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CN111374150A - Preparation method of nano-silver/hydrogen peroxide/salicylic acid composite disinfection material - Google Patents

Preparation method of nano-silver/hydrogen peroxide/salicylic acid composite disinfection material Download PDF

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Publication number
CN111374150A
CN111374150A CN201811630841.5A CN201811630841A CN111374150A CN 111374150 A CN111374150 A CN 111374150A CN 201811630841 A CN201811630841 A CN 201811630841A CN 111374150 A CN111374150 A CN 111374150A
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China
Prior art keywords
solution
silver
hydrogen peroxide
nano
salicylic acid
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Pending
Application number
CN201811630841.5A
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Chinese (zh)
Inventor
单加维
孙文明
张流波
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Hengshui Zhongke East Asia Nano Material Technology Co ltd
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Hengshui Zhongke East Asia Nano Material Technology Co ltd
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Priority to CN201811630841.5A priority Critical patent/CN111374150A/en
Publication of CN111374150A publication Critical patent/CN111374150A/en
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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
    • A01N59/16Heavy metals; 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
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/36Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
    • A01N37/38Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
    • A01N37/40Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
    • 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

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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (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)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a preparation method of a nano-silver/hydrogen peroxide/salicylic acid composite disinfection material. The method comprises the following steps of preparing a silver ammonia solution: adding silver nitrate into deionized water, adding ammonia water, and adjusting the pH value to 9. Then adding a reducing agent and a protective agent solution under the condition of stirring, mixing for reaction, further performing ultrasonic treatment and filtering to obtain a colorless and transparent nano silver solution. And adding the nano-silver solution into a hydrogen peroxide solution, and adding salicylic acid to finally prepare the nano-silver/hydrogen peroxide/salicylic acid composite disinfection material. The nano-silver/hydrogen peroxide/salicylic acid composite disinfection material prepared by the method is safe, environment-friendly and nontoxic, can realize a spectrum and lasting sterilization and disinfection effect, and can solve the problem of bacterial and viral pollution in indoor air environments of public places, particularly hospitals and the like.

Description

Preparation method of nano-silver/hydrogen peroxide/salicylic acid composite disinfection material
Technical Field
The invention relates to a preparation method of enhanced spectrum sterilization, in particular to a preparation method of a nano-silver/hydrogen peroxide/salicylic acid composite sterilization material with strong sterilization and disinfection capability, multiple types and lasting effect.
Background
At present, in public places, particularly in hospital environments, more than 200 kinds of bacteria and viruses such as traditional influenza germs, avian influenza, pneumococci and the like are dispersed in the air, and the health of human beings is threatened all the time. Along with the rise of air temperature and the deterioration of environment, the traditional virus generates drug resistance, the novel bacteria and viruses are endless, the bacteria and the viruses are spread along with the air, the speed is high, the influence is wide, large-scale epidemic situation is easily caused, and immeasurable potential influence is brought to the life and property and social order of people.
The existing quaternary ammonium salt disinfection material is applied in large scale due to the characteristics of lasting sterilization and disinfection capability, spectrum, low toxicity and the like on the surface of an object, but the capability of the atomized quaternary ammonium salt for killing viruses and bacteria in the air is extremely limited. And the chlorine-containing disinfection material, ozone or hydrogen peroxide and the like have good killing effect on bacteria and viruses in the air. However, chlorine-containing disinfection materials and ozone have pungent odor, and are emitted in the air, so that the chlorine-containing disinfection materials and the ozone have potential harm to human bodies. The instability and poor disinfection of conventional low concentration hydrogen peroxide solutions also limit their utility. There is a high demand for a new type of sterilization material to cope with the current severe environment.
The problem can be solved by the appearance of the nano-silver/hydrogen peroxide/salicylic acid composite disinfection material, and the composite material has the following functions and characteristics: (1) the nano silver/hydrogen peroxide/salicylic acid composite disinfection material is odorless, colorless and non-foaming, and belongs to a non-toxic grade under the condition that the use concentration is 10 times that recommended. (2) The nano-silver particle size in the prepared nano-silver/hydrogen peroxide/salicylic acid composite disinfection material is less than 5nm, and the nano-silver/hydrogen peroxide/salicylic acid composite disinfection material has very high activity and can quickly sterilize and inhibit bacteria; (3) the low-concentration hydrogen peroxide solution has obviously enhanced oxidizing property and obviously improved sterilizing and disinfecting capability under the acidic condition. The salicylic acid has good sterilization and bacteriostasis effects, the hydrogen peroxide solution can be adjusted to be acidic, and after the salicylic acid is added into the hydrogen peroxide solution, the nano-silver/hydrogen peroxide/salicylic acid composite disinfection material has the advantage that the sterilization and disinfection capacity is improved in geometric grade by virtue of the coupling effect. (4) The low concentration hydrogen peroxide solution is easily decomposed, resulting in short life and greatly reduced performance. However, the nano silver solution is added into hydrogen peroxide and exists as a stabilizing agent, the stabilizing agent can prevent the slow decomposition of the hydrogen peroxide, the composite sterilizing material can be stored for at least 28 months, and the sterilization is carried outThe material can maintain the disinfection effect for a long time and high efficiency, has large application elasticity, is hardly influenced by temperature and light, and even enhances the disinfection capability at high temperature. (5) Two basic components (H) of the composite sterilizing material202And nano silver) improves respective advantages through cooperation, and the sterilization and disinfection effects are more rapid and concentrated. The bacteria and the viruses have a biological film protective layer, the most important means for killing the bacteria and the viruses is that the biological film can be thoroughly destroyed, the nano-silver can destroy cell membranes of the bacteria or the viruses, and then the hydrogen peroxide instantly oxidizes middle proteins of the bacteria or the viruses, so that the bacteria and the viruses can be efficiently and quickly killed. (6) The composite sterilizing material has powerful broad-spectrum sterilization, can kill more than 200 bacteria and viruses of traditional influenza germs, avian influenza, pneumococcus and the like, and can also kill super bacteria and viruses of poliomyelitis, Norwalk and the like which are difficult to kill in hospitals. (7) The nano silver/hydrogen peroxide/salicylic acid composite disinfection material is used for sterilizing through oxidation, so that the problem of drug resistance of viruses, bacteria, fungi, microorganisms and other unknown diseases is solved, and the nano silver/hydrogen peroxide/salicylic acid composite disinfection material can be used for a long time. (8) The nano silver particles in the nano silver/hydrogen peroxide/salicylic acid composite disinfection material have good catalytic oxidation performance under the action of hydrogen peroxide, can quickly remove formaldehyde, peculiar smell and other problems in the space, and greatly expands the application range of the invention.
Disclosure of Invention
The invention aims to provide a preparation method of a nano-silver/hydrogen peroxide/salicylic acid composite disinfection material. The composite sterilizing material is safe, environment-friendly and nontoxic, can realize a spectrum and a lasting sterilizing and disinfecting effect, and can solve the problem of bacterial and viral pollution in indoor air environments of public places, particularly hospitals and the like. The purpose of the invention is realized by the following technical scheme:
(1) preparing a silver ammonia solution: adding silver nitrate into deionized water, wherein the total weight ratio of the silver nitrate to the deionized water is 1: (100-250), adding ammonia water, and adjusting the pH value to 9-11 to prepare a silver ammonia solution as the solution A.
(2)Preparing a nano silver solution: weighing a reducing agent and a protective agent, dissolving the reducing agent and the protective agent in deionized water to obtain a solution B, and dropwise adding the solution B into the solution A by using a burette, wherein the solution A is 30 degrees centigrade in the dropwise adding process0C-500C, mixing and reacting for 2-3 hours under the condition of 150-300rpm, then carrying out ultrasonic treatment on the mixed solution for 60-100 minutes, and finally filtering the mixed solution by using an aqueous filtering membrane to obtain a colorless and transparent nano silver solution.
(3) The reducing agent is one of hydrogen peroxide, hydrazine hydrate, acetone and glucose; the protective agent is one of polyvinylpyrrolidone, stearic acid and polysorbate.
(4) Adding the nano silver solution into a hydrogen peroxide solution, wherein after the addition is finished, the concentration of the hydrogen peroxide solution is 2% -3%, and thus a solution C is obtained;
(5) adding a certain amount of salicylic acid into the solution C, adjusting the pH value to 4-5, and finally preparing the nano-silver/hydrogen peroxide/salicylic acid composite disinfection material.
Detailed Description
Example 1:
0.1g of silver nitrate is weighed and added into 20ml of deionized water, ammonia water is added, and the PH value is adjusted to 9, so that a silver-ammonia solution is prepared and serves as the solution A. 0.4g of hydrazine hydrate reducing agent and 0.3g of polyvinylpyrrolidone protective agent are weighed and dissolved in 80ml of deionized water to obtain a solution B, the solution B is dripped into the solution A by using a burette, and in the dripping process, the solution A is at 30 degrees0And C, mixing and reacting for 2 hours at 150rpm, then carrying out ultrasonic treatment on the mixed solution for 60 minutes, and finally filtering the mixed solution by using an aqueous filtering membrane to obtain a colorless and transparent nano silver solution. Adding the nano silver solution into 100ml of hydrogen peroxide solution with the concentration of 4 percent; 0.13g of salicylic acid is weighed and added to prepare the nano silver/hydrogen peroxide/salicylic acid composite sterilizing material finally.
Example 2:
0.2g of silver nitrate is weighed and added into 20ml of deionized water, ammonia water is added, and the PH value is adjusted to 10, so that a silver-ammonia solution is prepared and serves as the solution A. 0.8g of glucose reducing agent and 0.6g of polysorbate protecting agent are weighed and dissolved in 80ml of deionized water to obtain solution BDripping the solution B into the solution A by using a burette, wherein the solution A is at 40 DEG in the dripping process0And C, mixing and reacting for 3 hours at 200rpm, then carrying out ultrasonic treatment on the mixed solution for 60 minutes, and finally filtering the mixed solution by using an aqueous filtering membrane to obtain a colorless and transparent nano silver solution. Adding the nano silver solution into 300ml of hydrogen peroxide solution with the concentration of 4 percent; 0.27g of salicylic acid is weighed and added to prepare the nano silver/hydrogen peroxide/salicylic acid composite sterilizing material finally.
The nano-silver/hydrogen peroxide/salicylic acid composite disinfection material prepared in the example was tested, and the test results were as follows:
the sterilization effect of the composite sterilization material on microorganisms is evaluated by adopting a bacterial suspension quantitative sterilization experimental method, and test strains are escherichia coli, staphylococcus aureus and candida albicans. The results show that: the composite sterilizing material acts for 3 minutes at the temperature of 20 ℃, the killing rate to escherichia coli and staphylococcus aureus is 100 percent, the killing rate to candida albicans is 99.9999 percent, and the bacteriostasis rate to escherichia coli, staphylococcus aureus and candida albicans reaches more than 99.9999 percent.

Claims (5)

1. A preparation method of a nano-silver/hydrogen peroxide/salicylic acid composite disinfection material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
preparing a silver ammonia solution: adding silver nitrate into deionized water, wherein the total weight ratio of the silver nitrate to the deionized water is 1: (100-250), adding ammonia water, and adjusting the pH value to 9-11 to prepare a silver ammonia solution as the solution A.
2. Preparing a nano silver solution: weighing a reducing agent and a protective agent, dissolving the reducing agent and the protective agent in deionized water to obtain a solution B, and dropwise adding the solution B into the solution A by using a burette, wherein the solution A is 30 degrees centigrade in the dropwise adding process0C-500C, mixing and reacting for 2-3 hours under the condition of 150-300rpm, then carrying out ultrasonic treatment on the mixed solution for 60-100 minutes, and finally filtering the mixed solution by using an aqueous filtering membrane to obtain a colorless and transparent nano silver solution.
3. The reducing agent is one of hydrogen peroxide, hydrazine hydrate, acetone and glucose; the protective agent is one of polyvinylpyrrolidone, stearic acid and polysorbate.
4. And (3) adding the nano silver solution into a hydrogen peroxide solution, wherein after the addition is finished, the concentration of the hydrogen peroxide solution is 2% -3%, and thus a solution C is obtained.
5. Adding a certain amount of salicylic acid into the solution C, adjusting the pH value to 4-5, and finally preparing the nano-silver/hydrogen peroxide/salicylic acid composite disinfection material.
CN201811630841.5A 2018-12-29 2018-12-29 Preparation method of nano-silver/hydrogen peroxide/salicylic acid composite disinfection material Pending CN111374150A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114946880A (en) * 2022-07-05 2022-08-30 桂林清研皓隆新材料有限公司 A kind of silver-loaded titanium dioxide, preparation method and application thereof, and a disinfection and deodorization spray comprising silver-loaded titanium dioxide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103563983A (en) * 2012-07-24 2014-02-12 上海纳米技术及应用国家工程研究中心有限公司 Nano-silver peroxide composite antibacterial solution and preparation method thereof
CN110326625A (en) * 2019-08-07 2019-10-15 山东卓高新材料有限公司 A kind of use in toilet nano-disinfection scavenging material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103563983A (en) * 2012-07-24 2014-02-12 上海纳米技术及应用国家工程研究中心有限公司 Nano-silver peroxide composite antibacterial solution and preparation method thereof
CN110326625A (en) * 2019-08-07 2019-10-15 山东卓高新材料有限公司 A kind of use in toilet nano-disinfection scavenging material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114946880A (en) * 2022-07-05 2022-08-30 桂林清研皓隆新材料有限公司 A kind of silver-loaded titanium dioxide, preparation method and application thereof, and a disinfection and deodorization spray comprising silver-loaded titanium dioxide

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Application publication date: 20200707