CN114885957A - Composite antibacterial material - Google Patents

Composite antibacterial material Download PDF

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Publication number
CN114885957A
CN114885957A CN202210596420.5A CN202210596420A CN114885957A CN 114885957 A CN114885957 A CN 114885957A CN 202210596420 A CN202210596420 A CN 202210596420A CN 114885957 A CN114885957 A CN 114885957A
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salt
antibacterial agent
inorganic high
molybdenum
efficiency antibacterial
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刘飞
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Jinan Zhangqiu Hanxi Biotechnology Center
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Jinan Zhangqiu Hanxi Biotechnology Center
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/02Sulfur; Selenium; Tellurium; Compounds thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against 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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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Inorganic Chemistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to an inorganic high-efficiency antibacterial agent, which is characterized in that the preparation method comprises the following steps: adding Zn salt, Mo salt, Zr salt, thiourea and sodium dodecyl benzene sulfonate into water/glycol, and quickly stirring and uniformly mixing; the mol ratio of the Zn salt, the Mo salt, the Zr source and the thiourea is 1: 1: (0.03-0.1): 3; the material ratio of Zn salt to sodium dodecyl benzene sulfonate is (10-20) mmol: (10-20) mg; adding the mixed solution into a high-pressure reaction kettle, and reacting; centrifuging and washing the product to obtain popcorn-shaped Zr doped-MoS 2 Composite material of/ZnS, simultaneous Zr incorporation into MoS 2 And in the crystal lattice of ZnS, the crystallinity is improved, and the sterilization rate of the composite material is improved; the popcorn-shaped structure exposes a large amount of photocatalytic sites, further improves the sterilization rate and has stronger killing effect on staphylococcus aureus and escherichia coli.

Description

Composite antibacterial material
Technical Field
The invention relates to a preparation method of a high-efficiency antibacterial agent, and particularly relates to Zr-doped MoS 2 A preparation method of a/ZnS composite antibacterial agent.
Background
With the continuous development of society, people have higher and higher requirements on life quality, and pay more attention to the relationship among microorganisms, environment and self health. Therefore, antibacterial materials have once been the focus of research. The inorganic antibacterial material has received more and more attention due to low price, high safety performance, no toxicity and high-efficiency continuous sterilization, and is widely applied to the fields of building materials, medical treatment, disposable hygienic products, textiles, shoe materials, environmental protection and cosmetics.
CN112931531A discloses a carbon-doped nickel phosphide composite antibacterial material and a preparation method and application thereof, wherein the method comprises the following steps: (1) adding carbon nanospheres, nickel nitrate hexahydrate, urea and water into a beaker, and uniformly stirring to obtain a mixed solution; (2) adding the mixed solution into a reaction kettle, and placing the reaction kettle in a drying oven for hydrothermal reaction; (3) centrifuging, washing and drying the mixed solution obtained by the hydrothermal reaction to obtain solid powder; (4) and (3) calcining the solid powder and sodium hypophosphite in a tubular furnace in a nitrogen atmosphere to obtain the carbon-doped nickel phosphide composite antibacterial material.
CN111838148A discloses a preparation method of a cobalt-doped zinc oxide/molybdenum disulfide nano composite antibacterial agent, which utilizes the advantages of large specific surface area, strong surface adsorption capacity and the like of a molybdenum disulfide nano sheet to adsorb bacteria to the surface of the molybdenum disulfide nano sheet, and then the bacteria cooperate with cobalt (Co) -doped zinc oxide (ZnO) loaded on the surface and between layers of the molybdenum disulfide nano sheet to play a role in high-efficiency antibacterial action; CN113040169A discloses carbon doped MoS 2 A/CoP/C composite antibacterial material and a preparation method and application thereof belong to the technical field of material preparation and antibacterial materials. The method comprises the following steps: (1) uniformly stirring nano carbon spheres, cobalt nitrate hexahydrate, urea and water to obtain a mixed solution, placing the mixed solution into a reaction kettle, and then placing the reaction kettle into an oven to perform hydrothermal reaction; (2) centrifuging, washing and drying the mixed solution obtained by the hydrothermal reaction to obtain solid powder; (3) calcining the solid powder and sodium hypophosphite in a tubular furnace in a nitrogen atmosphere to obtain carbon-doped CoP/C; (4) adding CoP/C, thioacetamide and sodium molybdate into a beaker, uniformly stirring to obtain a mixed solution, placing the mixed solution into a reaction kettle, and then placing the reaction kettle into a drying oven for hydrothermal reaction; (5) centrifuging and washing the mixed solution obtained by the hydrothermal reaction, and drying to obtain the carbon-doped MoS 2 the/CoP/C composite antibacterial material.
Disclosure of Invention
The invention aims to provide a high-efficiency antibacterial agent which is simple in preparation process and low in price.
An inorganic high-efficiency antibacterial agent is characterized by comprising the following steps:
step (1): adding Zn salt, Mo salt, Zr source, thiourea, sodium dodecyl benzene sulfonate and Cu source into water/ethylene glycol, and rapidly stirring and uniformly mixing; the mol ratio of Zn salt, Mo salt, Zr salt and thiourea is 1: 1: (0.03-0.1): 3; the material ratio of Zn salt to sodium dodecyl benzene sulfonate is (10-20) mmol: (10-20) mg;
step (2): adding the mixed solution into a high-pressure reaction kettle, and reacting;
and (3): centrifuging and washing the product to obtain popcorn-shaped Zr doped-MoS 2 The particle size of the/ZnS composite material is 5-8 microns.
Preferably, the Zn salt is zinc nitrate, zinc sulfate, zinc chloride and zinc acetate;
preferably, the Mo salt is molybdenum nitrate, molybdenum sulfate, molybdenum chloride and molybdenum acetate;
preferably, the reaction temperature is 180-220 ℃; the reaction time is 12-20 h;
preferably, deionized water and ethanol are alternately washed for 2 to 4 times;
preferably, the volume ratio of water to glycol is 1: (0.5-1);
the popcorn-shaped Zr-doped MoS is prepared by adopting a water-solvothermal method in one step 2 The preparation process of the/ZnS is simple and low in cost, and Zr is synchronously doped into MoS 2 And in the crystal lattice of ZnS, the crystallinity is improved, and the sterilization rate of the composite material is improved; the popcorn-shaped structure exposes a large amount of photocatalytic sites, further improves the sterilization rate and has stronger killing effect on staphylococcus aureus and escherichia coli.
Drawings
Fig. 1 is an SEM image of the composite material of the present application.
Detailed Description
Example 1
Step (1): adding 10mmo of zinc nitrate, 10mmol of molybdenum nitrate, 1mmol of zirconium nitrate, 30mmol of thiourea and 18mg of sodium dodecyl benzene sulfonate into 80ml of the mixture with the volume ratio of 1: 1, rapidly stirring and uniformly mixing the mixture in water/glycol;
step (2): adding the mixed solution into a high-pressure reaction kettle, and reacting at the temperature of 180 ℃ for 15 h;
and (3): centrifuging and washing the product to obtain popcorn-shaped Zr doped-MoS 2 a/ZnS composite material.
Example 2
Step (1): adding 10mmo of zinc nitrate, 10mmol of molybdenum nitrate, 30mmol of thiourea, 1mmol of zirconium nitrate and 16mg of sodium dodecyl benzene sulfonate into 80ml of the mixture with the volume ratio of 1: 0.5 of water/glycol, quickly stirring and uniformly mixing;
step (2): adding the mixed solution into a high-pressure reaction kettle, and reacting at 190 ℃ for 18 h;
and (3): centrifuging and washing the product to obtain popcorn-shaped Zr doped-MoS 2 a/ZnS composite material.
Comparative example 1
Step (1): adding 10mmo of zinc nitrate, 10mmol of molybdenum nitrate, 30mmol of thiourea and 16mg of sodium dodecyl benzene sulfonate into 80ml of the mixture with the volume ratio of 1: 0.5 of water/glycol, quickly stirring and uniformly mixing;
step (2): adding the mixed solution into a high-pressure reaction kettle, and carrying out water-solvent thermal reaction at the temperature of 190 ℃ for 18 h;
and (3): centrifuging and washing the product to obtain MoS 2 a/ZnS composite material.
Comparative example 2
Step (1): adding 10mmo of zinc nitrate, 1mmol of zirconium nitrate, 10mmol of thiourea and 16mg of sodium dodecyl benzene sulfonate into 80ml of the mixture with the volume ratio of 1: 0.5 of water/glycol, quickly stirring and uniformly mixing;
step (2): adding the mixed solution into a high-pressure reaction kettle, and reacting at 190 ℃ for 18 h;
and (3): and centrifuging and washing the product to obtain the Zr-doped ZnS composite material.
Comparative example 3
Step (1): adding 10mmol of molybdenum nitrate, 1mmol of zirconium nitrate, 20mmol of thiourea and 16mg of sodium dodecyl benzene sulfonate into 80ml of solution with the volume ratio of 1: 0.5 of water/glycol, quickly stirring and uniformly mixing;
step (2): adding the mixed solution into a high-pressure reaction kettle, and reacting at 190 ℃ for 18 h;
and (3): centrifuging and washing the product to obtain popcorn-shaped Zr doped-MoS 2 A composite material.
The antibacterial performance of the materials of examples 1-2 and comparative examples 1-3 was tested according to GB/T21510-2008 method for testing antibacterial performance of inorganic nano-materials, and the results are shown in the following table:
staphylococcus aureus (Sterilization rate) Escherichia coli (Sterilization rate)
Example 1 99.6% 99.7%
Example 2 99.6% 99.6%
Comparative example 1 83.2% 84.1%
Comparative example 2 81.5% 89.0%
Comparative example 3 83.9% 88.5%
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (6)

1. An inorganic high-efficiency antibacterial material is characterized in that the preparation method comprises the following steps:
step (1): adding Zn salt, Mo salt, Zr source, thiourea and sodium dodecyl benzene sulfonate into water/ethylene glycol, and quickly stirring and uniformly mixing; the mol ratio of Zn salt, Mo salt, Zr salt and thiourea is 1: 1: (0.03-0.1): 3; the material ratio of Zn salt to sodium dodecyl benzene sulfonate is (10-20) mmol: (10-20) mg;
step (2): adding the mixed solution into a high-pressure reaction kettle, and reacting;
and (3): centrifuging and washing the product to obtain popcorn-shaped Zr doped-MoS 2 The particle size of the/ZnS composite material is 5-8 microns.
2. The inorganic high-efficiency antibacterial agent according to claim 1, wherein the Zn salt is zinc nitrate, zinc sulfate, zinc chloride or zinc acetate.
3. The inorganic high-efficiency antibacterial agent according to claim 1, wherein the Mo salt is molybdenum nitrate, molybdenum sulfate, molybdenum chloride or molybdenum acetate.
4. The inorganic high-efficiency antibacterial agent as claimed in claim 1, wherein the reaction temperature is 180-220 ℃; the reaction time is 12-20 h.
5. The inorganic high-efficiency antibacterial agent according to claims 1 to 4, which is washed by deionized water and ethanol for 2 to 4 times alternately.
6. The inorganic high-efficiency antibacterial agent according to claim 1, wherein the Zr salt is zirconium nitrate or zirconium sulfate.
CN202210596420.5A 2022-05-30 2022-05-30 Composite antibacterial material Withdrawn CN114885957A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115413673A (en) * 2022-09-30 2022-12-02 安徽江淮汽车集团股份有限公司 Antibacterial agent suitable for thermoplastic plastics and preparation method thereof
CN117705896A (en) * 2024-02-04 2024-03-15 西安电子科技大学 Flexible NO 2 Preparation method of gas sensor and sensor

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115413673A (en) * 2022-09-30 2022-12-02 安徽江淮汽车集团股份有限公司 Antibacterial agent suitable for thermoplastic plastics and preparation method thereof
CN117705896A (en) * 2024-02-04 2024-03-15 西安电子科技大学 Flexible NO 2 Preparation method of gas sensor and sensor

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Application publication date: 20220812