CN113082205A - Nano titanium dioxide photocatalytic antibacterial material, preparation method and application thereof - Google Patents
Nano titanium dioxide photocatalytic antibacterial material, preparation method and application thereof Download PDFInfo
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- CN113082205A CN113082205A CN202110378195.3A CN202110378195A CN113082205A CN 113082205 A CN113082205 A CN 113082205A CN 202110378195 A CN202110378195 A CN 202110378195A CN 113082205 A CN113082205 A CN 113082205A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 61
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 49
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 138
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- 238000000034 method Methods 0.000 claims description 19
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- 239000011261 inert gas Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 230000000415 inactivating effect Effects 0.000 claims description 9
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- 239000010936 titanium Substances 0.000 claims description 8
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 6
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Images
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0057—Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/513—Organic macromolecular compounds; Dendrimers
- A61K9/5161—Polysaccharides, e.g. alginate, chitosan, cellulose derivatives; Cyclodextrin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5192—Processes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B01J35/39—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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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
Abstract
The invention discloses a preparation method of a nano titanium dioxide photocatalytic antibacterial material, which comprises the steps of calcining a cigarette filter at high temperature to obtain a carbonized cigarette filter, immersing the carbonized cigarette filter into a titanium dioxide growth solution and stirring, placing the soaked carbonized cigarette filter under high temperature and high pressure for reaction, cooling, washing and drying a reaction product to obtain the carbonized cigarette filter loaded with nano TiO2An antibacterial material. Carbonizing the cigarette filter tip to obtain the nano TiO2Is negativeThe material is carried, so that waste consumables are recycled, a new green and economic purpose is provided for daily waste, and after the cigarette filter is carbonized, a super-porous structure in the cigarette filter can provide a larger specific surface area and a larger pore volume to load more nano TiO2The particles provide a reaction platform for photocatalytic reaction, are more favorable for attachment of reaction substances, and effectively improve photocatalytic efficiency. The invention also discloses a nano titanium dioxide photocatalytic antibacterial material and application thereof.
Description
Technical Field
The invention relates to the technical field of inorganic antibacterial materials, in particular to a nano titanium dioxide photocatalytic antibacterial material, a preparation method and application thereof.
Background
At present, common antibacterial materials are mainly classified into organic antibacterial materials and inorganic antibacterial materials. The organic antibacterial material is mostly toxic, is easy to generate microbial drug resistance and drug resistance, and is greatly limited in practical application, the inorganic antibacterial material mainly comprises an ionic antibacterial material taking silver ions as a main component and an inorganic material utilizing photocatalysis antibacterial, although the silver ion antibacterial effect is good, the inorganic material is unstable and the processing cost is high, and the n-type semiconductor photocatalysis material taking titanium dioxide as a main component can be repeatedly used for a plurality of times to keep the light dispersion efficiency unchanged due to the characteristics of high photocatalysis efficiency, no secondary pollution, wide application range, no toxicity, no harm, low price and the like, so that the organic antibacterial material becomes the most popular photocatalysis antibacterial inorganic material in recent years and is widely applied to various fields needing antibiosis and bacteriostasis.
Titanium dioxide only depends on photocatalysis in the process of inactivating bacteria and viruses, and the principle is as follows: when the titanium dioxide is irradiated by light, electrons on the valence band of the semiconductor are excited to jump to the conduction band to form negatively charged high-activity electrons e-And corresponding photo-generated holes are generated on the valence band, are separated under the action of an electric field and migrate to the surface of ions, have strong electronic capacity and strong oxidizability, can enable oxygen molecules to be changed into active oxygen and enable water molecules to generate hydroxyl radicals, and the titanium dioxide photocatalysis sterilization effect is mainly the result of the joint action of the active oxygen and the hydroxyl radicals on bacteria or viruses. However, the single titanium dioxide antibacterial agent has disadvantages in that electron-hole recombination is easy, particles are easily agglomerated, and the photocatalytic reaction is not continuously and stably performed. In order to overcome the above disadvantages, methods such as loading are currently used to improve the photocatalytic activity, and glass fibers or activated carbon fibers are generally used as carriers.
The abandoned cigarette filter tip produced by the cigarette consumed every year in the world is more than eighty-ten-thousand tons, the main component of the cigarette filter tip is non-biodegradable cellulose acetate, the abandoned cigarette filter tip can produce a large amount of garbage, and the environment can be polluted by heavy metal in the abandoned cigarette filter tip, but the carbonized cigarette filter tip can be used as a novel porous material due to the ultrahigh porosity of the cigarette filter tip, and a new choice is provided for a nanometer titanium dioxide photocatalyst carrier.
Disclosure of Invention
The invention aims to overcome at least one defect (deficiency) of the prior art, provides a nano titanium dioxide photocatalytic antibacterial material, a preparation method and application thereof, overcomes the self limitation of a single antibacterial agent, enables the specific surface area of the prepared photocatalytic material to be larger, further improves the light utilization rate, and can effectively improve the catalytic efficiency by carbonizing a filter tip to enable the titanium dioxide electron hole pairs to be separated more easily.
The technical scheme adopted by the invention is that the preparation method of the nano titanium dioxide photocatalytic antibacterial material comprises the steps of calcining a cigarette filter at high temperature to obtain a carbonized cigarette filter, immersing the carbonized cigarette filter into a titanium dioxide growth solution and stirring, reacting the soaked carbonized cigarette filter at high temperature and high pressure, cooling, washing and drying a reaction product to obtain the carbonized cigarette filter loaded with nano TiO2An antibacterial material.
In the technical scheme, in the whole photocatalysis process, the nano TiO2No mass loss and harmful substance precipitation, and nano TiO in the whole photocatalysis process2Can be repeatedly used for at least 12 times while keeping light dispersion efficiency unchanged, and can be used as nano TiO after carbonizing cigarette filter tip as daily waste2The inner super-porous structure provides larger specific surface area and larger pore volume and can load more nano TiO2The particles can be more beneficial to the attachment of reaction substances, a reaction platform is provided for the photocatalytic reaction, and the acetate fiber of the filter tip is carbonized to ensure that the nano TiO2The electron hole pairs are easier to separate, particle agglomeration is avoided, the photocatalytic reaction is continuously and stably carried out, and the photocatalytic efficiency can be effectively improved.
Preferably, the method specifically comprises the following steps:
s1, placing the cigarette filter into a tube furnace, introducing inert gas, slowly heating to 700-900 ℃ at a speed of 10-20 ℃/min in an inert gas environment, keeping constant temperature, calcining for 20-40 min, and naturally cooling to obtain a carbonized cigarette filter;
s2, adding secondary distilled water into the surfactant, stirring until the secondary distilled water is fully dissolved, adjusting the pH value to 8-11, and adding a titanium dioxide precursor solution to prepare a titanium dioxide growth solution;
s3, soaking the carbonized cigarette filter tip into the titanium dioxide growth solution and stirring for 25-40 min;
s4, placing the carbonized cigarette filter tip soaked with the titanium dioxide growth solution into a hydrothermal reactor, heating the hydrothermal reactor to enable the titanium dioxide growth solution in the carbonized cigarette filter tip to react at high temperature and high pressure, naturally cooling after the reaction, and taking out a crude product;
s5, washing the crude product to be neutral, and drying to obtain the carbonized cigarette filter loaded with nano TiO2An antibacterial material.
In the technical scheme, the cigarette filter is carbonized firstly, and in the process, the cigarette filter is calcined at a specific heating rate, temperature and time, so that the cigarette filter can be ensured to reach the appropriate load of nano TiO2The carbonization effect of the nano TiO can avoid incomplete carbonization when the temperature is too low and over high carbonization degree when the calcination temperature is too high, the porous structure in the cigarette filter is easy to break and collapse, the specific surface area is greatly reduced, and the nano TiO is used for preparing the nano TiO-based composite material2The load is less, is not favorable to the going on of photocatalytic reaction, and rate of rise too high can lead to the temperature delay in the tubular furnace, is difficult to accurate control heat preservation temperature, can destroy the boiler tube even, and rate of rise too low can make the intensification time overlength, the extravagant energy.
Carbonized cigarette filter tip as nano TiO2The loading platform can adopt various methods to prepare the nano TiO loaded on the porous structure of the filter tip2In the technical scheme, the solution can fully enter a porous structure by adopting a hydrothermal method for preparation, so that the prepared nano TiO2The crystal can be uniformly loaded on the surface of the nano TiO2Purity of the crystalThe degree is higher, is favorable to improving the efficiency of the photocatalytic reaction.
Preferably, in step S1, slowly raising the temperature to 800 ℃ at a rate of 15 ℃/min under an inert gas environment, keeping the constant temperature for calcination for 30min, and then naturally cooling to obtain the carbonized cigarette filter.
Preferably, in step S2, the surfactant is dodecylamine.
Preferably, in step S2, the titania precursor solution is a titanium (iv) isopropoxide salt solution.
Preferably, in step S2, Ti in the titania growth solution4+The concentration of the ions was 0.25 mol/L.
In the technical scheme, Ti in the titanium dioxide growth solution is controlled4+The concentration of ions is maintained at a certain concentration, so that the nano TiO prepared when the concentration is too high is avoided2The crystal is easy to agglomerate, and the stable proceeding of the photocatalytic reaction is influenced.
Preferably, in step S4, the hydrothermal reactor is heated to 120-180 ℃.
In the technical scheme, as a hydrothermal method is adopted, the nano TiO is generated at a certain temperature and the autogenous pressure of water2Crystals of nano TiO with increasing temperature2The grain size of the crystal is increased continuously, and when the temperature is increased to a certain stage, the nano TiO2The increase in the crystal grain size is gradually reduced, and therefore, the nano TiO can be obtained by setting the heating temperature in this range2The particle size of the crystal is kept in a proper range, so that the particle size is not too small due to too small heating temperature, the light absorption capacity of the material is reduced, the efficiency of the photocatalytic reaction is influenced, and energy is not wasted due to too large heating temperature.
Preferably, in step S5, the crude product is washed to neutrality and then dried at 70-90 ℃.
The nano titanium dioxide photocatalytic antibacterial material is prepared by the method and comprises a carbonized cigarette filter tip and nano titanium dioxide, wherein the nano titanium dioxide is loaded on the surface and pore channels of the carbonized cigarette filter tip.
In the technical scheme, the nano TiO in the antibacterial material2The crystals are uniformly loaded on the surface and pore channels of the carbonized cigarette filter tip, the self limitations that single titanium dioxide antibacterial agent is easy to compound electron-hole and easy to agglomerate can be overcome, the specific surface area of the antibacterial material is larger, and more nano TiO can be loaded2Besides, more reaction substances can be favorably attached to the surface and pore channels of the antibacterial material, the light utilization rate is further improved, the photocatalytic reaction is promoted to be carried out, and the cellulose acetate fibers of the filter tip can be carbonized to ensure that the nano TiO2The electron hole pairs are easier to separate, and the catalytic efficiency can be effectively improved.
The application of the nano titanium dioxide photocatalytic antibacterial material is used for inactivating escherichia coli.
Escherichia coli is a conditional pathogen, which harms human beings and various animals to cause gastrointestinal tract infection or urinary tract infection and other local tissue and organs under certain conditions, and can only effectively prevent the Escherichia coli infection by paying attention to diet sanitation at present, while the nano TiO is used for preventing the Escherichia coli infection2High activity, good stability, no toxicity and no harm, in the technical scheme, the carbonized cigarette filter tip is used as a photocatalyst reaction platform, which is more beneficial to the attachment of escherichia coli and improves the inactivation efficiency, and the nano TiO is used2Generating photo-generated holes with oxidation property to convert oxygen molecules into active oxygen, generating oxygen free radicals from water, and performing redox reaction with Escherichia coli to inactivate it, and nanometer TiO2The method has the advantages of no toxicity, no mass loss, high utilization rate, no harm to human body, and applicability to human body for preventing Escherichia coli infection.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention takes the carbonized cigarette filter tip as the nanometer TiO2The load material enables waste consumables to be recycled, and provides a new green and economic use for daily waste;
(2) after the cigarette filter tip is carbonized, the inner super-porous structure of the cigarette filter tip can provide larger specific surface area and larger pore volume for loadingMore nano TiO2The particles provide a reaction platform for photocatalytic reaction, are more favorable for adhesion of reaction substances, and effectively improve photocatalytic efficiency;
(3) the cellulose acetate fiber of the cigarette filter can carbonize the nano TiO2The electron hole pairs are easy to separate, particle agglomeration is avoided, the photocatalytic reaction is continuously and stably carried out, and the photocatalytic efficiency can be effectively improved;
(4) the carbonized cigarette filter tip and the nano TiO of the invention2The product is completely harmless to human body, can be inactivated by oxidation-reduction reaction with Escherichia coli, has high inactivation efficiency, and can be used for preventing Escherichia coli infection.
Drawings
Fig. 1 is an SEM image of a carbonized cigarette filter prepared in example 1 of the present invention.
Fig. 2 is an SEM image of the nano titanium dioxide photocatalytic antibacterial material prepared in example 1 of the present invention.
Detailed Description
The drawings are only for purposes of illustration and are not to be construed as limiting the invention. For a better understanding of the following embodiments, certain features of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The preparation method of the nano titanium dioxide photocatalytic antibacterial material comprises the following steps: calcining the cigarette filter tip at high temperature to obtain a carbonized cigarette filter tip, immersing the carbonized cigarette filter tip into a titanium dioxide growth solution and stirring, placing the soaked carbonized cigarette filter tip under high temperature and high pressure for reaction, cooling, washing and drying the reaction product to obtain the carbonized cigarette filter tip loaded with nano TiO2An antibacterial material.
The method specifically comprises the following steps:
s1, placing the cigarette filter into a tube furnace, introducing inert gas, slowly heating to 700-900 ℃ at a speed of 10-20 ℃/min in an inert gas environment, keeping constant temperature, calcining for 20-40 min, and naturally cooling to obtain a carbonized cigarette filter;
s2, adding secondary distilled water into the surfactant, stirring until the secondary distilled water is fully dissolved, adjusting the pH value to 8-11, and adding a titanium dioxide precursor solution to prepare a titanium dioxide growth solution;
s3, soaking the carbonized cigarette filter tip into the titanium dioxide growth solution and stirring for 25-40 min;
s4, placing the carbonized cigarette filter tip soaked with the titanium dioxide growth solution into a hydrothermal reactor, heating the hydrothermal reactor to enable the titanium dioxide growth solution in the carbonized cigarette filter tip to react at high temperature and high pressure, naturally cooling after the reaction, and taking out a crude product;
s5, washing the crude product to be neutral, and drying to obtain the carbonized cigarette filter loaded with nano TiO2An antibacterial material.
In step S2, the surfactant is dodecylamine.
In step S2, the titania precursor solution is a titanium (iv) isopropoxide salt solution.
In step S2, Ti in the titania growth solution4+The concentration of the ions was 0.25 mol/L.
In step S4, the hydrothermal reactor is heated to 120-180 ℃.
In step S5, the crude product is washed to neutrality and then dried at 70-90 ℃.
The prepared carbonized cigarette filter tip carries nano TiO2The antibacterial material is tested by inactivating escherichia coli to evaluate the photocatalytic efficiency and the escherichia coli inactivating effect of the antibacterial material, and the specific test method comprises the following steps:
sterilizing the container and nutrient agar plate at 121 deg.C for 20min, inoculating Escherichia coli into the nutrient agar plate, culturing at 37 deg.C for one day, adding 10ml sterile physiological saline solution, and diluting to obtain bacteria with concentration of 108CFU/ml bacterial suspension, and adding 8mg of the prepared carbonized cigarette filter tip loaded with nano TiO into the bacterial suspension under aseptic condition2Antibacterial material, after 70 minutes of simulated sunlight irradiation at room temperature using a 300 watt xenon lamp, the bacterial suspension is diluted 10 times with sterile physiological saline, and 10. mu.L of the diluted bacterial suspension is spreadCulturing on sterilized nutrient agar plate at 37 deg.C in dark environment for 12 hr, and counting the number of viable Escherichia coli colonies; the test method is repeated for three times to obtain the number of the counted and surviving escherichia coli colonies, and the number is averaged to obtain the photocatalytic efficiency and escherichia coli inactivation effect of the material.
The method provided by the invention carbonizes the cigarette filter tip which is daily waste to be used as nano TiO2The inner super-porous structure provides larger specific surface area and larger pore volume to load more nano TiO2The particles are more beneficial to the attachment of reaction substances, a reaction platform is provided for photocatalytic reaction, and the acetate fibers of the filter tip carbonize to ensure that the nano TiO2The electron hole pair is easier to separate, particle agglomeration is avoided, the photocatalytic reaction is continuously and stably carried out, the photocatalytic efficiency can be effectively improved, the photocatalytic efficiency is completely harmless to a human body, the photocatalytic efficiency can be inactivated by carrying out an oxidation-reduction reaction with escherichia coli, the inactivation efficiency is high, and the method can be applied to the human body to prevent escherichia coli infection.
Example 1
In this embodiment, a preparation method of a nano titanium dioxide photocatalytic antibacterial material specifically includes the following steps:
s1, placing the cigarette filter into a tube furnace, introducing inert gas, slowly heating to 800 ℃ at a speed of 15 ℃/min under the inert gas environment, keeping constant temperature, calcining for 30min, and naturally cooling to obtain a carbonized cigarette filter;
s2, adding secondary distilled water into surfactant dodecylamine, stirring until the secondary distilled water is fully dissolved, adjusting the pH value to 8, and adding titanium (IV) isopropoxide salt solution to enable Ti in the titanium dioxide growth solution4+The concentration of the ions is 0.25mol/L, and a titanium dioxide growth solution is prepared;
s3, dipping the carbonized cigarette filter tip into the titanium dioxide growth solution and stirring for 30 min;
s4, placing the carbonized cigarette filter tip soaked with the titanium dioxide growth solution into a hydrothermal reactor, placing the carbonized cigarette filter tip into an oven, heating the hydrothermal reactor to 120 ℃, enabling the titanium dioxide growth solution in the carbonized cigarette filter tip to react at high temperature and high pressure, naturally cooling after the reaction, and taking out a crude product;
s5 washing the crude product with redistilled water and absolute ethyl alcohol respectively to neutrality, and drying at 80 ℃ to obtain the carbonized cigarette filter-tip loaded nano TiO2An antibacterial material.
The carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material is subjected to repeated 3 experiments by adopting the test method for inactivating escherichia coli, and the number of counted and surviving escherichia coli bacterial colonies is averaged to obtain that 49% of bacterial colonies still survive after photocatalytic inactivation of the carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material.
Example 2
In this embodiment, a preparation method of a nano titanium dioxide photocatalytic antibacterial material specifically includes the following steps:
s1, placing the cigarette filter into a tube furnace, introducing inert gas, slowly heating to 700 ℃ at the speed of 10 ℃/min under the inert gas environment, keeping constant temperature, calcining for 40min, and naturally cooling to obtain a carbonized cigarette filter;
s2, adding secondary distilled water into surfactant dodecylamine, stirring until the secondary distilled water is fully dissolved, adjusting the pH value to 9, and adding titanium (IV) isopropoxide salt solution to enable Ti in the titanium dioxide growth solution4+The concentration of the ions is 0.25mol/L, and a titanium dioxide growth solution is prepared;
s3, dipping the carbonized cigarette filter tip into the titanium dioxide growth solution and stirring for 25 min;
s4, placing the carbonized cigarette filter tip soaked with the titanium dioxide growth solution into a hydrothermal reactor, placing the carbonized cigarette filter tip into an oven to heat the hydrothermal reactor to 140 ℃, enabling the titanium dioxide growth solution in the carbonized cigarette filter tip to react at high temperature and high pressure, naturally cooling after the reaction, and taking out a crude product;
s5, washing the crude product to neutrality by using secondary distilled water and absolute ethyl alcohol respectively, and drying at 70 ℃ to obtain the carbonized cigarette filter-tip loaded nano TiO2An antibacterial material.
The carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material is subjected to repeated experiments for 3 times by adopting the test method for inactivating escherichia coli, and the number of counted and surviving escherichia coli bacterial colonies is averaged to obtain that 54% of bacterial colonies still survive after photocatalytic inactivation of the carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material.
Example 3
In this embodiment, a preparation method of a nano titanium dioxide photocatalytic antibacterial material specifically includes the following steps:
s1, placing the cigarette filter into a tube furnace, introducing inert gas, slowly heating to 750 ℃ at the speed of 20 ℃/min under the inert gas environment, keeping constant temperature, calcining for 20min, and naturally cooling to obtain a carbonized cigarette filter;
s2, adding secondary distilled water into surfactant dodecylamine, stirring until the secondary distilled water is fully dissolved, adjusting the pH value to 10, and adding titanium (IV) isopropoxide salt solution to enable Ti in the titanium dioxide growth solution4+The concentration of the ions is 0.25mol/L, and a titanium dioxide growth solution is prepared;
s3, dipping the carbonized cigarette filter tip into the titanium dioxide growth solution and stirring for 40 min;
s4, placing the carbonized cigarette filter tip soaked with the titanium dioxide growth solution into a hydrothermal reactor, placing the carbonized cigarette filter tip into an oven to heat the hydrothermal reactor to 160 ℃, enabling the titanium dioxide growth solution in the carbonized cigarette filter tip to react at high temperature and high pressure, naturally cooling after the reaction, and taking out a crude product;
s5, washing the crude product to be neutral by using secondary distilled water and absolute ethyl alcohol respectively, and drying at 90 ℃ to obtain the carbonized cigarette filter tip loaded with nano TiO2An antibacterial material.
The carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material is subjected to repeated 3 experiments by adopting the test method for inactivating escherichia coli, and the number of counted and surviving escherichia coli bacterial colonies is averaged to obtain that 45% of bacterial colonies still survive after photocatalytic inactivation of the carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material.
Example 4
In this embodiment, a preparation method of a nano titanium dioxide photocatalytic antibacterial material specifically includes the following steps:
s1, placing the cigarette filter into a tube furnace, introducing inert gas, slowly heating to 900 ℃ at a speed of 15 ℃/min under the inert gas environment, keeping constant temperature, calcining for 40min, and naturally cooling to obtain a carbonized cigarette filter;
s2, adding secondary distilled water into surfactant dodecylamine, stirring until the secondary distilled water is fully dissolved, adjusting the pH value to 11, and adding titanium (IV) isopropoxide salt solution to enable Ti in the titanium dioxide growth solution4+The concentration of the ions is 0.25mol/L, and a titanium dioxide growth solution is prepared;
s3, dipping the carbonized cigarette filter tip into the titanium dioxide growth solution and stirring for 30 min;
s4, placing the carbonized cigarette filter tip soaked with the titanium dioxide growth solution into a hydrothermal reactor, placing the carbonized cigarette filter tip into an oven to heat the hydrothermal reactor to 180 ℃, enabling the titanium dioxide growth solution in the carbonized cigarette filter tip to react at high temperature and high pressure, naturally cooling after the reaction, and taking out a crude product;
s5 washing the crude product with redistilled water and absolute ethyl alcohol respectively to neutrality, and drying at 80 ℃ to obtain the carbonized cigarette filter-tip loaded nano TiO2An antibacterial material.
The carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material is subjected to repeated experiments for 3 times by adopting the test method for inactivating escherichia coli, and the number of counted and surviving escherichia coli bacterial colonies is averaged to obtain that 46% of bacterial colonies still survive after photocatalytic inactivation of the carbonized cigarette filter tip loaded nano titanium dioxide antibacterial material.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the technical solutions of the present invention, and are not intended to limit the specific embodiments of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention claims should be included in the protection scope of the present invention claims.
Claims (10)
1. Preparation method of nano titanium dioxide photocatalytic antibacterial material and nano titanium dioxide photocatalytic antibacterial materialCharacterized in that the carbonized cigarette filter tip is obtained by calcining the cigarette filter tip at high temperature, the carbonized cigarette filter tip is dipped into the titanium dioxide growth solution and stirred, the soaked carbonized cigarette filter tip is placed under high temperature and high pressure for reaction and then cooled, and the reaction product is washed and dried to obtain the carbonized cigarette filter tip loaded with nano TiO2An antibacterial material.
2. The preparation method of the nano titanium dioxide photocatalytic antibacterial material according to claim 1 is characterized by comprising the following steps:
s1, placing the cigarette filter into a tube furnace, introducing inert gas, slowly heating to 700-900 ℃ at a speed of 10-20 ℃/min in an inert gas environment, keeping constant temperature, calcining for 20-40 min, and naturally cooling to obtain a carbonized cigarette filter;
s2, adding secondary distilled water into the surfactant, stirring until the secondary distilled water is fully dissolved, adjusting the pH value to 8-11, and adding a titanium dioxide precursor solution to prepare a titanium dioxide growth solution;
s3, soaking the carbonized cigarette filter tip into the titanium dioxide growth solution and stirring for 25-40 min;
s4, placing the carbonized cigarette filter tip soaked with the titanium dioxide growth solution into a hydrothermal reactor, heating the hydrothermal reactor to enable the titanium dioxide growth solution in the carbonized cigarette filter tip to react at high temperature and high pressure, naturally cooling after the reaction, and taking out a crude product;
s5, washing the crude product to be neutral, and drying to obtain the carbonized cigarette filter loaded with nano TiO2An antibacterial material.
3. The method for preparing nano titanium dioxide photocatalytic antibacterial material according to claim 2, wherein in step S1, the temperature is slowly raised to 800 ℃ at a rate of 15 ℃/min under inert gas environment, the temperature is maintained at constant temperature, the material is calcined for 30min and then naturally cooled to obtain the carbonized cigarette filter.
4. The method for preparing nano titanium dioxide photocatalytic antibacterial material according to claim 2, wherein in step S2, the surfactant is dodecylamine.
5. The method for preparing nano titanium dioxide photocatalytic antibacterial material according to claim 2, wherein in step S2, the titanium dioxide precursor solution is titanium (iv) isopropoxide salt solution.
6. The method of claim 2, wherein in step S2, Ti in the titanium dioxide growth solution is4+The concentration of the ions was 0.25 mol/L.
7. The method for preparing nano titanium dioxide photocatalytic antibacterial material according to claim 2, wherein in step S4, the hydrothermal reactor is heated to 120-180 ℃.
8. The method for preparing the nano titanium dioxide photocatalytic antibacterial material according to claim 2, wherein in step S5, the crude product is washed to be neutral and then dried at 70-90 ℃.
9. The nano titanium dioxide photocatalytic antibacterial material is prepared by the method according to any one of claims 1 to 8, and comprises a carbonized cigarette filter and nano titanium dioxide, wherein the nano titanium dioxide is loaded on the surface and pore channels of the carbonized cigarette filter.
10. The use of the nano titanium dioxide photocatalytic antibacterial material as claimed in claim 9, wherein the nano titanium dioxide photocatalytic antibacterial material is used for inactivating escherichia coli.
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