CN114766512B - Preparation method of inorganic nano material with high efficiency and lasting disinfection and sterilization - Google Patents
Preparation method of inorganic nano material with high efficiency and lasting disinfection and sterilization Download PDFInfo
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Abstract
The invention discloses a preparation method of an inorganic nano material with high efficiency and lasting disinfection, which comprises the steps of firstly growing a compact ultrathin zinc organic frame heterostructure in situ to realize effective adsorption and activation of O at metal positions under sunlight 2 OH and OH ‑ Forming a strong oxidative active radical; further preparing a bimetallic coupling silver-zinc organic framework heterogeneous material through Ag ion exchange, providing rich antibacterial active sites, promoting interfacial transfer between electrons and killing oxidative stress generation of bacteria; ag in solution + Zn on catalyst surface 2+ The superfine AgZn nano alloy particle enlarging material has broad antibacterial spectrum and antibacterial rate. The preparation method is simple in process and mild in reaction condition; the raw materials and the equipment are cheap and easy to obtain, and the cost is low; short synthesis time, high efficiency, lasting and safe broad-spectrum antibacterial disinfection, and suitability for large-scale production.
Description
Technical Field
The invention belongs to the field of nano material preparation and photocatalysis, and in particular relates to a preparation method of an inorganic nano material with high efficiency and lasting disinfection.
Background
Each epidemic situation is a great test for human beings, and the invention of the disinfectant promotes the development of health and sanitation industries of various countries in the world. In order to meet the huge demand of disinfectant and the high requirement on sterilization and disinfection effects, the development of efficient, durable disinfection and low-toxicity disinfectant is urgent. The national Wei Jian commission proposal shows that the disinfectant capable of effectively killing viruses at present is mainly a medium-high-efficiency disinfectant, which comprises the following components: chlorine-containing compound disinfectant, peroxide disinfectant and alcohol disinfectant. The action mechanism of the chlorine-containing disinfectant represented by 84 disinfectant is to oxidize bacteria/virus nucleic acid substances by self strong oxidizing property so as to kill the bacteria/virus nucleic acid substances. The main representative product of the alcohol disinfectant is 75% ethanol, which kills bacteria or inactivates viruses by dehydrating or dissolving viral lipid coating by pathogenic microorganisms. Peroxide disinfectants include hydrogen peroxide, peracetic acid, chlorine dioxide, and the like, which utilize strong oxidizing properties to kill microorganisms to which they are sensitive. However, the existing disinfectants on the market have more or less defects, such as irritation, corrosiveness and instability of chlorine-containing disinfectant, the effective concentration of alcohol needs to be kept above 75%, strict requirements on storage environment are met, and phenolic disinfectant and quaternary ammonium salt disinfectant are ineffective against coronavirus. In recent years, in order to develop efficient, durable and low-toxicity disinfectants, some novel sterilization and disinfection materials are receiving more and more attention, such as metal nanoparticles, metal Organic Frameworks (MOFs) and semiconductor photocatalysts. Among them, ag nanoparticles (Ag NPs) are widely studied as broad-spectrum antibacterial agents capable of releasing ag+ to destroy bacterial membranes, interfere with DNA/RNA replication, thereby destroying bacteria, and do not produce resistant bacteria. The MOF has large specific surface area and rich metal nodes, can release metal ions in the solution, and has remarkable effect of inhibiting colony growth. The super-oxygen free radical and the hydroxyl free radical generated by the semiconductor catalyst under the light excitation have remarkable killing effect on bacteria and viruses. The silver-zinc organic framework heterostructure is prepared through the structure of the metal ion antibacterial performance of Ag and MOFs and the ZnO semiconductor photocatalytic sterilization performance, has high-efficiency metal ion release capacity and strong photothermal conversion effect, and has high-efficiency and durable antibacterial effect on escherichia coli, staphylococcus aureus and the like. The patent has important significance for developing high-efficiency disinfection products.
Disclosure of Invention
The invention aims at providing an inorganic nano material with high efficiency and lasting disinfection and sterilization, which is suitable for playing a great role in antibiosis and sterilization in various occasions and environments.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the inorganic nano material with high efficiency and lasting disinfection and sterilization comprises the following steps:
s1, uniformly stirring 4-20 parts by mass of a matrix material, 2 parts by mass of zinc acetate dihydrate and 2 parts by mass of an organic framework material in N, N-dimethylformamide, performing solvothermal reaction at 90-160 ℃ for 6 hours, and performing centrifugal separation to obtain a zinc organic framework heterogeneous material;
s2, dispersing the obtained zinc organic framework heterogeneous material into a silver nitrate/methanol solution with the concentration of 3%, uniformly stirring the zinc organic framework heterogeneous material and the silver nitrate in a mass ratio of 100:1 in a dark environment, reacting for 5 minutes in an illumination condition, centrifugally drying to obtain a powder sample, and calcining for 1h at 340-400 ℃ in a reducing atmosphere to obtain the high-efficiency and durable disinfection and sterilization inorganic nano material.
Further, the matrix material of the step (1) is selected from ZnO and TiO 2 、WO 3 、SnO 2 、 ZrO 2 、Fe 2 O 3 、ZnS、SrTiO 3 Or SiO 2 。
Further, the organic framework material of the step (1) is selected from imidazole, 2-methylimidazole, 2-amino terephthalic acid, 1, 4-phthalic acid (PTA) and 2-hydroxy terephthalic acid (H) 2 BDC) or polyethylene glycol 20000 (PEG 20000).
Further, the illumination condition of the step (2) is illumination for 5-10 min under 400nm 300W xenon lamp.
Further, the reducing atmosphere in the step (2) is a mixed gas of hydrogen and argon, wherein the hydrogen accounts for 5-10%.
The invention has the beneficial effects that:
(1) The metal organic frame structure contributes to rich hole structures, so that the contact area of materials, bacteria and viruses can be increased, and the inactivation efficiency is improved.
(2) ZnO is used as a photocatalysis support body and is used as a metal node of metal organic frameworks MOFs and a source of ultra-small alloys, and in-situ growth of a compact ultra-thin zinc organic framework heterostructure can realize effective adsorption and activation of O by metal sites under sunlight 2 OH and OH - Forming strong oxidative active free radicals, providing antibacterial ability.
(3) On the basis of the porous metal organic framework material, double (multi) metal coupling is realized through silver ion exchange, ag-X (X is matrix metal) clusters or particles are generated by reduction in pore channels after calcination, and compared with single silver or other metal elements, the particles can provide richer antibacterial active sites, promote the generation of strong oxidative free radicals/oxidative stress (ROS), block the replication of virus DNA/RNA and destroy the cell structure of bacteria virus, and realize high-efficiency, lasting, safe and broad-spectrum antibacterial disinfection.
(4) Compared with the traditional silver antibacterial material, the particle size of the Ag-X clusters in the inorganic nano material obtained by the method is small and the Ag-X clusters are distributed in the pore channels of the material, so that the silver loading capacity is greatly reduced, and the inorganic nano material is more economical; meanwhile, most of silver is anchored on the material and cannot fall off, so that the antibacterial coating material has little influence on human bodies and environment.
(5) The method provided by the invention has the advantages of mild reaction conditions, simple operation process, short reaction period, and suitability for materials with environmental pollution, and is suitable for industrial production.
Drawings
FIG. 1 is a scanning electron microscope image of an inorganic nanomaterial with high-efficiency and durable disinfection and sterilization obtained in example 1 of the present invention;
FIG. 2 is an XRD pattern of the inorganic nanomaterial obtained in example 1 of the present invention that is highly effective and durable in disinfection and sterilization;
FIG. 3 is a graph showing the colony count of blank samples tested in example 1 of the present invention;
FIG. 4 shows colony counts of antibacterial samples tested on ZnO nanoplatelets used in example 1 of the present invention;
FIG. 5 shows the colony count of the antibacterial samples tested on the heterogeneous materials of the zinc organic frameworks obtained in example 1 of the present invention;
FIG. 6 shows the colony count of the antibacterial samples tested by the inorganic nanomaterial (AgZn@Ag-Zn-MOFs/ZnO) with high-efficiency and lasting disinfection and sterilization obtained in example 1 of the present invention.
Detailed Description
The invention will be further elucidated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is to be understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Example 1
(1) 200mg ZnO nano-sheets were combined with 100mg Zn (AC) 2 ·2H 2 O and 100mg of 2-methylimidazole are dissolved in 60mL of N, N-dimethylformamide and stirred for 30min, then the mixture is subjected to solvothermal reaction at 90 ℃ for 6h, and the mixture is subjected to centrifugal separation to prepare the Zn-MOFs/ZnO photocatalyst.
(2) Uniformly dispersing 30mg of Zn-MOFs/ZnO photocatalyst to contain 3wt% of AgNO 3 30 Stirring in the dark for 20 min, continuously stirring for 5min under illumination of 300W xenon lamp with wavelength of more than 400nm, centrifuging, and drying to obtain gray powder, and adding into a solvent, stirring under stirring to obtain a powder, stirring under stirring for 5min, and stirring under stirring to obtain a powder, wherein the powder is 5%H 2 Calcining for 1h at 370 ℃ in Ar atmosphere to obtain the inorganic nano material (AgZn@Ag-Zn-MOFs/ZnO) with high-efficiency and lasting disinfection and sterilization.
And (3) carrying out photocatalysis sterilization performance test on the obtained inorganic nano material: and adding an equal amount of target photocatalytic bactericide into the phosphate buffer solution containing the same concentration of escherichia coli, carrying out adsorption balance in a constant-temperature dark-state shaking table, irradiating with a 300W cold light source xenon lamp for 1h to kill bacteria, and uniformly coating 100 mu L of bacterial suspension on an agar plate. After one night of culture in a constant temperature incubator, a large number of colonies are observed to remain in the culture medium of the ZnO nano-sheets and the Zn-MOFs/ZnO photocatalyst (figures 3-5), and the number of colonies in the culture medium of the inorganic nano-material is zero (figure 6), which proves that the sterilization rate is more than 99%, and the culture medium has remarkable sterilization and disinfection performance.
Example 2
(1) 300mg ZnO nano-sheet was combined with 50mg Zn (AC) 2 ·2H 2 O and 50mg of 2-methylimidazole are dissolved in 60mL of N, N-dimethylformamide and stirred for 30min, then the mixture is subjected to solvothermal reaction at 100 ℃ for 6h, and the mixture is subjected to centrifugal separation to prepare the Zn-MOFs/ZnO photocatalyst.
(2) Uniformly dispersing 30mg of Zn-MOFs/ZnO nano-sheets to contain 3wt% of AgNO 3 In 30g of methanol solution, stirring in the dark for 30min, illuminating with 400nm 300W xenon lamp, stirring continuously for 10min, centrifuging, drying to obtain powder sample, and collecting powder in 10% H 2 Calcining for 1h at 340 ℃ in Ar atmosphere to obtain the inorganic nano material (AgZn@Ag-Zn-MOFs/ZnO) with high-efficiency and lasting disinfection and sterilization.
The antibacterial property was tested according to the method of example 1, and the number of colonies in the culture medium of the inorganic nanomaterial was observed to be zero, demonstrating that the sterilization rate was >99%, and the antibacterial property was remarkable.
Example 3
(1) 200mg of TiO 2 Nanotube and 20mg Zn (AC) 2 ·2H 2 O and 20mg of 2-methylimidazole are dissolved in 60mL of N, N-dimethylformamide and stirred for 30min, and then reacted for 6h at 160 ℃ in a solvothermal mode, and the Zn-MOFs/TiO is prepared by centrifugal separation 2 A photocatalyst.
(2) 30mg of Zn-MOFs/TiO 2 Uniformly dispersed to contain 3wt% AgNO 3 In 30g of methanol solution, stirring in the dark for 20 min, illuminating with 400nm 300W xenon lamp, stirring continuously for 5min, centrifuging, drying to obtain powder sample, and concentrating the powder in 10% H 2 Calcining at 360 ℃ for 1h in Ar atmosphere to obtain the inorganic nano material (AgZn@Ag-Zn-MOFs/TiO) with high-efficiency and lasting disinfection and sterilization 2 )。
The antibacterial property was tested according to the method of example 1, and the number of colonies in the culture medium of the inorganic nanomaterial was observed to be zero, demonstrating that the sterilization rate was >99%, and the antibacterial property was remarkable.
Example 4
(1) 120mg of WO 3 Nanoplatelets and 20mg Zn (AC) 2 ·2H 2 O and 20mg of polyvinyl alcohol 20000 are dissolved in 60mL of N, N-dimethylformamide and stirred for 30min, then the mixture is subjected to solvothermal reaction at 150 ℃ for 6h, and the mixture is centrifugally separated to prepare Zn-MOFs/WO 3 A photocatalyst.
(2) 30mg of Zn-MOFs/WO 3 Uniformly dispersed to contain 3wt% AgNO 3 In 30g of methanol solution, stirring in the dark for 20 min, illuminating with 400nm 300W xenon lamp, stirring continuously for 5min, centrifuging, drying to obtain powder sample, and concentrating the powder in 10% H 2 Calcining at 400 ℃ for 1h in Ar atmosphere to obtain the inorganic nano material (AgZn@Ag-Zn-MOFs/WO) with high-efficiency and lasting disinfection and sterilization 3 )。
The antibacterial property was tested according to the method of example 1, and the number of colonies in the culture medium of the inorganic nanomaterial was observed to be zero, demonstrating that the sterilization rate was >99%, and the antibacterial property was remarkable.
Example 5
(1) 150mg SnO 2 Nanoplatelets and 20mg Zn (AC) 2 ·2H 2 O and 20mg of 1, 4-phthalic acid (PTA) are dissolved in 60mL of N, N-dimethylformamide and stirred for 30min, and then reacted for 6h at 150 ℃ in a solvothermal mode, and the Zn-MOFs/SnO is prepared by centrifugal separation 2 A photocatalyst.
(2) 30mg of Zn-MOFs/SnO 2 Uniformly dispersed to contain 3wt% AgNO 3 In 30g of methanol solution, stirring in the dark for 20 min, illuminating with 400nm 300W xenon lamp, stirring continuously for 5min, centrifuging, drying to obtain powder sample, and concentrating the powder in 10% H 2 Calcining at 400 ℃ for 1h in Ar atmosphere to obtain the inorganic nano material (AgZn@Ag-Zn-MOFs/SnO) with high-efficiency and lasting disinfection and sterilization 2 )。
The antibacterial property was tested according to the method of example 1, and the number of colonies in the culture medium of the inorganic nanomaterial was observed to be zero, demonstrating that the sterilization rate was >99%, and the antibacterial property was remarkable.
Claims (3)
1. The preparation method of the inorganic nano material with high efficiency and lasting disinfection and sterilization is characterized by comprising the following steps:
(1) Uniformly stirring 4-20 parts by mass of matrix material, 2 parts by mass of zinc acetate dihydrate and 2 parts by mass of organic framework material in N, N-dimethylformamide, performing solvothermal reaction at 90-160 ℃ for 6 hours, and performing centrifugal separation to obtain a zinc organic framework heterogeneous material; the matrix material is selected from ZnO and TiO 2 、WO 3 、SnO 2 、ZrO 2 、Fe 2 O 3 、ZnS、SrTiO 3 Or SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The organic framework material is selected from imidazole, 2-methylimidazole, 2-amino terephthalic acid, 1, 4-phthalic acid, 2-hydroxy terephthalic acid or polyethylene glycol 20000;
(2) Dispersing the obtained zinc organic framework heterogeneous material into a silver nitrate/methanol solution with the mass fraction of 3%, uniformly stirring the zinc organic framework heterogeneous material and the silver nitrate in a dark environment, reacting for 5 minutes under the illumination condition, centrifugally drying to obtain a powder sample, and calcining for 1 hour at 340-400 ℃ in a reducing atmosphere to obtain the high-efficiency and durable disinfection and sterilization inorganic nano material.
2. The method according to claim 1, wherein the illumination condition of the step (2) is 300W xenon lamp illumination with a wavelength equal to 400nm for 5-10 minutes.
3. The method according to claim 1, wherein the reducing atmosphere in the step (2) is a mixture of hydrogen and argon, and the hydrogen accounts for 5-10%.
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