CN113498786B - Preparation process of inorganic-organic compound complex antibacterial agent - Google Patents
Preparation process of inorganic-organic compound complex antibacterial agent Download PDFInfo
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- CN113498786B CN113498786B CN202110728910.1A CN202110728910A CN113498786B CN 113498786 B CN113498786 B CN 113498786B CN 202110728910 A CN202110728910 A CN 202110728910A CN 113498786 B CN113498786 B CN 113498786B
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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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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- 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
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Abstract
The invention discloses a preparation process of an inorganic-organic compound complex antibacterial agent, which relates to the technical field of inorganic-organic compound antibacterial agents, solves the problems of poor discoloration resistance, poor antibacterial durability and poor salt resistance of the conventional silver ion antibacterial agent through the preparation of a complex, successfully realizes the application of the prepared antibacterial agent in light-colored products, alkaline environments and products or environments containing chloride ions, expands the application range of the antibacterial agent and ensures the application effect of the antibacterial agent.
Description
The technical field is as follows:
the invention relates to the technical field of inorganic-organic composite antibacterial agents, in particular to a preparation process of an inorganic-organic composite complex antibacterial agent.
Background art:
the antibacterial agent is a medicament capable of killing or inhibiting harmful microorganisms such as bacteria, viruses and the like, and mainly comprises an organic antibacterial agent and an inorganic antibacterial agent. Compared with organic antibacterial agents, the inorganic antibacterial agent has the characteristics of good safety, high thermal decomposition temperature, good stability, strong antibacterial property, lasting antibacterial property and the like. The inorganic antibacterial agent is generally composed of an antibacterial component and a carrier, and a metal or metal ion having antibacterial ability is immobilized on the carrier by physical adsorption or ion exchange. The metal ions having antibacterial activity include metal ions such as silver, zinc, iron, aluminum, chromium, nickel, and cobalt, but silver ions are preferred from the viewpoint of antibacterial activity and safety, and therefore, silver ion antibacterial agents are widely used as inorganic antibacterial agents.
Currently, silver ion antibacterial agents are usually prepared by loading silver ions on carriers such as zeolite, activated carbon, phosphate, silicate and the like by adsorption or ion exchange principles. However, such silver ion antibacterial agents have the following drawbacks: (1) the silver carrying amount is low, so that the high-efficiency performance of antibacterial performance is influenced; (2) the tarnish resistance is poor, silver ions are easily reduced into silver simple substances to become black, and the application of the silver simple substances in light-colored products is influenced; (3) the antibacterial durability is poor, and silver ions are easy to generate silver oxide precipitates in an alkaline environment; (4) the silver ion has poor salt resistance, and when the silver ion encounters a product containing chloride ions or an environment, silver chloride precipitates are easily generated and lose activity.
The invention content is as follows:
the invention aims to provide a preparation process of an inorganic-organic compound complex antibacterial agent, which improves the antibacterial performance of the prepared antibacterial agent by preparing a silver ion complex and carrying silver on montmorillonite and well solves the application defects of the conventional silver ion antibacterial agent.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation process of an inorganic-organic compound complex antibacterial agent comprises the following process steps:
(1) dissolving soluble silver salt in deionized water to obtain a solution I;
(2) dissolving 3-cyanopyridone in deionized water to obtain a solution II;
(3) heating and stirring the solution I, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction in a reflux state to obtain a solution III;
(4) dispersing montmorillonite in the solution III, placing the obtained mixture in a reaction kettle for hydrothermal reaction, cooling, performing solid-liquid separation, and vacuum drying the obtained solid to obtain the complex antibacterial agent.
The soluble silver salt is one of silver nitrate and silver acetate.
The molar ratio of the soluble silver salt to the 3-cyanopyridone is 1: 1.
The dosage of the montmorillonite is 3-10 times of the total mass of the soluble silver salt and the 3-cyanopyridone.
The purity of the montmorillonite is more than or equal to 99%.
The reaction temperature of the hydrothermal reaction is 120-180 ℃, the reaction pressure is 3-12MPa, and the reaction time is 2-8 h.
The temperature of the vacuum drying is 60-90 ℃.
The soluble silver salt is dissolved at normal temperature or heated.
The dissolving condition of the 3-cyanopyridone is normal temperature dissolving or heating dissolving.
The heating and stirring temperature of the solution I is 50-70 ℃.
The 3-cyanopyridone provides lone pair electrons, the silver ions provide empty tracks, and the 3-cyanopyridone reacts with soluble silver salt to form a silver ion complex which has good stability and can well solve the problems that the silver ions are easy to discolor and generate silver oxide and silver chloride precipitates.
The inorganic-organic composite antibacterial agent loaded with the silver ion complex is prepared by utilizing the adsorption effect of the montmorillonite, the advantages of the montmorillonite silver-loaded antibacterial agent and the silver ion complex antibacterial agent are efficiently integrated, and the antibacterial effect is greatly enhanced.
The time required by the montmorillonite for carrying silver is shortened through hydrothermal reaction, the silver carrying amount is improved, the prepared complex antibacterial agent is small in particle size and uniform in distribution, the uniform dispersion of the antibacterial agent in processing raw materials of products can be promoted, and the problems of reduction of mechanical properties and poor antibacterial performance of the products caused by agglomeration are solved.
In order to improve the adsorbability of the montmorillonite and further increase the silver loading, the inventor also carries out the following pretreatment on the montmorillonite before silver loading:
adding water into glycerol to dilute the glycerol into a solution, then adding montmorillonite, carrying out ultrasonic treatment, filtering, drying filter residues in an oven with the temperature of 100-.
The mass ratio of the glycerol to the water to the montmorillonite is 1 (1-5) to 0.2-2.
The frequency of the ultrasonic treatment is 20-40kHz, and the power is 100-1000W.
The method comprises the steps of adopting glycerol as a pretreating agent, enabling the diluted glycerol to enter internal pore channels of the montmorillonite through a permeation effect, filling all micropores of the montmorillonite under the action of ultrasonic waves, expanding the micropores, removing the glycerol through high-temperature roasting, and leaving cavities in the interior and on the surface of the montmorillonite, so that the pore diameter and the pore volume are increased, and the adsorption effect is improved.
The invention has the beneficial effects that:
(1) the invention solves the problems of poor discoloration resistance, poor antibacterial durability and poor salt resistance of the conventional silver ion antibacterial agent through the preparation of the complex, successfully realizes the application of the prepared antibacterial agent in light-colored products, alkaline environments and products or environments containing chloride ions, expands the application range of the antibacterial agent and ensures the application effect of the antibacterial agent.
(2) The invention takes the montmorillonite as a carrier, improves the heat resistance and the ultraviolet resistance of the antibacterial agent by loading the silver ion complex, has high silver loading amount and ensures the high-efficiency play of the antibacterial action of the antibacterial agent.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
(1) Dissolving 0.2mol of silver nitrate in deionized water at normal temperature to obtain a solution I.
(2) Heating and dissolving 0.2mol of 3-cyanopyridone in deionized water to obtain a solution II.
(3) Heating the solution I to 50 ℃, stirring, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction for 5 hours in a reflux state to obtain a solution III.
(4) Dispersing montmorillonite in the solution III, wherein the using amount of the montmorillonite is 3 times of the total mass of silver nitrate and 3-cyanopyridone, placing the obtained mixture in a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃, the reaction pressure of 5MPa and the reaction time of 6h, cooling, performing solid-liquid separation, and drying the obtained solid in vacuum at the temperature of 70 ℃ to obtain the complex antibacterial agent.
Example 2
(1) Dissolving 0.2mol of silver nitrate in deionized water at normal temperature to obtain a solution I.
(2) Heating and dissolving 0.2mol of 3-cyanopyridone in deionized water to obtain a solution II.
(3) Heating the solution I to 60 ℃, stirring, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction for 5 hours in a reflux state to obtain a solution III.
(4) Dispersing montmorillonite in the solution III, wherein the using amount of the montmorillonite is 5 times of the total mass of silver nitrate and 3-cyanopyridone, placing the obtained mixture in a reaction kettle for hydrothermal reaction at the reaction temperature of 130 ℃, the reaction pressure of 8MPa and the reaction time of 8h, cooling, performing solid-liquid separation, and drying the obtained solid in vacuum at the temperature of 75 ℃ to obtain the complex antibacterial agent.
Example 3
(1) Heating and dissolving 0.2mol of silver acetate in deionized water to obtain a solution I.
(2) Heating and dissolving 0.2mol of 3-cyanopyridone in deionized water to obtain a solution II.
(3) Heating the solution I to 60 ℃, stirring, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction for 4 hours in a reflux state to obtain a solution III.
(4) Dispersing montmorillonite in the solution III, wherein the using amount of the montmorillonite is 5 times of the total mass of the silver acetate and the 3-cyanopyridone, placing the obtained mixture in a reaction kettle for hydrothermal reaction at the reaction temperature of 180 ℃, the reaction pressure of 4MPa and the reaction time of 5h, cooling, performing solid-liquid separation, and drying the obtained solid in vacuum at the temperature of 70 ℃ to obtain the complex antibacterial agent.
Example 4
(1) Heating and dissolving 0.2mol of silver acetate in deionized water to obtain a solution I.
(2) Heating and dissolving 0.2mol of 3-cyanopyridone in deionized water to obtain a solution II.
(3) Heating the solution I to 70 ℃, stirring, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction for 5 hours under a reflux state to obtain a solution III.
(4) Dispersing montmorillonite in the solution III, wherein the using amount of the montmorillonite is 6 times of the total mass of the silver acetate and the 3-cyanopyridone, placing the obtained mixture in a reaction kettle for hydrothermal reaction, wherein the reaction temperature is 150 ℃, the reaction pressure is 5MPa, and the reaction time is 6h, cooling, performing solid-liquid separation, and performing vacuum drying on the obtained solid at 80 ℃ to obtain the complex antibacterial agent.
Example 5 and example 6 are the same as example 4 except that pretreatment of montmorillonite is added to example 4.
Example 5
(1) Diluting 100g of glycerol with 200g of water to obtain a solution, adding 50g of montmorillonite, performing ultrasonic treatment for 1h at the frequency of 28kHz and the power of 1000W, filtering, drying filter residues in a 120 ℃ oven for 5h to remove water, roasting in a 350 ℃ tube furnace for 3h to remove glycerol, and crushing the obtained solid into powder to obtain the pretreated montmorillonite.
(2) Heating and dissolving 0.2mol of silver acetate in deionized water to obtain a solution I.
(3) Heating and dissolving 0.2mol of 3-cyanopyridone in deionized water to obtain a solution II.
(4) Heating the solution I to 70 ℃, stirring, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction for 5 hours under a reflux state to obtain a solution III.
(5) Dispersing the pretreated montmorillonite in the solution III, wherein the consumption of the montmorillonite is 6 times of the total mass of the silver acetate and the 3-cyanopyridone, placing the obtained mixture in a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃, the reaction pressure of 5MPa and the reaction time of 6h, cooling, performing solid-liquid separation, and performing vacuum drying on the obtained solid at the temperature of 80 ℃ to obtain the complex antibacterial agent.
Example 6
(1) Diluting 100g of glycerol with 100g of water to obtain a solution, adding 50g of montmorillonite, performing ultrasonic treatment for 2h at the frequency of 28kHz and the power of 500W, filtering, drying filter residues in a 100 ℃ oven for 8h to remove water, roasting in a 400 ℃ tube furnace for 2h to remove glycerol, and crushing the obtained solid into powder to obtain the pretreated montmorillonite.
(2) Heating and dissolving 0.2mol of silver acetate in deionized water to obtain a solution I.
(3) Heating and dissolving 0.2mol of 3-cyanopyridone in deionized water to obtain a solution II.
(4) Heating the solution I to 70 ℃, stirring, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction for 5 hours under a reflux state to obtain a solution III.
(5) Dispersing the pretreated montmorillonite in the solution III, wherein the consumption of the montmorillonite is 6 times of the total mass of the silver acetate and the 3-cyanopyridone, placing the obtained mixture in a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃, the reaction pressure of 5MPa and the reaction time of 6h, cooling, performing solid-liquid separation, and performing vacuum drying on the obtained solid at the temperature of 80 ℃ to obtain the complex antibacterial agent.
Comparative examples 1 and 2 are comparative examples in which 3-cyanopyridone or montmorillonite, respectively, was not used in the preparation of the antibacterial agent, and the remainder is the same as in example 1.
Comparative example 1
(1) Dissolving 0.2mol of silver nitrate in deionized water at normal temperature to obtain a solution I.
(2) Dispersing montmorillonite in the solution I, wherein the using amount of the montmorillonite is 3 times of the mass of silver nitrate, placing the obtained mixture in a reaction kettle for hydrothermal reaction, the reaction temperature is 150 ℃, the reaction pressure is 5MPa, the reaction time is 6h, cooling, carrying out solid-liquid separation, and carrying out vacuum drying on the obtained solid at 70 ℃ to obtain the antibacterial agent.
Comparative example 2
(1) Dissolving 0.2mol of silver nitrate in deionized water at normal temperature to obtain a solution I.
(2) Heating and dissolving 0.2mol of 3-cyanopyridone in deionized water to obtain a solution II.
(3) Heating the solution I to 50 ℃, stirring, then dropwise adding the solution II, continuing heating after dropwise adding is finished, carrying out heat preservation reaction for 5 hours in a reflux state to obtain a solution III, cooling, and freeze-drying to obtain the antibacterial agent.
The antibacterial agents prepared in the embodiments 1-6 and the comparative examples 1-2 are respectively mixed with polyacrylonitrile and then dissolved in DMF to obtain spinning solution, the dosage of the antibacterial agent is 0.5 percent of the weight of the polyacrylonitrile, the spinning solution is subjected to electrostatic spinning to obtain polyacrylonitrile fibers, and the polyacrylonitrile fibers are woven to prepare polyacrylonitrile fabrics.
According to the standard GB/T20944.2-2007 evaluation part 2 of antibacterial properties of textiles: the absorption method is used for measuring the antibacterial performance, and the silver-carrying amount of the antibacterial agent is measured by adopting a dithizone extraction spectrophotometry, the set wavelength is 462nm, and the measurement result is shown in table 1.
TABLE 1 antimicrobial Rate and silver Loading of the antimicrobial agent of the present invention
| Escherichia coli | Staphylococcus aureus | Candida albicans | Silver loading capacity | |
| Example 1 | ≥99.5％ | ≥99.5％ | ≥99.5％ | 20.2％ |
| Example 2 | ≥99.5％ | ≥99.5％ | ≥99.5％ | 20.6％ |
| Example 3 | ≥99.5％ | ≥99.5％ | ≥99.5％ | 20.9％ |
| Example 4 | ≥99.5％ | ≥99.5％ | ≥99.5％ | 21.4％ |
| Example 5 | ≥99.5％ | ≥99.5％ | ≥99.5％ | 25.2％ |
| Example 6 | ≥99.5％ | ≥99.5％ | ≥99.5％ | 25.7％ |
| Comparative example 1 | 98-99％ | 98-99％ | 98-99％ | 18.1％ |
| Comparative example 2 | 98-99％ | 98-99％ | 98-99％ | / |
As can be seen from the data in Table 1, the complex antibacterial agent prepared by the invention has good antibacterial performance, and under the condition that the addition amount is 0.5%, the antibacterial rate of the complex antibacterial agent on escherichia coli, staphylococcus aureus and candida albicans can reach more than 99.5%, and the silver loading is high.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation process of an inorganic-organic compound complex antibacterial agent is characterized by comprising the following process steps:
(1) dissolving soluble silver salt in deionized water to obtain a solution I;
(2) dissolving 3-cyanopyridone in deionized water to obtain a solution II;
(3) heating and stirring the solution I, then dropwise adding the solution II, continuing heating after dropwise adding is finished, and carrying out heat preservation reaction in a reflux state to obtain a solution III;
(4) dispersing montmorillonite into the solution III, placing the obtained mixture into a reaction kettle for hydrothermal reaction, cooling, performing solid-liquid separation, and performing vacuum drying on the obtained solid to obtain a complex antibacterial agent;
the soluble silver salt is one of silver nitrate and silver acetate;
the molar ratio of the soluble silver salt to the 3-cyanopyridone is 1: 1;
the dosage of the montmorillonite is 3-10 times of the total mass of the soluble silver salt and the 3-cyanopyridone;
the reaction temperature of the hydrothermal reaction is 120-180 ℃, the reaction pressure is 3-12MPa, and the reaction time is 2-8 h.
2. The process for producing an inorganic-organic complex antibacterial agent according to claim 1, characterized in that: the purity of the montmorillonite is more than or equal to 99%.
3. The process for producing an inorganic-organic complex antibacterial agent according to claim 1, characterized in that: the temperature of the vacuum drying is 60-90 ℃.
4. The process for producing an inorganic-organic complex antibacterial agent according to claim 1, characterized in that: the soluble silver salt is dissolved at normal temperature or heated.
5. The process for producing an inorganic-organic complex antibacterial agent according to claim 1, characterized in that: the dissolving condition of the 3-cyanopyridone is normal temperature dissolving or heating dissolving.
6. The process for producing an inorganic-organic complex antibacterial agent according to claim 1, characterized in that: the heating and stirring temperature of the solution I is 50-70 ℃.
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| CN102599164A (en) * | 2012-01-19 | 2012-07-25 | 西安文理学院 | Preparation method of nano-grade layered silver-carrying-amino acid complex antibacterial agent |
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| CN102599164A (en) * | 2012-01-19 | 2012-07-25 | 西安文理学院 | Preparation method of nano-grade layered silver-carrying-amino acid complex antibacterial agent |
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