then stirring the mixed solution for 12h at 100 r/min;
heating the mixed solution obtained in S3 and S2 to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and fully grinding for 0.5 hour at the rotating speed of 50r/min by using a planetary ball mill to obtain solid powder;
and (3) heating the solid powder in the S4 and S3 for 2 hours under the conditions of air atmosphere and 400 ℃, cooling to room temperature, grinding and grinding for 40 minutes at the rotating speed of 50r/min by using a planetary ball mill, wherein the prepared catalyst is a monoatomic antibacterial and antiviral catalyst, and referring to figure 1, transition metal of the monoatomic antibacterial and antiviral catalyst is anchored in a monoatomic form in defect sites on the surface of a carrier.
Preparation example 2
The preparation of the single-atom antibacterial antiviral catalyst comprises the following steps:
s1 preparation of the nano-silica carrier by a chemical precipitation method:
s1.1, preparing an ethanol water solution with a volume ratio of 1:8, weighing sodium silicate, dissolving the sodium silicate in the ethanol water solution, and preparing a 0.4mol/L sodium silicate solution;
s1.2, and adding 0.5g of cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) into the sodium silicate solution;
s1.3, preparing 100ml of ammonium chloride solution with the concentration of 1.5mol/L, placing the prepared ammonium chloride solution on a constant-temperature magnetic stirrer, controlling the stirring speed to be 500rpm, controlling the temperature to be 40 ℃, dripping the sodium silicate solution in the S1.2 into the ammonium chloride solution at the speed of 100 mu L/S until the pH value reaches 8.5, continuing stirring and reacting for 1h, centrifugally washing the obtained precipitate by using ethanol water solution added with CTAB, wherein the ethanol water solution of CTAB is 0.1mol/L ethanol water solution of CTAB, and the ethanol water solution is ethanol water solution with the volume ratio of 1:8,
s1.4, drying the obtained white powder in an oven at 100 ℃, calcining the white powder for 4 hours in a muffle furnace at 500 ℃, and grinding the white powder in a planetary ball mill until the granularity is 100nm to obtain a nano silicon oxide carrier;
s2, adding 10g/L of copper acetylacetonate water solution into the nano silicon oxide carrier in S1.4 at a dropping speed of 100 mu L/S, wherein the mass ratio of the transition metal to the carrier is 1:50, carrying out ultrasonic treatment on the obtained solution for 30min under the condition of 100kHz to uniformly disperse, and then stirring the mixed solution for 20h at a speed of 150 r/min;
heating the mixed solution obtained in S3 and S2 to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and fully grinding for 1 hour at the rotating speed of 100r/min by using a planetary ball mill to obtain solid powder;
and (3) heating the solid powder in the S4 and S3 for 2 hours in the air atmosphere at the temperature of 400 ℃, cooling to room temperature, and grinding for 40 minutes at the rotating speed of 100r/min by using a planetary ball mill to obtain the catalyst, namely the monatomic antibacterial and antiviral catalyst.
Preparation example 3
The preparation of the single-atom antibacterial antiviral catalyst comprises the following steps:
s1 preparation of the nano-silica carrier by a chemical precipitation method:
s1.1, preparing an ethanol water solution with a volume ratio of 1:8, weighing sodium silicate, dissolving the sodium silicate in the ethanol water solution, and preparing a 0.4mol/L sodium silicate solution;
s1.2, and adding 0.5g of cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) into the sodium silicate solution;
s1.3, preparing 100ml of ammonium chloride solution with the concentration of 1.5mol/L, placing the prepared ammonium chloride solution on a constant-temperature magnetic stirrer, controlling the stirring speed to be 500rpm, controlling the temperature to be 40 ℃, dripping the sodium silicate solution in the S1.2 into the ammonium chloride solution at the speed of 100 mu L/S until the pH value is 8.5, continuing stirring and reacting for 1h, centrifugally washing the obtained precipitate by using ethanol water solution added with CTAB, wherein the ethanol water solution of CTAB is 0.1mol/L ethanol water solution of CTAB, and the ethanol water solution is ethanol water solution with the volume ratio of 1: 8;
s1.4, drying the obtained white powder in an oven at 100 ℃, calcining the white powder for 4 hours in a muffle furnace at 500 ℃, and grinding the white powder in a planetary ball mill until the granularity is 100nm to obtain a nano silicon oxide carrier;
s2, adding 5g/L of zinc acetylacetonate water solution into the nano silicon oxide carrier in S1.4 at a dropping speed of 100 mu L/S, wherein the mass ratio of the transition metal to the carrier is 1:200, carrying out ultrasonic treatment on the obtained solution for 30min under the condition of 100kHz to uniformly disperse, and then stirring the mixed solution for 48h at 200 r/min;
heating the mixed solution obtained in S3 and S2 to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and fully grinding for 3 hours at the rotating speed of 500r/min by using a planetary ball mill to obtain solid powder;
and (3) heating the solid powder in the S4 and S3 for 2 hours in the air atmosphere at the temperature of 800 ℃, cooling to room temperature, and grinding for 40 minutes at the rotating speed of 500r/min by using a planetary ball mill to obtain the catalyst, namely the monatomic antibacterial antiviral catalyst.
Preparation example 4
The preparation of the single-atom antibacterial antiviral catalyst comprises the following steps:
s1 preparation of the nano-silica carrier by a chemical precipitation method:
s1.1, preparing an ethanol water solution with a volume ratio of 1:8, weighing sodium silicate, dissolving the sodium silicate in the ethanol water solution, and preparing a 0.4mol/L sodium silicate solution;
s1.2, and adding 0.5g of cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) into the sodium silicate solution;
s1.3, preparing 100ml of ammonium chloride solution with the concentration of 1.5mol/L, placing the prepared ammonium chloride solution on a constant-temperature magnetic stirrer, controlling the stirring speed to be 500rpm, controlling the temperature to be 40 ℃, dripping the sodium silicate solution in the S1.2 into the ammonium chloride solution at the speed of 100 mu L/S until the pH value is 8.5, continuing stirring and reacting for 1h, centrifugally washing the obtained precipitate by using ethanol water solution added with CTAB, wherein the ethanol water solution of CTAB is 0.1mol/L ethanol water solution of CTAB, and the ethanol water solution is ethanol water solution with the volume ratio of 1: 8;
s1.4, drying the obtained white powder in an oven at 100 ℃, calcining the white powder for 4 hours in a muffle furnace at 500 ℃, and grinding the white powder in a planetary ball mill until the granularity is 100nm to obtain a nano silicon oxide carrier;
s2, adding 50g/L of silver acetylacetonate water solution into the nano silicon oxide carrier in S1.4 at a dropping speed of 100 mu L/S, wherein the mass ratio of the transition metal to the carrier is 1:50, carrying out ultrasonic treatment on the obtained solution under the condition of 100kHz for 60min to uniformly disperse, and then stirring the mixed solution for 24h at 500 r/min;
heating the mixed solution obtained in S3 and S2 to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and fully grinding for 1 hour at the rotating speed of 300r/min by using a planetary ball mill to obtain solid powder;
and (3) heating the solid powder in the S4 and S3 for 5 hours in the air atmosphere at the temperature of 800 ℃, cooling to room temperature, and grinding for 40 minutes at the rotating speed of 500r/min by using a planetary ball mill to obtain the catalyst, namely the monatomic antibacterial antiviral catalyst.
Preparation example 5
The preparation of the single-atom antibacterial antiviral catalyst comprises the following steps:
s1, preparing the nano silicon oxide carrier by a chemical precipitation method:
s1.1, preparing an ethanol water solution with a volume ratio of 1:8, weighing sodium silicate, dissolving the sodium silicate in the ethanol water solution, and preparing a 0.4mol/L sodium silicate solution;
s1.2, and adding 0.5g of cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) into the sodium silicate solution;
s1.3, preparing 100ml of ammonium chloride solution with the concentration of 1.5mol/L, placing the prepared ammonium chloride solution on a constant-temperature magnetic stirrer, controlling the stirring speed to be 500rpm, controlling the temperature to be 40 ℃, dripping the sodium silicate solution in the S1.2 into the ammonium chloride solution at the speed of 100 mu L/S until the pH value is 8.5, continuing stirring and reacting for 1h, centrifugally washing the obtained precipitate by using ethanol water solution added with CTAB, wherein the ethanol water solution of CTAB is 0.1mol/L ethanol water solution of CTAB, and the ethanol water solution is ethanol water solution with the volume ratio of 1: 8;
s1.4, drying the obtained white powder in an oven at 100 ℃, calcining the white powder for 4 hours in a muffle furnace at 500 ℃, and grinding the white powder in a planetary ball mill until the granularity is 100nm to obtain a nano silicon oxide carrier;
s2, adding 50g/L ferric acetylacetonate, 100g/L copper acetylacetonate, 100g/L zinc acetylacetonate and 50g/L silver acetylacetonate aqueous solution into the nano silicon oxide carrier in S1.4 at a dropping speed of 100 mu L/S, wherein the mass ratio of transition metal to the carrier is 1:20, the mass ratio of the ferric acetylacetonate, the copper acetylacetonate, the zinc acetylacetonate and the silver acetylacetonate is 1:1:1, carrying out ultrasonic treatment on the obtained solution for 90min under the condition of 100kHz, uniformly dispersing, and then stirring the mixed solution for 12h at 500 r/min;
heating the mixed solution obtained in S3 and S2 to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and fully grinding for 1 hour at the rotating speed of 300r/min by using a planetary ball mill to obtain solid powder;
and (3) heating the solid powder in the S4 and S3 for 2 hours in the air atmosphere at the temperature of 800 ℃, cooling to room temperature, and grinding for 30 minutes at the rotating speed of 500r/min by using a planetary ball mill to obtain the catalyst, namely the monatomic antibacterial and antiviral catalyst.
Examples
Example one
The application discloses a high-efficiency and durable single-atom antibacterial and antiviral spray coating, which comprises the following components in percentage by weight: 10% of the monoatomic antibacterial antiviral catalyst of preparation example 1, 25% of water-based polyurethane, 25% of 2.5% of the degussa nonionic wetting dispersant BREAK-THRU DA646, 2.5% of a non-silicone mineral oil defoamer, 5% of the Digaku wetting agent WET KL245, 3% of propylene glycol phenyl ether, 2% of the TeVANTEX-T, a pH regulator of Istman Eastman, USA brand, and 50% of deionized water.
A preparation method of a high-efficiency durable monoatomic antibacterial antiviral spray coating comprises the following steps:
s1, weighing the monatomic antibacterial and antiviral catalyst and the nonionic dispersant in the preparation example 1 according to the mixture ratio, stirring and mixing for 5min in a high-speed dispersion kettle at the rotating speed of 200rpm, and grinding to the fineness of less than 10 microns by using a sand mill to obtain a component A;
s2, dispersing the component A and the water-based polyurethane for 5min at the rotating speed of 450r/min until the components are uniformly dispersed to obtain a component B;
and S3, uniformly dispersing the mixture of the component A and the component B, adding deionized water with accurate measurement, a Digao base material wetting agent WET KL245 and propylene glycol phenyl ether, mechanically stirring and dispersing for 10min at the rotating speed of 400rpm, adding VANTEX-T with accurate measurement and a pH regulator of Eastman of American Istman in the stirring process, and adjusting the pH value to be 7.1-7.5 to prepare the monatomic antibacterial and antiviral spray.
Example two
The difference between the second embodiment and the first embodiment is that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 2.
EXAMPLE III
The difference between the third embodiment and the first embodiment is that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 3.
Example four
The difference between the fourth embodiment and the first embodiment is that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 3.
EXAMPLE five
The difference between the fifth embodiment and the first embodiment is that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 5.
EXAMPLE six
The application discloses a high-efficiency and durable single-atom antibacterial and antiviral spray coating, which comprises the following components in percentage by weight: 10% of the monatomic antibacterial and antiviral catalyst of preparation example 1, 10% of water-based polyurethane, 4% of the degussa nonionic wetting dispersant BREAK-THRU DA646, 5% of the non-silicone mineral oil defoamer, 5% of the diutan high base wetting agent WET KL245, 4% of propylene glycol phenyl ether, 2% of the TeVANTEX-T, the pH regulator of Istmann, USA, and 60% of deionized water.
A preparation method of a high-efficiency durable monoatomic antibacterial antiviral spray coating comprises the following steps:
s1, weighing the monatomic antibacterial and antiviral catalyst and the nonionic dispersant in the preparation example 1 according to the mixture ratio, stirring and mixing for 5min in a high-speed dispersion kettle at the rotating speed of 200rpm, and grinding to the fineness of less than 10 microns by using a sand mill to obtain a component A;
s2, dispersing the component A and the water-based polyurethane for 5min at the rotating speed of 450r/min until the components are uniformly dispersed to obtain a component B;
and S3, uniformly dispersing the mixture of the component A and the component B, adding deionized water with accurate measurement, a Digao base material wetting agent WET KL245 and propylene glycol phenyl ether, mechanically stirring and dispersing for 10min at the rotating speed of 400rpm, adding VANTEX-T with accurate measurement and a pH regulator of Eastman of American Istman in the stirring process, and adjusting the pH value to be 7.1-7.5 to prepare the monatomic antibacterial and antiviral spray.
EXAMPLE seven
The seventh embodiment differs from the sixth embodiment in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 2.
Example eight
The difference between the eighth embodiment and the sixth embodiment is that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 3.
Example nine
The difference between the ninth embodiment and the sixth embodiment is that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 4.
Example ten
The difference between the tenth embodiment and the sixth embodiment is that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 5.
EXAMPLE eleven
The application discloses a high-efficiency and durable single-atom antibacterial and antiviral spray coating, which comprises the following components in percentage by weight: 10% of the monoatomic antibacterial and antiviral catalyst of preparation example 1, 20% of water-based polyurethane, 2.5% of a Delgaset non-ionic wetting dispersant BREAK-THRU DA646, 2.5% of a non-silicone mineral oil defoamer, 5% of a Digaku base wetting agent WET KL245, 4% of propylene glycol phenyl ether, 2% of a TeVANTEX-T, a pH regulator of Isyman Eastman, USA, and 55% of deionized water.
A preparation method of a high-efficiency durable monoatomic antibacterial antiviral spray coating comprises the following steps:
s1, weighing the monatomic antibacterial and antiviral catalyst and the nonionic dispersant in the preparation example 1 according to the mixture ratio, stirring and mixing for 5min in a high-speed dispersion kettle at the rotating speed of 200rpm, and grinding to the fineness of less than 10 microns by using a sand mill to obtain a component A;
s2, dispersing the component A and the water-based polyurethane for 5min at the rotating speed of 450r/min until the components are uniformly dispersed to obtain a component B;
and S3, uniformly dispersing the mixture of the component A and the component B, adding deionized water with accurate measurement, a Digao base material wetting agent WET KL245 and propylene glycol phenyl ether, mechanically stirring and dispersing for 10min at the rotating speed of 400rpm, adding VANTEX-T with accurate measurement and a pH regulator of Eastman of American Istman in the stirring process, and adjusting the pH value to be 7.1-7.5 to prepare the monatomic antibacterial and antiviral spray.
Example twelve
Example twelve differs from example eleven in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 2.
EXAMPLE thirteen
The thirteenth embodiment differs from the eleventh embodiment in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 3.
Example fourteen
The fourteenth embodiment differs from the eleventh embodiment in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 4.
Example fifteen
The fifteenth embodiment differs from the eleventh embodiment in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the same amount as in preparation example 1.
Example sixteen
The application discloses a high-efficiency and durable single-atom antibacterial and antiviral spray coating, which comprises the following components in percentage by weight: 10% of the monatomic antibacterial and antiviral catalyst of preparation example 1, 25% of water-based polyurethane, 4% of the degussa nonionic wetting dispersant BREAK-THRU DA646, 4% of the non-silicone mineral oil defoamer, 4% of the diutan high base wetting agent WET KL245, 3% of propylene glycol phenyl ether, 2% of the TeVANTEX-T, pH regulator of Istmann, USA, and 48% of deionized water.
A preparation method of a high-efficiency durable monoatomic antibacterial antiviral spray coating comprises the following steps:
s1, weighing the monatomic antibacterial and antiviral catalyst and the nonionic dispersant in the preparation example 1 according to the mixture ratio, stirring and mixing for 5min in a high-speed dispersion kettle at the rotating speed of 200rpm, and grinding to the fineness of less than 10 microns by using a sand mill to obtain a component A;
s2, dispersing the component A and the water-based polyurethane for 5min at the rotating speed of 450r/min until the components are uniformly dispersed to obtain a component B;
and S3, uniformly dispersing the mixture of the component A and the component B, adding deionized water with accurate measurement, a Digao base material wetting agent WET KL245 and propylene glycol phenyl ether, mechanically stirring and dispersing for 10min at the rotating speed of 400rpm, adding VANTEX-T with accurate measurement and a pH regulator of Eastman of American Istman in the stirring process, and adjusting the pH value to be 7.1-7.5 to prepare the monatomic antibacterial and antiviral spray.
Example seventeen
Example seventeen differs from example sixteenth in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 2.
EXAMPLE eighteen
The eighteenth embodiment differs from the sixteenth embodiment in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 3.
Example nineteen
The nineteen examples differ from the sixteen examples in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 4.
Example twenty
Example twenty differs from example sixteen in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 5.
Example twenty one
The application discloses a high-efficiency and durable single-atom antibacterial and antiviral spray coating, which comprises the following components in percentage by weight: 8% of the single-atom antibacterial and antiviral catalyst in preparation example 1, 20% of water-based polyurethane, 5% of a Delgasea nonionic wetting dispersant BREAK-THRU DA646, 4% of a non-silicone mineral oil antifoaming agent, 5% of a Digao base wetting agent WET KL245, 3% of propylene glycol phenyl ether, 2% of a TeVANTEX-T, a pH regulator of Isyman Eastman, USA, and 53% of deionized water.
A preparation method of a high-efficiency durable monoatomic antibacterial antiviral spray coating comprises the following steps:
s1, weighing the monatomic antibacterial and antiviral catalyst and the nonionic dispersant in the preparation example 1 according to the mixture ratio, stirring and mixing for 5min in a high-speed dispersion kettle at the rotating speed of 200rpm, and grinding to the fineness of less than 10 microns by using a sand mill to obtain a component A;
s2, dispersing the component A and the water-based polyurethane for 5min at the rotating speed of 450r/min until the components are uniformly dispersed to obtain a component B;
and S3, uniformly dispersing the mixture of the component A and the component B, adding deionized water with accurate measurement, a Digao base material wetting agent WET KL245 and propylene glycol phenyl ether, mechanically stirring and dispersing for 10min at the rotating speed of 400rpm, adding VANTEX-T with accurate measurement and a pH regulator of Eastman of American Istman in the stirring process, and adjusting the pH value to be 7.1-7.5 to prepare the monatomic antibacterial and antiviral spray.
Example twenty two
The embodiment twenty-two differs from the embodiment twenty-one in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 2.
Example twenty three
The twenty-three embodiment differs from the twenty-one embodiment in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 3.
Example twenty-four
The twenty-four embodiment differs from the twenty-one embodiment in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 4.
Example twenty-five
Example twenty-five differs from example twenty-one in that: the monoatomic antibacterial/antiviral catalyst used in preparation example 1 was replaced with the monoatomic antibacterial/antiviral catalyst used in preparation example 5.
Comparative example
Comparative example 1
The difference between the first comparative example and the first example is that: the monatomic antibacterial and antiviral catalyst in preparation example 1 was replaced with the nano-silica carrier prepared by the S1 chemical precipitation method in preparation example 1.
Comparative example No. two
The difference between the second comparative example and the sixth example is that: the monatomic antibacterial and antiviral catalyst in preparation example 1 was replaced with the nano-silica carrier prepared by the S1 chemical precipitation method in preparation example 2.
Comparative example No. three
The difference between the third comparative example and the sixth example is that: the monatomic antibacterial and antiviral catalyst in preparation example 1 was replaced with the nano-silica carrier prepared by the S1 chemical precipitation method in preparation example 3.
Comparative example No. four
The difference between the fourth comparative example and the sixth example is that: the monatomic antibacterial and antiviral catalyst in preparation example 1 was replaced with the nano-silica carrier prepared by the S1 chemical precipitation method in preparation example 4.
Comparative example five
The difference between the fifth comparative example and the sixth example is that: the monatomic antibacterial and antiviral catalyst in preparation example 1 was replaced with the nano-silica carrier prepared by the S1 chemical precipitation method in preparation example 5.
Performance test
1) Single atom antibacterial antiviral spray coating antibacterial experiment:
step 1, preparing a sample plate with the size of 50mm multiplied by 50mm, selecting a practical substrate (such as a metal plate and a plastic plate), uniformly spraying the monoatomic antibacterial antiviral spray on the substrate, naturally drying, and ensuring that a paint film of the test plate is completely dried and then used for an experiment.
Step 2, inoculate each sample with 20 μ L of bacterial test culture. The inoculation volume was spread evenly using a curved sterile pipette to ensure complete even coverage, spreading as close to the specimen edge as possible. The samples were then incubated for 120min in a controlled environment set at 42% relative humidity and 23 ℃. After an exposure period of 120 minutes, the test sample was neutralized in nutrient broth. Ten-fold serial dilutions of the neutralization solution were plated on tryptic soy agar plates using standard plating techniques and incubated for 48 hours at 36 deg.C (30 deg.C for Percola) to yield countable viable colonies (about 20-200 colonies per plate).
The experiment was repeated: each sample was inoculated with 20. mu.L of bacterial test culture. The inoculation volume was spread evenly using a curved sterile pipette to ensure complete even coverage, spreading as close to the specimen edge as possible. The samples were then incubated for 120min in a controlled environment set at 42% relative humidity and 23 ℃. After an exposure period of 120 minutes, the test sample was neutralized in nutrient broth. Ten-fold serial dilutions of the neutralization solution were plated on tryptic soy agar plates using standard plating techniques and incubated in a 36 + -1 deg.C biochemical incubator for 48 hours to produce countable viable colonies (approximately 20-200 colonies per plate).
2) Single atom antibacterial antiviral spray coating antiviral experiment:
step 1, mixing 900 mul of culture solution with 100 mul of enterovirus 71, influenza A H3N2 and influenza A H1N1 virus solutions, taking 600 mul of the mixture to a coating plate, placing the coating plate on a sterile culture dish, and placing the coating plate at room temperature.
And 2, taking out 5 mu L of the cell culture medium respectively at 30min, 1h, 6h, 12h and 24h, adding the cell culture medium into a cell culture hole, and observing the cell state and whether the cell has fluorescence or not.
The experiment was repeated: mixing 900 μ L culture solution with 100 μ L enterovirus 71, influenza A H3N2, and influenza A H1N1, collecting 600 μ L coated plate, and placing the coated plate in sterile culture dish. 400 μ L of enterovirus 71, influenza A H3N2, and influenza A H1N1 virus solutions remained as controls. Standing at room temperature, taking out 5 μ L of the culture solution at 1h, mixing with 400 μ L of the culture solution, adding into the cell culture well, and changing the culture solution after 2 h. The treatment methods of 1h, 3h, 6h, 12h and 24h are the same as above. The cell state and the presence or absence of fluorescence of the cells were observed.
Data analysis
TABLE 1 EXAMPLES 1-5 AND COMPARATIVE EXAMPLE 1 monatomic antibacterial antiviral spray coating antibacterial test parameters
TABLE 2 test parameters for the single atom antibacterial and antiviral spray coating antibacterial test of examples 6-10 and comparative example 2
TABLE 3 EXAMPLES 11-15 AND COMPARATIVE EXAMPLE 3 monoatomic antibacterial antiviral spray coating antibacterial test parameters
TABLE 4 EXAMPLES 16-20 AND COMPARATIVE EXAMPLE 4 monoatomic antibacterial antiviral spray coating antibacterial test parameters
TABLE 5 EXAMPLES 21-25 AND COMPARATIVE EXAMPLE 5 monoatomic antibacterial antiviral spray coating antibacterial test parameters
By combining the examples 1-25 and the comparative examples 1-5 and combining the tables 1-5, the killing rate of common bacteria of escherichia coli and staphylococcus aureus of the monatomic antibacterial antiviral spray coating prepared by the method reaches more than 99.9%; the inactivation rates of enterovirus 71, influenza A H3N2 and influenza A H1N1 all reach more than 99.9 percent.
TABLE 6 Experimental test parameters (virus inactivation ratio) for type 71 anti-enterovirus of the monatomic antibacterial and antiviral spray coatings of examples 1-25 and comparative examples 1-5
TABLE 7 experimental test parameters (virus inactivation rates) for the monatomic antibacterial and antiviral spray coatings of examples 1-25 and comparative examples 1-5 against H3N2 influenza A virus
TABLE 8 experimental test parameters (virus inactivation rates) for the monatomic antibacterial and antiviral spray coatings of examples 1-25 and comparative examples 1-5 against H1N1 influenza A virus
As can be seen by combining examples 1-25 and comparative examples 1-5 and combining tables 6-8, the monatomic antibacterial and antiviral spray coating prepared by the method has excellent effects of killing bacteria and viruses on enterovirus 71, influenza A H3N2 and influenza A H1N1, the antiviral rate reaches over 90% after 30min of test treatment, and the inactivation rate is maintained at over 99.9% after 1H, 6H, 12H and 24H.
To sum up, the monatomic antibacterial and antiviral spray coating completely inactivates enterovirus 71, influenza A H3N2 and influenza A H1N1, and the inactivation rate is maintained to be more than 99.9%, so that the coating prepared by the method has a good inactivation effect on the enterovirus 71, the influenza A H3N2 and the influenza A H1N 1.
The embodiments of the present invention are preferred embodiments of the present application, and the scope of protection of the present application is not limited by the embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. The high-efficiency and durable monatomic antibacterial and antiviral spray coating is characterized by being prepared from the following raw materials in percentage by mass: 5-10% of monoatomic antibacterial antiviral catalyst, 2-25% of water-based polyurethane, 1-5% of nonionic dispersant, 1-5% of defoaming agent, 4-5% of organic silicon base material wetting agent, 1-5% of film-forming assistant, 0.5-2% of pH regulator and 20-60% of deionized water.
2. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 1, wherein: the single-atom antibacterial and antiviral catalyst consists of a carrier and acetylacetone salt; the transition metal of the monatomic antibacterial and antiviral catalyst is anchored in the form of monatomic in the defect sites on the surface of the carrier.
3. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 2, wherein: the mass ratio of the transition metal to the carrier in the single-atom antibacterial and antiviral catalyst is 1:20-1:200, and the transition metal is selected from one or more of Fe, Cu, Zn and Ag.
4. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 2, wherein: the carrier is nano silicon oxide, and the fineness of the nano silicon oxide is 50-200 nm; the acetylacetone salt is selected from one or more of ferric acetylacetonate, copper acetylacetonate, zinc acetylacetonate, and silver acetylacetonate.
5. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 2, wherein: the synthesis steps of the monatomic antibacterial and antiviral catalyst are as follows:
s1: preparing a nano silicon oxide carrier by a chemical precipitation method;
s2, preparing a monoatomic antibacterial antiviral catalyst precursor: adding an aqueous solution of acetylacetone salt into a nano-silica carrier, wherein the mass ratio of transition metal to carrier is 1:20-1:200, carrying out ultrasonic treatment on the obtained solution for 30min, stirring the mixed solution for 12-72h, heating the obtained mixed solution to the boiling point of water, volatilizing at high temperature, evaporating the solvent, and grinding for 0.1-2 h to obtain solid powder;
and S3, performing high-temperature activation treatment to obtain the monatomic antibacterial antiviral catalyst.
6. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 1, wherein: the step 1: preparing a nano silicon oxide carrier by a chemical precipitation method:
s1.1, weighing a certain mass of sodium silicate to prepare an ethanol aqueous solution with a volume ratio of 1 (6-10), and dissolving the sodium silicate in the ethanol aqueous solution to prepare a 0.3-0.5mol/L sodium silicate solution;
s1.2, adding 0.3-1.5g of cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB);
s1.3, preparing 100ml of ammonium chloride solution with the concentration of 1.0-2.0mol/L, stirring the ammonium chloride solution, controlling the temperature to be 40 +/-1.5 ℃, and dripping the sodium silicate solution in the S1.1 into the ammonium chloride solution until the pH value is = 8.5;
s1.4, stirring and reacting for 1-2h, centrifugally washing the obtained precipitate by using an ethanol aqueous solution added with CTAB, drying the obtained white powder, calcining for 3-6h at 500 +/-10 ℃, and grinding until the particle size of the powder is 80-150 nm.
7. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 6, wherein: preparing the single-atom antibacterial and antiviral catalyst precursor in S2, adding 10-100g/L of an aqueous solution of acetylacetone salt into the nano silicon oxide carrier in S1 at a dropping speed of 80-120 mu L/S, wherein the mass ratio of the transition metal to the carrier is 1:20-1:200, performing ultrasonic treatment on the obtained solution under the condition of 100kHz for 30min to uniformly disperse the solution, and then stirring the mixed solution for 100-1000r/min for 12-72 h; heating the obtained mixed solution to the boiling point of water, volatilizing at high temperature, evaporating the solvent to dryness, and performing ball milling at the rotating speed of 50-600r/min for 0.1-2 hours to obtain solid powder.
8. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 6, wherein: and (3) performing high-temperature activation treatment in the S3 to obtain the monatomic antibacterial and antiviral catalyst, heating the solid powder in the S2 for 6-24h under the conditions of air atmosphere and the temperature of 200-1000 ℃, cooling to room temperature, and grinding for 30-60min at the rotating speed of 50r/min to obtain the monatomic antibacterial and antiviral catalyst.
9. A high efficiency, long lasting, monatomic antibacterial antiviral spray coating of claim 1, wherein: the water-based polyurethane is an adhesive formed by dissolving or dispersing polyurethane in water, the non-ionic dispersing agent is a Texaco non-ionic wetting dispersing agent BREAK-THRUDA646, the defoaming agent is a non-silicone mineral oil system, the film-forming assistant is propylene glycol phenyl ether, and the pH regulator is VaNTEX-T.
10. A method of preparing a high performance, long lasting, monatomic antibacterial and antiviral spray coating of any of claims 1-9, comprising the steps of:
s1, weighing the monoatomic antibacterial/antiviral catalyst and the nonionic dispersant according to the proportion, stirring and mixing uniformly, and grinding until the fineness is less than 10 mu m to obtain a component A;
s2, dispersing the component A and the water-based polyurethane at the rotating speed of 400-600r/min for 5-10min to obtain a component B;
and S3, uniformly dispersing the mixture of the component A and the component B, adding accurately weighed deionized water, an organic silicon base material wetting agent, a film forming aid and a defoaming agent, mechanically stirring and dispersing for 10min, adding a pH regulator during the mechanical stirring and regulating the pH value to be 7.1-7.5 to prepare the monatomic antibacterial antiviral spray.
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