CN114190402A - Preparation method and application of inorganic sterilization material - Google Patents
Preparation method and application of inorganic sterilization material Download PDFInfo
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- CN114190402A CN114190402A CN202111519817.6A CN202111519817A CN114190402A CN 114190402 A CN114190402 A CN 114190402A CN 202111519817 A CN202111519817 A CN 202111519817A CN 114190402 A CN114190402 A CN 114190402A
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- alooh
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- 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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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
Abstract
The invention relates to a preparation method of an inorganic sterilization material, which comprises the steps of firstly preparing a sterilization material containing Zn (OH)2NaCl suspension, adding powder AlOOH into the suspension, and mixing to obtain suspension containing Zn (OH)2The mixed slurry of/AlOOH/NaCl is then dropped into the silver nitrate solution drop by drop, and the AgCl-Zn (OH) is obtained after stirring2Suspension of/AlOOH mixed precipitateWashing the turbid liquid, and drying to obtain powder AgCl-Zn (OH)2AlOOH sterilizing material. The invention also provides application of the sterilizing material in water treatment. The preparation method disclosed by the invention is energy-saving and environment-friendly, and the obtained sterilization material is high in safety, low in metal ion dissolution concentration, remarkable in sterilization effect and wide in application prospect.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to preparation of an inorganic sterilizing material, in particular to a preparation method of a silver-loaded sterilizing material, and also relates to application of the material in a water purification technology.
[ background of the invention ]
A filter element in a household water purifier is very easy to breed bacteria to harm human health, and one solution is to carry out compounding and forming on an antibacterial and bactericidal material and carbon powder or carbon fiber to obtain the filter element with the antibacterial and bactericidal functions.
The inorganic antibacterial materials are mainly classified into heavy metal antibacterial materials and photocatalytic antibacterial materials. The heavy metal antibacterial and bactericidal material is metal and compound of Au, Ag, Hg, Cu, Zn, Ba, Bi, Ta, etc., and various metals have different toxicity to human body and different bactericidal effects. The antibacterial mechanism of the heavy metal antibacterial and bactericidal material is generally considered as follows: in the action process of the antibacterial and bactericidal material, the gradually dissolved metal ions and the mercapto group (-SH) and the amino group (-NH) existing in the protein and the nucleic acid in the organism2) The functional groups containing sulfur and nitrogen react to make some necessary enzymes lose activity, thereby achieving the aim of antibiosis. The photocatalytic bacteriostatic and bactericidal material is mainly n-type semiconductor oxide with wide forbidden band, such as TiO2、ZnO、CdS、WO3、Fe2O3、PnS、SnO2、ZnS、SiO2And the like. The antibacterial principle is as follows: electrons on the valence band of the semiconductor oxide under light irradiation (e)-) Excited to transfer to the conduction band, leaving positively chargedVoid (H)+)，e-And H+Will be adsorbed with O on the surface of the material2OH and water to produce OH-、O2 -And H2O2And the like. In which OH having a very strong oxidizing activity-Can decompose various components forming the microorganism to achieve the aim of sterilization; o is2 -The strong reducibility of the antibacterial agent also plays an antibacterial role.
As a heavy metal bacteriostatic and bactericidal material, the silver-loaded material has good bactericidal and antibacterial effects and is widely applied to the fields of disinfection and water purification. According to the requirements of the water quality index and limit value of the sanitary standard GB5749-2006 for the drinking water, Ag is contained in the drinking water+The limit value of (2) is 0.05mg/L, however, the dissolution of silver ions in the filter element containing the silver-loaded antibacterial material is easy to exceed the standard, and how to control the silver ions of the silver-loaded material to exceed the standard is a key problem faced by the silver-loaded antibacterial material.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art, provides an inorganic bacteriostatic and bactericidal material which reduces the risk of silver ion dissolution, has lower production cost, simultaneously carries two metal ions with bactericidal and bacteriostatic effects, namely silver and zinc, expects the material to have the capability of adsorbing bacteria, can effectively improve the bactericidal efficiency and has a larger application prospect in the aspect of purifying water.
The idea of the invention is to adopt Zn (OH) with small ion product constant2And AgCl is used as an effective component for sterilization and bacteriostasis, and the two active components are loaded on AlOOH according to a certain compounding ratio to obtain AgCl-Zn (OH)2AlOOH antibacterial material. The silver-containing antibacterial agent simultaneously contains two components of silver chloride and zinc hydroxide for synergistic sterilization, so that the effects of reducing the risk of silver ion dissolution, reducing the manufacturing cost and having the capability of adsorbing bacteria are achieved.
Based on the above, the invention provides a preparation method of an inorganic sterilization material, which comprises the following steps:
(1)
respectively preparing 0.5-2mol/L sodium hydroxide solution and 0.5-2mol/L zinc chloride solution, dissolving sodium hydroxideDropwise adding the solution into zinc chloride solution to generate white precipitate, and obtaining the zinc chloride solution containing Zn (OH)2NaCl suspension, wherein the volume ratio of the sodium hydroxide solution to the zinc chloride solution is 2: 1;
(2)
adding powder AlOOH into the suspension, and fully and uniformly mixing to obtain the suspension containing Zn (OH)2AlOOH/NaCl mixed slurry, wherein the molar ratio of AlOOH to zinc chloride is 10: 1;
(3)
preparing silver nitrate solution with the concentration of 0.05-0.2mol/L, and dropwise adding the silver nitrate solution into the solution containing Zn (OH) at room temperature2Stirring the mixed slurry of/AlOOH/NaCl to obtain the product containing AgCl-Zn (OH)2A suspension of the AlOOH mixed precipitate, wherein the volume ratio of the silver nitrate solution to the zinc chloride solution is 1: 1;
(4)
filtering the obtained mixed precipitate, thoroughly washing with deionized water, and drying to obtain powdery AgCl-Zn (OH)2AlOOH sterilizing material.
As a preferred embodiment, in step (1), the sodium hydroxide solution is dropped dropwise into the zinc chloride solution at room temperature.
Preferably, in the step (3), the silver nitrate solution is dropwise added to the Zn (OH) -containing solution at room temperature2AlOOH/NaCl mixed slurry.
The drying in step (4) is carried out at 60-95 ℃.
In the preparation method of the invention, the basic reaction is as follows:
ZnCl2+2NaOH＝＝＝Zn(OH)2↓+2NaCl
NaCl+AgNO3＝＝＝AgCl↓+NaNO3
powdery AgCl-Zn (OH) of the present invention2The working principle of the AlOOH sterilization material is as follows: AlOOH is used as a base material, a large amount of-OH exists on the surface of the AlOOH, and the-OH can adsorb bacterial fungi to a bacteriostatic and bactericidal material AgCl-Zn (OH)2Ag dissolved from the surface of AlOOH and material+With Zn2+Firmly adsorbed to cell membrane by coulomb attraction, and then puncturedThe bacterial proteins are coagulated by the wall entering the cell, and the cell loses its ability to divide and multiply and dies. In addition Ag+With Zn2+Can also destroy microorganism electron transmission system, respiratory system and substance transmission system, and Ag is generated after thallus loses activity+With Zn2+And the metal ions are dissociated from the thalli and repeatedly sterilized, and the redundant metal ions are adsorbed and complexed by-OH on the surface of AlOOH to realize free Zn and complex Zn2+And Ag+The dynamic balance of the process reduces the risk of overproof metal ion dissolution.
According to Zn2+And Ag+Known data of (a):
due to K of silver chloridespIs 1.56X 10-10When the silver chloride is dissolved in water in balance, the concentration of silver ions in the water can reach 1.39mg/L, and the risk of excessive dissolution is high, so that AlOOH is used as a substrate material, AgCl and Zn (OH)2Complexing and attaching on the substrate material, and utilizing-OH functional group richly contained in AlOOH surface to make free Ag+Performing adsorption complexation to realize free Ag and complexed Ag+Ensure the Ag in the solution in the sterilization and bacteriostasis processes+And the standard is not exceeded.
K of zinc hydroxide, on the other handspIs 1.8X 10-14When the zinc hydroxide is dissolved and balanced in water, the concentration of zinc ions in the water is 0.137mg/L and is higher than the minimum inhibitory concentration MIC (0.0065mg/L) of the zinc ions, the requirement that the effective inhibitory requirement is far lower than the water quality index and limit value of the sanitary standard GB5749-2006 for drinking water can be met by 1mg/L, and the requirement for safe inhibitory can be met. Therefore, the silver chloride and the zinc hydroxide are jointly used as the effective components for bacteriostasis and sterilization, so that the risk of over standard dissolution of silver ions can be further reduced, the bacteriostasis and sterilization efficiency is improved, and the cost is reduced.
On the other hand, AlOOH is used as a base material, has the capability of adsorbing bacteria, can adsorb the bacteria in the water body to the surface of the base material, and is favorable for improving the complexation and the adhesion of AgCl andZn(OH)2AgCl-Zn (OH)2The antibacterial and bactericidal effects of AlOOH.
Based on the above, the invention provides the application of the inorganic sterilization material prepared by the preparation method in the preparation of filter elements, in particular to the application of the inorganic sterilization material as a bacteriostatic and bactericidal material in the filter elements.
Further, the invention also provides application of the inorganic sterilization material prepared by the preparation method in tap water sterilization.
Wherein the dosage of the non-polar sterilizing material in tap water is 0.5-25 g/L. Within the dosage range, the bactericidal effect is obvious, and Zn2+And Ag+The elution amount of the ions meets the requirements of the water quality index and the limit value of the sanitary standard GB5749-2006 for drinking water.
Compared with the prior art, the preparation method provided by the invention has the advantages of energy conservation and environmental protection without high-temperature and high-pressure conditions, and is pollution-free and environment-friendly. The sodium chloride formed after the zinc chloride reacts with the sodium hydroxide can react with the silver nitrate to form silver chloride precipitate, and reaction raw materials can be fully utilized.
According to the invention, silver chloride and zinc hydroxide are used as the effective components for bacteriostasis and sterilization, so that the risk of over standard dissolution of silver ions is effectively reduced, the bacteriostasis and sterilization efficiency is improved, and the cost is reduced.
In addition, AlOOH is used as a base material, and the surface of the AlOOH is rich in-OH functional groups, so that free Zn can be added2+And Ag+Adsorption complexation is carried out, thus obtaining the composite material AgCl-Zn (OH)2AlOOH, realizing Zn in free state and complex state2+And Ag+Ensure the Zn in the solution in the sterilization and bacteriostasis processes2+And Ag+And the standard is not exceeded. The AlOOH has the capability of adsorbing bacteria, can adsorb the bacteria in the water body to the surface of the AlOOH, and is favorable for improving the AgCl-Zn (OH)2The antibacterial and bactericidal effects of AlOOH.
[ description of the drawings ]
FIG. 1 shows AgCl-Zn (OH)2A working schematic diagram of the AlOOH antibacterial material;
FIG. 2 shows AgCl-Zn (OH)2AlOOH antibacterial material sampleSEM electron micrograph.
FIG. 3 shows AgCl-Zn (OH)2XRD standard card comparison of the/AlOOH antibacterial and bactericidal material.
[ detailed description ] embodiments
Example 1
100mL of 2mol/L sodium hydroxide solution was added dropwise to 50mL of 2mol/L zinc chloride solution to form a white precipitate, and a mixed slurry Zn (OH) was obtained2NaCl. 60g of powder AlOOH was added to the resulting mixed slurry Zn (OH))2In NaCl, mechanically stirring for 1h, and fully and uniformly mixing to obtain mixed slurry Zn (OH)2AlOOH/NaCl. Then 50mL of silver nitrate solution with a concentration of 0.2mol/L was added dropwise to the above mixed slurry Zn (OH)2In AlOOH/NaCl, stirring continuously to obtain a final product AgCl-Zn (OH)2AlOOH mixed precipitation, precipitation filtration, washing with deionized water for 3-5 times, drying at 60 deg.C to obtain AgCl-Zn (OH)2AlOOH antibacterial material.
Example 2
200mL of 1mol/L sodium hydroxide solution was added dropwise to 100mL of 1mol/L zinc chloride solution to form a white precipitate, and a mixed slurry Zn (OH) was obtained2NaCl. 60g of powder AlOOH was added to the resulting mixed slurry Zn (OH))2In NaCl, mechanically stirring for 1h, and fully and uniformly mixing to obtain mixed slurry Zn (OH)2AlOOH/NaCl. Then 50mL of silver nitrate solution with a concentration of 0.2mol/L was added dropwise to the above mixed slurry Zn (OH)2In AlOOH/NaCl, stirring continuously to obtain a final product AgCl-Zn (OH)2AlOOH mixed precipitation, precipitation filtration, washing with deionized water for 3-5 times, drying at 60 deg.C to obtain AgCl-Zn (OH)2AlOOH antibacterial material.
SEM micrograph of the obtained Material As shown in FIG. 2, it can be observed that many fine particles are attached to the AlOOH surface, indicating that Zn (OH)2And AgCl are attached to porous AlOOH particles with a large specific surface area.
The obtained material was examined with a Nippon-based Ultima IV X-ray diffractometer (rated output: 3KW) with a scanning angle range ofThe comparison graph of the XRD standard card obtained under the conditions of 5-90 DEG and 5 DEG/min of scanning speed is shown in figure 3, and the obtained material is AgCl-Zn (OH)2/AlOOH。
As can be seen from FIGS. 2 and 3, the composite material of the present invention is obtained by complexing and adhering AgCl and Zn (OH) to a material based on AlOOH2The AgCl-Zn (OH) obtained2A/AlOOH composite material.
Example 3 Sterilization Performance verification
Prepared at a concentration of 106cfu/ml of activated Escherichia coli in tap water, the AgCl-Zn (OH) of example 1 was weighed20.05g, 0.25g, 0.5g, 1g and 2.5g of AlOOH sterilizing material are respectively added into 100g of activated escherichia coli bacterial liquid, and the bacterial liquid without the sterilizing material is used as a control.
The bacterial liquid is stirred for 4 hours on a stirrer, 5mL of each sample is sampled after 4 hours, the number of the residual viable bacteria is tested by a common culture method, and the sterilization performance of each sterilization material is calculated.
An additional 15mL sample was taken from each sample, allowed to stand for 4, 24, 48, and 96 hours, filtered, and the ion concentration of the solution was measured by an emission spectrometer (ICP) at each time point. The results are shown in Table 1.
TABLE 1 Performance of antibacterial and bactericidal materials with different dosages and same bacterial liquid concentrations
The experimental results are shown in table 1, the five groups of parallel samples have excellent sterilization effects, the sterilization rates are all 100%, and the sterilization material still has good sterilization effects under the condition that the addition concentration of the sterilization material is as low as 0.05g/100g of escherichia coli bacterial liquid. In the aspect of metal ion dissolution, Zn is subjected to the requirements of water quality indexes and limit values of sanitary standard GB5749-2006 of drinking water2+Has a limiting value of 1mg/L for Ag+Has a limit value of 0.05mg/L, and the sample material Zn is within 96 hours2+And Ag+The dissolution amount is within the range of national sanitary standard, the performance is excellent, and the safety is good.
Further, the concentrations were set to 10 respectively4cfu/ml，105cfu/ml，106cfu/ml，107cfu/ml，108100g of a bacterial suspension of Escherichia coli (cfu/ml) in tap water, to which AgCl-Zn (OH) of example 1 was added20.05g of AlOOH antibacterial and bactericidal material, and taking bacterial liquid without the bactericidal material as a control, and stirring for 4h respectively.
5mL of the sample is respectively taken, and the number of the viable bacteria is detected by the same method to calculate the sterilization performance of the sterilization material on bacteria liquid with various concentrations.
15mL of each sample was taken out, and the resulting solution was left standing for 4, 24, 48 and 96 hours, and then filtered to measure the ion elution concentration by the same method.
TABLE 2 Performance of antibacterial and bactericidal materials with the same dosage and different bacteria liquid concentrations
As shown in Table 2, the bactericidal material added in the amount as low as 0.05g/100g of bacterial suspension exhibited good bactericidal effect against bacterial suspension of each concentration, and the bactericidal rate was 100%. Furthermore, Zn2+And Ag+All the materials are qualified within 96h of dissolution and are within the range of national sanitary standards. Two groups of experimental results show that the antibacterial and bactericidal material has an obvious bactericidal effect, can complete a bactericidal task within 4 hours, has high safety and wide application prospect, and the elution amount of metal ions is far lower than the national standard limit value.
Claims (7)
1. A method for preparing an inorganic sterilizing material, comprising the steps of:
(1)
respectively preparing 0.5-2mol/L sodium hydroxide solution and 0.5-2mol/L zinc chloride solution, dropwise adding the sodium hydroxide solution into the zinc chloride solution to generate white precipitate, and obtaining the zinc chloride solution containing Zn (OH)2NaCl suspension, wherein the volume ratio of the sodium hydroxide solution to the zinc chloride solution is 2: 1;
(2)
adding powder into the suspensionAlOOH, and fully and uniformly mixing to obtain the product containing Zn (OH)2AlOOH/NaCl mixed slurry, wherein the molar ratio of AlOOH to zinc chloride is 10: 1;
(3)
preparing silver nitrate solution with concentration of 0.05-0.2mol/L, and dropwise adding the silver nitrate solution into the solution containing Zn (OH) at room temperature2Stirring the mixed slurry of/AlOOH/NaCl to obtain the product containing AgCl-Zn (OH)2A suspension of the AlOOH mixed precipitate, wherein the volume ratio of the silver nitrate solution to the zinc chloride solution is 1: 1;
(4)
filtering the obtained mixed precipitate, thoroughly washing with deionized water, and drying to obtain powdery AgCl-Zn (OH)2AlOOH sterilizing material.
2. The production method according to claim 1, characterized in that in the step (1), the sodium hydroxide solution is dropped dropwise into the zinc chloride solution at room temperature.
3. The production method according to claim 1, wherein in the step (3), the silver nitrate solution is dropped dropwise into the solution containing Zn (OH) at room temperature2AlOOH/NaCl mixed slurry.
4. The method according to claim 1, wherein the drying in the step (4) is carried out at 60 to 95 ℃.
5. The use of the inorganic sterilization material prepared by the preparation method according to any one of claims 1 to 4 in the preparation of filter elements.
6. Use of the inorganic bactericidal material prepared by the preparation method according to any one of claims 1 to 4 for the sterilization of tap water.
7. The use according to claim 6, characterized in that the amount of the non-polar sterilizing material in tap water is 0.5-25 g/L.
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