CN111194749A - Preparation method and application of zinc zeolite antibacterial material - Google Patents
Preparation method and application of zinc zeolite antibacterial material Download PDFInfo
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- CN111194749A CN111194749A CN202010042229.7A CN202010042229A CN111194749A CN 111194749 A CN111194749 A CN 111194749A CN 202010042229 A CN202010042229 A CN 202010042229A CN 111194749 A CN111194749 A CN 111194749A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
Abstract
The invention discloses a preparation method and application of a zinc zeolite antibacterial material, belonging to the technical field of antibacterial materials, wherein the preparation method of the antibacterial material comprises the following steps: weighing zeolite powder, adding ZnCl2Shaking the solution to fully perform ion exchange, centrifuging, washing with distilled water until the washing solution is Zn-free2+Ionizing and drying to obtain zinc zeolite complex powder; in the nanometer TiO2Adding deionized water and Ce (NO)3)3Dispersing for later use; adding zinc zeolite complex powder to Ce/TiO2Adding dilute HNO into the matrix3Regulating the pH value of the reaction solution, stirring in a constant-temperature water bath at 60-70 ℃ for 0.5h, taking out, filtering,drying, roasting at 800 deg.C under 300-2The antibacterial material can be applied to disinfection products or antibacterial products, and has the advantages of mould resistance, moisture resistance and good stability.
Description
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to a preparation method and application of a zinc zeolite antibacterial material.
Background
Along with the continuous improvement of the life quality of people, the application of the antibacterial material is wider and wider. Many researches show that the silver-based antibacterial agent has a good inhibition effect on bacteria and mould and has wide research and application in various fields. With the widespread use of silver, people are increasingly exposed to silver ions. As a heavy metal element which is not needed by human body, the silver ion can generate toxic action when being accumulated in the human body too much. In addition, silver-based antibacterial agents are expensive, and silver ions are unstable and are easily reduced and deposited to cause color change, so that the development of other inorganic antibacterial agents is of great significance. Heavy metal ions all have certain antibacterial effect, but the better effect is silver, copper and zinc. The use of copper ions is greatly limited because of their severe color impact; the zinc is a necessary trace element for human body, the zinc participates in the metabolic process of more than 80 enzymes in the human body, is an essential substance in important physiological processes of growth and development, reproductive inheritance, immune endocrine, nerve, body fluid and the like of the human body, and the zinc deficiency can generate adverse effect on each system of the human body. Therefore, the method for preparing the antibacterial material by using the zinc ions is a good method for killing two birds with one stone when being applied to the daily life of people.
The antibacterial zeolite is prepared by taking zeolite as a substrate and connecting bactericidal metal ions, is a multifunctional material, and has the functions of acid resistance, alkali resistance, long-acting and broad-spectrum sterilization and bacteriostasis. It has excellent bactericidal effect on colibacillus, mold, hot fatty bacillus, Bacillus subtilis, etc. At present, various natural and synthetic zeolites have been studied, and methods for preparing antibacterial zeolites by a dry-wet cycle method, a liquid phase ion exchange method, a solid phase reaction method, and the like have been explored.
The photocatalytic antibacterial material is TiO2、ZrO2ZnO, etc. Among these photocatalytic materials, TiO is the most studied2A series of antibacterial materials. As photocatalytic materialTiO2Mainly has two crystal forms, one is anatase type TiO2Its forbidden band width is 3.2 ev; the other is rutile type TiO2Its forbidden band width is about 3.0 ev. Photoexcitation causes valence band electrons to transit to the conduction band, where it is the excited electrons that have strong reducibility, and the holes in the valence band have strong oxidizing power. Anatase type TiO2At PH 1, the band gap is 312ev, which corresponds to the energy of light having a wavelength of 400nm, and under the irradiation of ultraviolet light (the wavelength of ultraviolet light is 387.5nm), radiation having an energy higher than the forbidden band width thereof is absorbed, and valence band electrons are transited to the conduction band, so that holes are formed in the valence band, and electrons, that is, hole-electron pairs, are formed in the conduction band. Due to the energy level bending of the surface space charge layer, holes form a potential drop along the surface and move to the surface. The holes attract electrons and have an oxidizing ability. Due to energy transfer, active oxygen such as free radicals and superoxide ions with strong activity are formed to induce photocatalytic reaction, have photocatalytic ability and can sterilize bacteria.
In view of the above, the present invention provides a preparation method and an application of a novel zinc zeolite antibacterial material.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the preparation method and the application of the zinc zeolite antibacterial material, which have the advantages of mildew resistance, moisture resistance and good stability and overcome the defects of high cost, poor effect and the like of the traditional antibacterial material.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a zinc zeolite antibacterial material comprises the following steps:
s1 preparation of Zinc Zeolite Complex powder
Weighing 10-13.5g of zeolite powder with the particle size of less than 0.12mm, and adding 1-2mol/L ZnCl2Shaking the solution 50ml at 40-70 deg.C for 2-10h to fully perform ion exchange, centrifuging, washing with distilled water until the washing solution is Zn-free2+Ionizing, and drying the washed zeolite powder at 75-95 ℃ to obtain zinc zeolite complex powder;
S2、Ce/TiO2preparation of the substrate
In the nanometer TiO2Adding deionized water and then according to TiO2With Ce (NO)3)3The ratio of the amounts of substances (A) to (B) is 20-80: 1, adding Ce (NO)3)3Dispersing for 15-50min by an ultrasonic oscillator to obtain Ce/TiO2A substrate;
s3, Zinc Zeolite-Ce/TiO2Preparation of antibacterial material
Adding the zinc zeolite complex powder prepared in step S1 to the Ce/TiO zeolite complex powder prepared in step S22Adding dilute HNO into the matrix3Regulating the pH value of the reaction solution to control the pH value of the reaction solution to be 3-11, stirring for 0.5h in a constant-temperature water bath at 60-70 ℃, taking out, filtering in a suction filtration mode by using a Buchner funnel, drying for 2h in a blast drying box, roasting for 2h at 800 ℃ in a muffle furnace, and grinding to obtain the zinc zeolite-Ce/TiO2An antibacterial material.
Through the technical scheme, the zeolite powder plays a good adsorption role, and the surface of the zinc zeolite is coated with a layer of uniformly distributed nano TiO2And the zinc zeolite-Ce/TiO formed2The antibacterial material is still in a nanometer level, has good inhibition effect on escherichia coli and mould, has good stability, and is simple in preparation method. Introduction of Ce into TiO2Within the lattice structure, thereby introducing new charges into the lattice, forming defects or changing the type of lattice, influencing the movement of photogenerated electrons and holes, adjusting their distribution or changing the TiO2Band structure of (3), ultimately resulting in TiO2The photocatalytic activity of the compound is changed.
More preferably: the nano TiO2The mass is 3g, and the deionized water is 100 ml.
More preferably: in step S3, the buchner funnel includes a funnel body and a cartridge, the funnel body includes an outer cylinder and a tube connected to the bottom of the outer cylinder, the cartridge is detachably mounted in the outer cylinder, and the cartridge is used for placing the material to be suction filtered.
More preferably: the cylinder core comprises an inner cylinder and an inner pipe, the top of the inner cylinder is open, a filter plate is fixed at the bottom of the inner cylinder, the filter plate is gradually sunken towards the middle part, a water outlet and a central opening are formed in the filter plate, the central opening is positioned in the center of the filter plate, and the water outlet is communicated with the central opening;
the inner tube is fixed at the bottom of the filter plate and inserted in the tube body, and the inner tube is communicated with the inner tube through the water outlet and the central opening.
More preferably: the water outlets are uniformly distributed around the central opening, and the width of the water outlets gradually narrows towards the direction close to the central opening.
More preferably: the inner tube top is fixed with the journal stirrup, the journal stirrup sets up the relative both sides of inner tube, urceolus top both sides seted up with the corresponding breach of journal stirrup, the journal stirrup supports in the breach.
More preferably: and bearing platforms are fixed on the periphery of the inner wall of the outer barrel, the bearing platforms are positioned at the lower part of the outer barrel, and the filter plate is supported on the bearing platforms.
More preferably: the cushion cap is supported at the peripheral edge of the filter plate, and the upper surface of the filter plate is arc-shaped and is matched with the bottom surface of the filter plate.
The application of the zinc zeolite antibacterial material is to apply the prepared zinc zeolite antibacterial material to disinfection products or antibacterial products.
In conclusion, the invention has the following beneficial effects: nano TiO 22Has the advantages of high activity, high antibacterial speed, good thermal stability, long-term effectiveness, low price, no harm to human bodies and the like, thereby becoming an inorganic antibacterial material which is most concerned. However, nano TiO2The zinc zeolite is used as a carrier and the nano TiO is used as the carrier, so that the agglomeration phenomenon can occur to cause different particle diameters of the particles2The cerium is doped as a main raw material, and a certain antibacterial and mildewproof effect is generated by photocatalysis, so that the antibacterial material with antibacterial, mildewproof, moisture-proof and good stability is prepared. Compared with the traditional antibacterial material, the zinc zeolite-Ce/TiO prepared by the invention2The zeolite powder has good adsorption effect, and the surface of the zinc zeolite is coated with a layer of uniformly distributed nano TiO2And the zinc zeolite-Ce/TiO formed2The antibacterial material is still in a nanometer level, has good inhibition effect on escherichia coli and mould, good stability and simple preparation method.
Drawings
FIG. 1 is a block diagram of a Buchner funnel of example 1, which is mainly used to embody the external structure of the Buchner funnel;
FIG. 2 is a top view of the Buchner funnel of example 1, which is mainly used to embody the structure of the Buchner funnel;
fig. 3 is a sectional view of the buchner funnel of example 1, mainly used to embody the internal structure of the buchner funnel;
FIG. 4 is a structural diagram of a Buchner funnel in example 1, which is mainly used for embodying the structure of the funnel body;
FIG. 5 is a structural diagram of a Buchner funnel of example 1, which is mainly used for embodying the structure of a cartridge core;
FIG. 6 shows the Zn zeolite-Ce/TiO of example 12-1 comparison of antibacterial effect with blank control, wherein the upper part of the picture is the antibacterial effect of the blank control, and the lower part of the picture is zinc zeolite-Ce/TiO2-1 antibacterial effect profile;
FIG. 7 shows the Zn zeolite-Ce/TiO of example 22-2 comparison of antibacterial effect with blank control, wherein the upper part of the picture is the antibacterial effect of the blank control, and the lower part of the picture is zinc zeolite-Ce/TiO2-2 antibacterial effect profile;
FIG. 8 is the Zinc Zeolite-Ce/TiO of example 32-3 comparison of antibacterial effect with blank control, wherein the upper part of the picture is the antibacterial effect of the blank control, and the lower part of the picture is zinc zeolite-Ce/TiO2-3 antibacterial effect profile;
FIG. 9 shows the Zn zeolite-Ce/TiO of example 42-4 comparison of antibacterial effect with blank control, wherein the upper part of the picture is the antibacterial effect of the blank control, and the lower part of the picture is zinc zeolite-Ce/TiO2-4 antibacterial effect profile;
FIG. 10 shows the Zn zeolite-Ce/TiO of example 52-5 comparison of antibacterial effect with blank control, wherein the upper part of the picture is the antibacterial effect of the blank control, and the lower part of the picture is zinc zeolite-Ce/TiO2-5 antibacterial effect profile.
In the figure, 1, a funnel body; 11. an outer cylinder; 12. a pipe body; 13. a bearing platform; 14. a notch; 2. a barrel core; 21. an inner barrel; 22. supporting a lug; 23. filtering the plate; 24. a water outlet; 25. a central opening; 26. an inner tube.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1: a preparation method of a zinc zeolite antibacterial material comprises the following steps:
s1 preparation of Zinc Zeolite Complex powder
Weighing 10g of zeolite powder with the particle size of less than 0.12mm, and adding 1mol/L ZnCl250ml of the solution was shaken at 40 ℃ for 5 hours to sufficiently perform ion exchange, and then centrifuged, and washed with distilled water until the washing solution was Zn-free2+Ionizing, and drying the washed zeolite powder at 75 ℃ to obtain zinc zeolite complex powder-1;
S2、Ce/TiO2preparation of the substrate
Weighing 3g of nano TiO2Then in the presence of nano TiO2Adding 100ml deionized water, and adding into TiO2With Ce (NO)3)3The ratio of the amounts of substances (a) to (b) is 20: 1, adding proper amount of Ce (NO)3)3Dispersing for 15min by an ultrasonic oscillator to obtain Ce/TiO2-1 a substrate;
s3, Zinc Zeolite-Ce/TiO2Preparation of antibacterial material
Adding the zinc zeolite complex powder-1 prepared in step S1 to the Ce/TiO prepared in step S22-1 matrix, adding dilute HNO3Adjusting pH of the reaction solution to 7, stirring in 60 deg.C constant temperature water bath for 0.5 hr, taking out, filtering with Buchner funnel, drying in forced air drying oven for 2 hr, and passing through muffle furnace at 5 deg.CRoasting at 00 deg.C for 2h, grinding to obtain antibacterial material zinc zeolite-Ce/TiO applicable to disinfection product or antibacterial product2-1。
Referring to fig. 1-5, in step S3, a buchner funnel includes a funnel body 1 and a cartridge 2. The funnel body 1 comprises an outer cylinder 11 and a pipe body 12 connected to the bottom of the outer cylinder 11, wherein the pipe body 12 is used for being inserted into a filter flask and being connected with the filter flask in a sealing mode. The upper end of the tube body 12 is fixed at the center of the bottom of the outer cylinder 11, the lower end is an inclined opening so that liquid can drip down, and the tube body 12 is communicated with the outer cylinder 11. The cylinder core 2 is detachably arranged in the outer cylinder 11, and the cylinder core 2 is used for placing materials to be subjected to suction filtration.
In above-mentioned technical scheme, traditional buchner funnel only has urceolus 11 and body 12, and the suction filtration in-process needs often extract body 12 from the buchner flask to lay filter paper, place the material and wash buchner funnel etc. buchner funnel inserts repeatedly, extracts, can influence the use of buchner flask bottleneck seal cover, makes the seal cover appear warping, causes the leakproofness between funnel body 1 and the buchner flask relatively poor, thereby influences going on of suction filtration. In order to reduce the extraction frequency of the pipe body 12, the invention detachably installs the cylinder core 2 for placing the materials to be filtered and the filter paper in the outer cylinder 11, and prevents the filter paper and the materials to be filtered from contacting with the outer cylinder 11, so that the cylinder core 2 only needs to be cleaned during cleaning, the effect is better if the filter cylinder is matched with a filter flask with a pouring port in the side direction, the funnel body 1 does not need to be repeatedly extracted, and the extraction frequency of the funnel body 1 is reduced.
Referring to fig. 1-5, the cartridge 2 includes an inner cartridge 21 and an inner tube 26. The top of the inner cylinder 21 is open, the bottom is fixed with a filter plate 23, the filter plate 23 gradually sinks towards the middle, and the filter plate 23 is positioned between the inner cylinder 21 and the inner pipe 26. The filter plate 23 is provided with a water outlet 24 and a central opening 25, the central opening 25 is a circular hole and is positioned in the center of the filter plate 23, one end of the water outlet 24 is close to the peripheral edge of the filter plate 23, and the other end is communicated with the central opening 25. The water outlets 24 are arranged in a plurality, the water outlets 24 are uniformly distributed around the central opening 25, and the width of the water outlets 24 gradually narrows towards the direction close to the central opening 25. The inner tube 26 is fixed to the bottom of the filter sheet 23 and inserted into the tube body 12, and the inner tube 21 communicates with the inner tube 26 through the water outlet 24 and the center opening 25. Specifically, the inner tube 26 includes an upper funnel section, the top surface of which is fixed to the peripheral edge of the bottom of the filter plate 23, and a lower tubular section, which is inserted into the tube 12 and contacts the inner wall of the tube 12. In order to prevent the material to be filtered from contacting the tube 12 and to allow the liquid to flow out rapidly, specifically, the lower end surface of the tubular section is a bevel, and the length of the tubular section cannot be smaller than the length of the tube 12, i.e., the lower end of the tubular section either extends out of the tube 12 or is flush with the bottom surface of the tube 12.
In the above technical scheme, the inner cylinder 21 and the inner tube 26 are arranged, mainly in order to prevent the material to be subjected to suction filtration from polluting the funnel body 1 in the suction filtration process of the buchner funnel, and after the inner cylinder 21 and the inner tube 26 are inserted into the outer cylinder 11 and the tube body 12, the material to be subjected to suction filtration cannot be in contact with the outer cylinder 11 and the tube body 12, so that the outer cylinder 11 and the tube body 12 do not need to be cleaned in cleaning, and only the cylinder core 2 needs to be taken out for cleaning. During the suction filtration, filter paper needs to be laid on the surface of the filter plate 23, then materials to be subjected to suction filtration are placed on the filter paper, and the filter plate 23 gradually sinks towards the middle, so that after the filter paper is laid on the filter plate 23, the middle of the filter paper also gradually sinks downwards, the rapid suction filtration is facilitated, and the liquid downflow speed is improved. The traditional filter hole has slow liquid flowing speed and is easy to leave materials, but the invention adopts the mode of the water outlet 24+ the central port 25, so that the materials are not easy to leave, the cleaning is more convenient, and the pumping filtration speed is faster.
Referring to fig. 1-5, the top of the inner cylinder 21 is fixed with a support lug 22, the support lugs 22 are arranged on two opposite sides of the inner cylinder 21, two sides of the top of the outer cylinder 11 are provided with notches 14 corresponding to the support lugs 22, and the support lugs 22 are matched with the notches 14 and supported in the notches 14. The periphery of the inner wall of the outer cylinder 11 is fixed with a bearing platform 13, the bearing platform 13 is annular and is positioned at the lower part of the outer cylinder 11, the filter plate 23 is supported on the bearing platform 13, and the bearing platform 13 is positioned at the outer side of the funnel section of the inner tube 26. The bearing platform 13 is supported at the peripheral edge of the filter plate 23, and the upper surface of the filter plate 23 is arc-shaped and is matched with the bottom surface of the filter plate 23.
In the above technical solution, in order to better support the cylinder core 2, and in order that the inclined plane of the lower end surface of the inner tube 26 exactly corresponds to the inclined plane of the lower end of the tube body 12, the inner tube 21 is provided with the support lug 22, and the outer tube 11 is provided with the bearing platform 13, so as to better position and support the inner tube 21 and the inner tube 26.
Example 2: a preparation method of a zinc zeolite antibacterial material comprises the following steps:
s1 preparation of Zinc Zeolite Complex powder
Weighing 12.5g of zeolite powder with the particle size of less than 0.12mm, and adding 2mol/L ZnCl250ml of the solution was shaken at 60 ℃ for 5 hours to sufficiently perform ion exchange, and then centrifuged, and washed with distilled water until the washing solution was Zn-free2+Ionizing, and drying the washed zeolite powder at 80 ℃ to obtain zinc zeolite complex powder-2;
S2、Ce/TiO2preparation of the substrate
Weighing 3g of nano TiO2Then in the presence of nano TiO2Adding 100ml deionized water, and adding into TiO2With Ce (NO)3)3The ratio of the amounts of substances (a) to (b) is 40: 1, adding proper amount of Ce (NO)3)3Dispersing for 30min by an ultrasonic oscillator to obtain Ce/TiO2-2 a substrate;
s3, Zinc Zeolite-Ce/TiO2Preparation of antibacterial material
Adding the zinc zeolite complex powder-2 prepared in step S1 to the Ce/TiO prepared in step S22-2 matrix, adding dilute HNO3Regulating the pH value of the reaction solution to control the pH value of the reaction solution to be 3, stirring for 0.5h in a constant-temperature water bath at 60 ℃, taking out, filtering in a suction filtration mode by using a Buchner funnel, drying for 2h in a blast drying oven, roasting for 2h at 300 ℃ by using a muffle furnace, and grinding to obtain the antibacterial material zinc zeolite-Ce/TiO applicable to disinfection products or antibacterial products2-2。
Example 3: a preparation method of a zinc zeolite antibacterial material comprises the following steps:
s1 preparation of Zinc Zeolite Complex powder
Weighing 13g of zeolite powder with the particle size of less than 0.12mm, and adding 1mol/L ZnCl250ml of the solution was shaken at 55 ℃ for 5 hours to sufficiently perform ion exchange, and then centrifuged, and washed with distilled water until the washing solution was Zn-free2+Ionizing, and drying the washed zeolite powder at 85 ℃ to obtain zinc zeolite complex powder-3;
S2、Ce/TiO2preparation of the substrate
Weighing 3g of nano TiO2Then in the presence of nano TiO2Adding 100ml deionized water, and adding into TiO2With Ce (NO)3)3The ratio of the amounts of substances of (a) to (b) is 60: 1, adding proper amount of Ce (NO)3)3Dispersing for 30min by an ultrasonic oscillator to obtain Ce/TiO2-3 a substrate;
s3, Zinc Zeolite-Ce/TiO2Preparation of antibacterial material
Adding the zinc zeolite complex powder-3 prepared in step S1 to the Ce/TiO prepared in step S22-3 matrix, adding dilute HNO3Regulating the pH value of the reaction solution to 11, stirring in a constant-temperature water bath at 60 ℃ for 0.5h, taking out, filtering in a suction filtration mode by using a Buchner funnel, drying in a forced air drying oven for 2h, roasting at 700 ℃ for 2h by using a muffle furnace, and grinding to obtain the antibacterial material zinc zeolite-Ce/TiO applicable to disinfection products or antibacterial products2-3。
Example 4: a preparation method of a zinc zeolite antibacterial material comprises the following steps:
s1 preparation of Zinc Zeolite Complex powder
Weighing 13.5g of zeolite powder with the particle size of less than 0.12mm, and adding 2mol/L ZnCl250ml of the solution was shaken at 50 ℃ for 2 hours to sufficiently perform ion exchange, and then centrifuged, and washed with distilled water until the washing solution was Zn-free2+Ionizing, and drying the washed zeolite powder at 90 ℃ to obtain zinc zeolite complex powder-4;
S2、Ce/TiO2preparation of the substrate
Weighing 3g of nano TiO2Then in the presence of nano TiO2Adding 100ml deionized water, and adding into TiO2With Ce (NO)3)3The ratio of the amounts of substances (a) to (b) is 70: 1, adding proper amount of Ce (NO)3)3Dispersing for 40min by an ultrasonic oscillator to obtain Ce/TiO2-4 a substrate;
s3, Zinc Zeolite-Ce/TiO2Preparation of antibacterial material
Adding the zinc zeolite complex powder-4 prepared in step S1 to the Ce/TiO prepared in step S22-4 matrix, adding dilute HNO3Regulating the pH value of the reaction solution to control the pH value of the reaction solution to be 9, stirring for 0.5h in a constant-temperature water bath at 70 ℃, taking out, filtering in a suction filtration mode by using a Buchner funnel, drying for 2h in a blast drying oven, roasting for 2h at 800 ℃ by using a muffle furnace, and grinding to obtain the antibacterial material zinc zeolite-Ce/TiO applicable to disinfection products or antibacterial products2-4。
Example 5: a preparation method of a zinc zeolite antibacterial material comprises the following steps:
s1 preparation of Zinc Zeolite Complex powder
Weighing 13g of zeolite powder with the particle size of less than 0.12mm, and adding 2mol/L ZnCl250ml of the solution was shaken at 70 ℃ for 10 hours to sufficiently perform ion exchange, and then centrifuged, and washed with distilled water until the washing solution was Zn-free2+Ionizing, and drying the washed zeolite powder at 95 ℃ to obtain zinc zeolite complex powder-5;
S2、Ce/TiO2preparation of the substrate
Weighing 3g of nano TiO2Then in the presence of nano TiO2Adding 100ml deionized water, and adding into TiO2With Ce (NO)3)3The ratio of the amounts of substances (a) to (b) is 80: 1, adding proper amount of Ce (NO)3)3Dispersing for 50min by an ultrasonic oscillator to obtain Ce/TiO2-5 a substrate;
s3, Zinc Zeolite-Ce/TiO2Preparation of antibacterial material
Adding the zinc zeolite complex powder-5 prepared in step S1 to the Ce/TiO prepared in step S22-5 matrix, adding dilute HNO3Regulating the pH value of the reaction solution to control the pH value of the reaction solution to be 5, stirring for 0.5h in a constant-temperature water bath at 90 ℃, taking out, filtering in a suction filtration mode by using a Buchner funnel, drying for 2h in a blast drying oven, roasting for 2h at 600 ℃ by using a muffle furnace, and grinding to obtain the antibacterial material zinc zeolite-Ce/TiO applicable to disinfection products or antibacterial products2-5。
Referring to FIGS. 6-10, the zinc zeolite-Ce/TiO in terms of colony counts2-1, Zinc Zeolite-Ce/TiO2-2, Zinc Zeolite-Ce/TiO2-3, Zinc Zeolite-Ce/TiO2-4 and zinc zeolite-Ce/TiO2The-5 has better antibacterial effect, in particular to zinc zeolite-Ce/TiO2-1, Zinc Zeolite-Ce/TiO2-2 and zinc zeolite-Ce/TiO2-4。
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that several improvements and modifications without departing from the principle of the present invention will occur to those skilled in the art, and such improvements and modifications should also be construed as within the scope of the present invention.
Claims (9)
1. A preparation method of a zinc zeolite antibacterial material is characterized by comprising the following steps: the method comprises the following steps:
s1 preparation of Zinc Zeolite Complex powder
Weighing 10-13.5g of zeolite powder with the particle size of less than 0.12mm, and adding 1-2mol/L ZnCl2Shaking the solution 50ml at 40-70 deg.C for 2-10h to fully perform ion exchange, centrifuging, washing with distilled water until the washing solution is Zn-free2+Ionizing, and drying the washed zeolite powder at 75-95 ℃ to obtain zinc zeolite complex powder;
S2、Ce/TiO2preparation of the substrate
In the nanometer TiO2Adding deionized water and then according to TiO2With Ce (NO)3)3The ratio of the amounts of substances (A) to (B) is 20-80: 1, adding Ce (NO)3)3Dispersing for 15-50min by an ultrasonic oscillator to obtain Ce/TiO2A substrate;
s3, Zinc Zeolite-Ce/TiO2Preparation of antibacterial material
Adding the zinc zeolite complex powder prepared in step S1 to the Ce/TiO zeolite complex powder prepared in step S22Adding dilute HNO into the matrix3The solution adjusts the pH value of the reaction solution,controlling the pH value of the reaction solution to be 3-11, stirring the reaction solution for 0.5h in a constant-temperature water bath at the temperature of 60-70 ℃, taking out the reaction solution, filtering the reaction solution in a suction filtration mode by using a Buchner funnel, drying the reaction solution for 2h in a blast drying box, roasting the dried reaction solution for 2h at the temperature of 800 ℃ in a muffle furnace, and grinding the dried reaction solution to obtain the zinc zeolite-Ce/TiO2An antibacterial material.
2. The method for preparing the zinc zeolite antibacterial material according to claim 1, characterized in that: the nano TiO2The mass is 3g, and the deionized water is 100 ml.
3. The method for preparing the zinc zeolite antibacterial material according to claim 1, characterized in that: in step S3, the buchner funnel includes a funnel body (1) and a cartridge (2), the funnel body (1) includes an outer cylinder (11) and a tube (12) connected to the bottom of the outer cylinder (11), the cartridge (2) is detachably mounted in the outer cylinder (11), and the cartridge (2) is used for placing the material to be filtered.
4. The method for preparing a zinc zeolite antibacterial material according to claim 3, characterized in that: the cylinder core (2) comprises an inner cylinder (21) and an inner tube (26), the top of the inner cylinder (21) is open, a filter plate (23) is fixed at the bottom of the inner cylinder, the filter plate (23) gradually sinks towards the middle, a water outlet (24) and a central opening (25) are formed in the filter plate (23), the central opening (25) is located in the center of the filter plate (23), and the water outlet (24) is communicated with the central opening (25);
the inner tube (26) is fixed at the bottom of the filter plate (23) and inserted in the tube body (12), and the inner tube (21) is communicated with the inner tube (26) through the water outlet (24) and the central opening (25).
5. The method for preparing the zinc zeolite antibacterial material according to claim 4, characterized in that: the water outlets (24) are arranged in a plurality, the water outlets (24) are uniformly distributed around the central opening (25), and the width of the water outlets (24) is gradually narrowed towards the direction close to the central opening (25).
6. The method for preparing the zinc zeolite antibacterial material according to claim 4, characterized in that: the inner tube (21) top is fixed with journal stirrup (22), journal stirrup (22) set up the relative both sides of inner tube (21), urceolus (11) top both sides seted up with corresponding breach (14) of journal stirrup (22), journal stirrup (22) support in breach (14).
7. The method for preparing the zinc zeolite antibacterial material according to claim 4, characterized in that: and bearing platforms (13) are fixed on the periphery of the inner wall of the outer barrel (11), the bearing platforms (13) are positioned at the lower part of the outer barrel (11), and the filter plates (23) are supported on the bearing platforms (13).
8. The method for preparing a zinc zeolite antibacterial material according to claim 7, characterized in that: the cushion cap (13) is supported on the peripheral edge of the filter plate (23), and the upper surface of the filter plate (23) is arc-shaped and is matched with the bottom surface of the filter plate (23).
9. The application of the zinc zeolite antibacterial material is characterized in that: the zinc zeolite antibacterial material prepared by any one of claims 1 to 8 is applied to disinfection products or antibacterial products.
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