CN111345316A - Disinfectant containing hydrogen peroxide silver ions and preparation method thereof - Google Patents

Disinfectant containing hydrogen peroxide silver ions and preparation method thereof Download PDF

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CN111345316A
CN111345316A CN202010365709.7A CN202010365709A CN111345316A CN 111345316 A CN111345316 A CN 111345316A CN 202010365709 A CN202010365709 A CN 202010365709A CN 111345316 A CN111345316 A CN 111345316A
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disinfectant
hydrogen peroxide
lactam
containing polymer
reducing agent
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严敬华
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Zhejiang Shiweikang Biomedical Materials Co ltd
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    • 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
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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    • 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
    • A01N25/22—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 ingredients stabilising the active ingredients
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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    • 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
    • A01N25/30—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 characterised by the surfactants
    • 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
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/40—Peroxides
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/02—Local antiseptics

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Abstract

The application belongs to the technical field of disinfectants, and particularly relates to a disinfectant containing hydrogen peroxide silver ions and a preparation method thereof. The raw materials comprise: 8-12mL of reducing agent, 8-10mL of silver salt, 3-5g of lactam-containing polymer and/or sodium alkyl sulfosuccinate, 70-90mL of hydrogen peroxide, 2-4g of polyethylene glycol and fatty alcohol condensate, and supplementing water to 1000 mL. The disinfectant has excellent bactericidal performance and good stability, can be used on the surface of any object, including but not limited to human skin, ceramic tiles, walls, floors, alloys, bathrooms, glass, tabletops, cooking benches, washing pools, toilets, clothes, curtains, sheets, bedding products, sofas, refrigerators, freezers, washing machines, microwave ovens, mops, plastics, rubbers and the like, and can also be used for air disinfection, for example, the indoor environment is infected by pathogens such as bacteria, viruses and the like which are attached to suspended particles.

Description

Disinfectant containing hydrogen peroxide silver ions and preparation method thereof
Technical Field
The invention belongs to the technical field of disinfectants, and particularly relates to a disinfectant containing hydrogen peroxide silver ions and a preparation method thereof.
Background
Sterilization and disinfection are indispensable links in production and life of people, especially in the present day when the novel coronavirus is very serious; however, the traditional sterilizing disinfectant, such as chlorine series sterilizing products, has poor sterilizing and disinfecting performance and can leave harmful substances; hydrogen peroxide with a certain concentration can be used as a disinfectant for sterilization and disinfection, but the hydrogen peroxide has poor storage stability; the slow sterilization speed of the hydrogen peroxide, the high concentration required and the like result in less extensive application.
The emergence of nanotechnology makes the bactericidal performance of silver in a nanometer state generate qualitative leap. The nano silver can generate strong sterilization effect under the condition of small dosage, has strong permeability, broad sterilization effect and no drug resistance; and the nano silver can promote the healing of wounds, the growth of cells and the repair of damaged cells, has no toxic reaction and has no stimulation reaction on skin. Therefore, the nano silver antibacterial material can be applied to the fields of functional plastics, functional coatings, textile fibers, air purification, food, daily chemicals, medical treatment and the like, has a very wide market prospect, and gradually becomes a research hotspot in recent years. The nano silver has strong inhibition and killing effects on dozens of pathogenic microorganisms such as escherichia coli, gonococcus, chlamydia trachomatis and the like, and can not generate drug resistance.
However, the existing hydrogen peroxide sterilization disinfectant also has the defects of weak sterilization capability, poor stability and the like.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a disinfectant containing silver hydroperoxide ions, comprising: 8-12mL of reducing agent, 8-10mL of silver salt, 3-5g of lactam-containing polymer and/or sodium alkyl sulfosuccinate, 70-90mL of hydrogen peroxide, 2-4g of polyethylene glycol and fatty alcohol condensate, and supplementing water to 1000 mL.
As a preferable technical scheme, the reducing agent is selected from at least one of hydrazine hydrate, sodium borohydride, glucose and organic alcohol.
As a preferred technical scheme, the reducing agent is selected from at least one of glycerol, lactitol, n-amyl alcohol, n-hexyl alcohol and n-dodecyl alcohol.
As a preferable technical scheme, the mass ratio of the lactam group-containing polymer to the sodium sulfosuccinate alkyl ester is (3-4): 1.
as a preferred technical scheme, the lactam group-containing polymer has a lactam group dipole moment of 30-42.
As a preferable technical scheme, the lactam group-containing polymer further comprises a methylene group in a long chain; the environments of two ends of the lactam group-containing polymer are different, one end of an oxygen atom is exposed, and one end containing an N atom is surrounded by methyl and methylene.
As a preferable technical scheme, the hydroxyl value of the polyethylene glycol and fatty alcohol condensate is 90-110mgKOH/g, and the HLB value is 12-14.
As a preferred technical scheme, the disinfectant also comprises 8-12mg of quinoxaline compounds and/or p-hydroxyacetanilide.
As a preferable technical scheme, the weight ratio of the quinoxaline compound to the p-hydroxyacetanilide is 1: (2-4).
The second aspect of the invention provides a preparation method of the disinfectant, which comprises the following steps:
(1) sequentially adding a reducing agent, a lactam group-containing polymer and/or sodium sulfosuccinate alkyl ester into 800mL of water at the rotation speed of 1000-1500r/min, and stirring until the mixture is transparent and clear; heating to 20-30 ℃, adding silver salt, continuing heating and stirring, and reacting for 2-4 hours; (2) and (2) adding a polyethylene glycol and fatty alcohol condensation product, hydrogen peroxide, a quinoxaline compound and/or p-hydroxyacetanilide into the step (1), and supplementing the residual amount of water to 1000mL to obtain the compound.
Has the advantages that: the disinfectant has excellent bactericidal performance and good stability, can be used on the surface of any object (can be diluted by 10-100 times according to actual requirements), and comprises but is not limited to human skin, ceramic tiles, walls, floors, alloys, bathrooms, glass, tabletops, cooking benches, washing pools, toilets, clothes, curtains, sheets, bedding products, sofas, refrigerators, freezers, washing machines, microwave ovens, mops, plastics, rubber and the like, and can also be used for air disinfection, for example, the indoor environment is infected by pathogens such as bacteria, viruses and the like on suspended particles; volatile gaseous pollutants such as radon, formaldehyde, benzene series, ammonia and the like after decoration and fitment; inhalable particles such as dust, smoke, pollen, etc.; the peculiar smell of life, such as metabolism in a new city, musty smell, garbage smell and the like; and (3) invasion of outdoor polluted air, such as industrial waste gas, automobile tail gas, soil bag dust and the like.
Detailed Description
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In order to solve the problems, the invention provides a disinfectant containing silver hydroperoxide ions, which comprises the following raw materials: 8-12mL of reducing agent, 8-10mL of silver salt, 3-5g of lactam-containing polymer and/or sodium alkyl sulfosuccinate, 70-90mL of hydrogen peroxide, 2-4g of polyethylene glycol and fatty alcohol condensate, and supplementing water to 1000 mL.
Reducing agent
Reducing the silver ions into nano silver by adding a reducing agent.
As a preferred embodiment, the reducing agent is selected from at least one of hydrazine hydrate, sodium borohydride, glucose, and organic alcohol. Preferably, the reducing agent is selected from at least one of glycerol, lactitol, n-pentanol, n-hexanol, and n-dodecanol. Alcohol with different proportions is compounded to control the reduction speed of silver ions, so that the preparation of nano silver with low particle size and uniform dispersion is facilitated; more preferably, the reducing agent is glycerol, n-pentanol, n-dodecanol; the weight ratio of the glycerol to the n-pentanol to the n-dodecanol is (6-8): 3: 1.
silver salts
The silver salt mainly provides silver ions, and is not particularly limited; in the present application, the silver salt is an aqueous nitrate solution. Wherein the concentration of the silver nitrate is 0.05 mol/L.
Lactam group-containing polymer and/or sodium sulfosuccinate
As a preferred embodiment, the mass ratio of the lactam-group containing polymer to the sodium sulfosuccinate alkyl ester is (3-4): 1.
as a preferred embodiment, the lactam-group containing polymer has a lactam-group dipole moment of 30 to 42; preferably, the lactam group of the lactam group-containing polymer is a butyrolactam group; more preferably, the lactam-group containing polymer further comprises a methylene group in the long chain; further preferably, the environments of both ends of the lactam group-containing polymer are different, one end of the oxygen atom is exposed, and the other end of the N atom is surrounded by a methyl group and a methylene group.
As a preferred embodiment, the lactam group-containing polymer has a viscosity (mPa.s/25 ℃/5% aq) of 1.1 to 2.7 and a number average molecular weight of 10000-40000.
In a preferred embodiment, the alkyl group in the sodium sulfosuccinate is at least one selected from the group consisting of ethyl, propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, n-pentyl, isopentyl, sec-pentyl, tert-pentyl, n-hexyl, and isohexyl.
More preferably, the alkyl group in the sodium sulfosuccinate is n-hexyl.
The preparation method of the sodium alkyl sulfosuccinate with n-hexyl alkyl comprises the following steps: 1) adding 4mol of maleic anhydride, 2mol of 1, 3-propylene glycol and a solid acid catalyst (the solid acid catalyst is 3 wt% of the maleic anhydride) into a reactor, uniformly stirring, heating to 100 +/-2.5 ℃, and reacting for 5-6 hours; 2) adding 5mol of n-hexanol into the step 1), uniformly stirring and heating to 200 +/-2.5 ℃, reacting for 4-5 hours to obtain a mixed solution of a compound 2, and filtering to remove the catalyst; 3) reducing the temperature to 110 +/-2.5 ℃, adding sodium hydroxide in the step 2) to adjust the pH value to 7, then adding 4mol of sodium bisulfite (sodium bisulfite water solution with the mass concentration of 35%) and reacting for 40-60min to obtain the sodium hydrogen sulfite. Wherein the solid acid catalyst is purchased from south university synthetic chemistry, ltd.
The nano silver obtained by the method can be combined with sulfydryl in metabolic enzyme of pathogenic bacteria, so that the metabolic enzyme loses activity; and form a reversible complex after reacting with peptidoglycan of the exposed bacterial cell wall, preventing the bacteria from transporting oxygen and energy into the cell interior; can also combine with the DNA of pathogenic bacteria to cause the structural denaturation of the DNA, and finally inhibit the DNA replication; particularly, the polymer containing lactam group and the sodium sulfosuccinate alkyl ester are added in the preparation process, so that the prepared disinfection sterilizing agent has excellent sterilizing performance; the conjecture is that the long chain of the polymer containing lactam group comprises methylene groups, the two ends of the lactam group are in different environments, so that the polymer is easy to adsorb on the surface of the generated nano-silver to play a role in protection, and after the alkyl ester sodium sulfosuccinate is added, the adsorption rate of the polymer containing lactam group and the newly generated nano-particles is promoted to be greater than the rate of Ag mutual aggregation, so that the obtained nano-silver has strong penetrating power while the surface activity is enhanced.
Hydrogen peroxide
Pure hydrogen peroxide is light blue viscous liquid, can be mixed and dissolved with water in any proportion, and is a strong oxidant; the medical hydrogen peroxide can kill intestinal pathogenic bacteria, pyogenic coccus and pathogenic yeast, and is generally used for disinfecting the surfaces of objects. The hydrogen peroxide has the oxidation effect, but the concentration of the medical hydrogen peroxide is equal to or lower than 3 percent, when the medical hydrogen peroxide is wiped on a wound surface, the wound surface can be burnt, and the surface is oxidized into white and bubbles are generated.
The hydrogen peroxide is a commercial product, and can be enumerated by 27.5% of hydrogen peroxide, 35% of hydrogen peroxide and 50% of hydrogen peroxide, and the hydrogen peroxide is 35% of hydrogen peroxide in mass fraction in the application and purchased from fine chemical engineering in the day of Anhui Ling.
Condensation product of polyethylene glycol and fatty alcohol
As a preferred embodiment, the condensate of polyethylene glycol and fatty alcohol has a hydroxyl value of 90 to 110mgKOH/g and an HLB value of 12 to 14. Preferably, the condensate of polyethylene glycol and fatty alcohol has a hydroxyl value of 90 to 100mgKOH/g and an HLB value of 13.
Wherein HLB refers to the hydrophilic-lipophilic balance.
The applicant has found that the addition of a polyethylene glycol and fatty alcohol condensate having a hydroxyl value of 90 to 100mgKOH/g and an HLB value of 13 improves the stability of hydrogen peroxide, which is a relatively unstable substance and causes a reduction in sterilization due to decomposition after being left for a certain period of time; however, after the disinfectant is placed at 50 ℃ for 4 hours, the reduction rate of hydrogen peroxide exceeds 50%, so that the disinfectant is difficult to play a good role in polar environments such as severe heat and the like, and the wide application of the disinfectant is limited; the applicant has surprisingly found that when the reducing agent is glycerol, n-pentanol, n-dodecanol, the disinfectant exhibits a hydrogen peroxide reduction of less than 30% after being left at 50 ℃ for 4 hours. The supposition is that the hydrophilic hydroxyl groups of the glycerol and the n-amyl alcohol are smaller and are reasonably inserted into the overlapped gaps of the n-dodecanol, the polyethylene glycol and the fatty alcohol condensation compound to form a tighter protection structure. And when the weight ratio of the glycerol to the n-amyl alcohol to the n-dodecyl alcohol is (6-8): 3: 1, the sterilization performance of the disinfectant is not affected, and the reduction rate of the hydrogen peroxide is less than 15 percent.
As a preferred embodiment, the disinfectant further comprises 8-12mg of quinoxaline compounds and/or p-hydroxyacetanilide; preferably, the weight ratio of the quinoxaline compound to the p-hydroxyacetanilide is 1: (2-4). Further preferably, the quinoxaline compound is 6, 7-dihydroxy-2-quinoxaline carboxylic acid. The 6, 7-dihydroxy-2-quinoxaline carboxylic acid has CAS number 122234-89-3. The CAS number of the p-hydroxyacetanilide is 103-90-2.
The disinfectant can be applied to the surface of any object (can be diluted by 10-100 times according to actual requirements); including but not limited to human skin, tiles, walls, floors, alloys, bathrooms, glass, tabletops, stovetops, sinks, toilets, clothing, curtains, sheets, bedding, sofas, refrigerators, freezers, washing machines, microwaves, mops, plastics, rubber, etc., and also for air disinfection, e.g. indoor environments subject to pathogens such as bacteria, viruses, etc. on suspended particles; volatile gaseous pollutants such as radon, formaldehyde, benzene series, ammonia and the like after decoration and fitment; inhalable particles such as dust, smoke, pollen, etc.; the peculiar smell of life, such as metabolism in a new city, musty smell, garbage smell and the like; and (3) invasion of outdoor polluted air, such as industrial waste gas, automobile tail gas, soil bag dust and the like.
The disinfectant basically has no corrosion effect on stainless steel and carbon steel, but has slight corrosion effect on copper, aluminum, magnesium and the like, and quinoxaline is added into the disinfectantThe compound and the p-hydroxyacetanilide reduce the corrosion effect of the disinfectant on copper, aluminum and magnesium, particularly the weight ratio of the quinoxaline compound to the p-hydroxyacetanilide is 1 (2-4), a magnesium alloy with the type of AZ31 is soaked in the disinfectant for 4 days, the corrosion inhibition efficiency exceeds 98 percent, the presumption is that the content of Al in the magnesium alloy AZ31 is 2.5-3.5 percent, Zn0.6-1.4 percent and Fe 0.003 percent, the magnesium alloy also contains Ni, Cu, Mn and the like, and belongs to a Mg-Al-Zn ternary system, the p-hydroxyacetanilide, 6, 7-dihydroxy-2-quinoxaline carboxylic acid and other components mutually promote, so that carboxyl and N atoms can be well in a second phase Mg with β in skeleton distribution among the branches and crystal boundaries of α bodies17Al12And the like to form a protective film.
A second aspect of the invention provides a method for preparing the disinfectant, comprising the steps of:
(1) sequentially adding a reducing agent, a lactam group-containing polymer and/or sodium sulfosuccinate alkyl ester into 800mL of water at the rotation speed of 1000-1500r/min, and stirring until the mixture is transparent and clear; heating to 20-30 ℃, adding silver salt, continuing heating and stirring, and reacting for 2-4 hours; (2) and (2) adding a polyethylene glycol and fatty alcohol condensation product, hydrogen peroxide, a quinoxaline compound and/or p-hydroxyacetanilide into the step (1), and supplementing the residual amount of water to 1000mL to obtain the compound.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
A disinfectant containing silver hydroperoxide ions comprises the following raw materials: 10mL of reducing agent, 9mL of silver salt, 4g of lactam-containing polymer and sodium sulfosuccinate alkyl ester, 80mL of hydrogen peroxide, 3g of polyethylene glycol and fatty alcohol condensate, 10mg of 6, 7-dihydroxy-2-quinoxaline carboxylic acid and p-hydroxyacetanilide, and supplementing water to 1000 mL.
The reducing agent is glycerol, n-amyl alcohol and n-dodecanol (CAS number: 27342-88-7); the weight ratio of the glycerol to the n-amyl alcohol to the n-dodecanol is 7: 3: 1.
the silver salt is silver nitrate water solution, and the concentration of the silver nitrate is 0.05 mol/L.
The mass ratio of the lactam-containing polymer to the sodium sulfosuccinate alkyl ester is 3.5: 1. the lactam group-containing polymer is polyvinylpyrrolidone; the polyvinylpyrrolidone is purchased from Ganbuke New Material science and technology (Shanghai) Co., Ltd, and the product specification is PVPK 30.
The alkyl in the succinic acid alkyl ester sodium sulfonate is n-hexyl.
The preparation method of the sodium alkyl sulfosuccinate with n-hexyl alkyl comprises the following steps: 1) adding 4mol of maleic anhydride, 2mol of 1, 3-propylene glycol and a solid acid catalyst (the solid acid catalyst is 3 wt% of the maleic anhydride) into a reactor, uniformly stirring, heating to 100 +/-2.5 ℃, and reacting for 5 hours; 2) adding 5mol of n-hexanol into the step 1), uniformly stirring, heating to 200 +/-2.5 ℃, reacting for 4 hours to obtain a mixed solution of a compound 2, and filtering to remove the catalyst; 3) reducing the temperature to 110 +/-2.5 ℃, adding sodium hydroxide in the step 2) to adjust the pH value to 7, then adding 4mol of sodium bisulfite (sodium bisulfite water solution with the mass concentration of 35%) and reacting for 50min to obtain the sodium hydrogen sulfite. Wherein the solid acid catalyst is purchased from south university synthetic chemistry, ltd.
The hydrogen peroxide is 35% hydrogen peroxide by mass and is purchased from fine chemical engineering in Rabdosia.
The condensate of the polyethylene glycol and the fatty alcohol is fatty alcohol-polyoxyethylene ether AEO-9.
The weight ratio of the 6, 7-dihydroxy-2-quinoxaline carboxylic acid to the p-hydroxyacetanilide is 1: 3.
the preparation method of the disinfectant comprises the following steps:
(1) sequentially adding a reducing agent, a polymer containing lactam group and sodium sulfosuccinate alkyl ester into 800mL of water at the rotating speed of 1000r/min, and stirring until the mixture is transparent and clear; heating to 30 ℃, adding silver salt, continuing heating and stirring, and reacting for 3 hours; (2) and (2) adding a polyethylene glycol and fatty alcohol condensation product, hydrogen peroxide, 6, 7-dihydroxy-2-quinoxaline carboxylic acid and p-hydroxyacetanilide into the step (1), and supplementing the residual amount of water to 1000mL to obtain the compound.
Example 2
A disinfectant containing silver hydroperoxide ions comprises the following raw materials: 10mL of reducing agent, 9mL of silver salt, 4g of lactam-containing polymer, 80mL of hydrogen peroxide, 3g of polyethylene glycol and fatty alcohol condensate, 10mg of 6, 7-dihydroxy-2-quinoxaline carboxylic acid and p-hydroxyacetanilide, and supplementing water to 1000 mL.
The reducing agent is glycerol, n-amyl alcohol and n-dodecanol; the weight ratio of the glycerol to the n-amyl alcohol to the n-dodecanol is 7: 3: 1.
the silver salt is silver nitrate water solution, and the concentration of the silver nitrate is 0.05 mol/L.
The lactam group-containing polymer is polyvinylpyrrolidone; the polyvinylpyrrolidone is purchased from Ganbuke New Material science and technology (Shanghai) Co., Ltd, and the product specification is PVPK 30.
The hydrogen peroxide is 35% hydrogen peroxide by mass and is purchased from fine chemical engineering in Rabdosia.
The condensate of the polyethylene glycol and the fatty alcohol is fatty alcohol-polyoxyethylene ether AEO-9.
The weight ratio of the 6, 7-dihydroxy-2-quinoxaline carboxylic acid to the p-hydroxyacetanilide is 1: 3.
the preparation method of the disinfectant has the specific steps as in example 1.
Example 3
A disinfectant containing silver hydroperoxide ions comprises the following raw materials: 10mL of reducing agent, 9mL of silver salt, 4g of succinic acid alkyl ester sodium sulfonate, 80mL of hydrogen peroxide, 3g of polyethylene glycol and fatty alcohol condensate, 10mg of 6, 7-dihydroxy-2-quinoxaline carboxylic acid and p-hydroxyacetanilide, and supplementing water to 1000 mL.
The reducing agent is glycerol, n-amyl alcohol and n-dodecanol; the weight ratio of the glycerol to the n-amyl alcohol to the n-dodecanol is 7: 3: 1.
the silver salt is silver nitrate water solution, and the concentration of the silver nitrate is 0.05 mol/L.
The alkyl in the succinic acid alkyl ester sodium sulfonate is n-hexyl.
The preparation method of the sodium alkyl sulfosuccinate with n-hexyl alkyl comprises the following steps: 1) adding 4mol of maleic anhydride, 2mol of 1, 3-propylene glycol and a solid acid catalyst (the solid acid catalyst is 3 wt% of the maleic anhydride) into a reactor, uniformly stirring, heating to 100 +/-2.5 ℃, and reacting for 5 hours; 2) adding 5mol of n-hexanol into the step 1), uniformly stirring, heating to 200 +/-2.5 ℃, reacting for 4 hours to obtain a mixed solution of a compound 2, and filtering to remove the catalyst; 3) reducing the temperature to 110 +/-2.5 ℃, adding sodium hydroxide in the step 2) to adjust the pH value to 7, then adding 4mol of sodium bisulfite (sodium bisulfite water solution with the mass concentration of 35%) and reacting for 50min to obtain the sodium hydrogen sulfite. Wherein the solid acid catalyst is purchased from south university synthetic chemistry, ltd.
The hydrogen peroxide is 35% hydrogen peroxide by mass and is purchased from fine chemical engineering in Rabdosia.
The condensate of the polyethylene glycol and the fatty alcohol is fatty alcohol-polyoxyethylene ether AEO-9.
The weight ratio of the 6, 7-dihydroxy-2-quinoxaline carboxylic acid to the p-hydroxyacetanilide is 1: 3.
the preparation method of the disinfectant containing hydrogen peroxide is the same as that of the embodiment 1.
Example 4
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the alkyl in the succinic acid alkyl ester sodium sulfonate is n-undecyl.
The preparation method of the sodium sulfosuccinate alkyl ester with the alkyl group being n-undecyl comprises the following steps: 1) adding 4mol of maleic anhydride, 2mol of 1, 3-propylene glycol and a solid acid catalyst (the solid acid catalyst is 3 wt% of the maleic anhydride) into a reactor, uniformly stirring, heating to 100 +/-2.5 ℃, and reacting for 5 hours; 2) adding 5mol of n-undecanol in the step 1), uniformly stirring, heating to 200 +/-2.5 ℃, reacting for 4 hours to obtain a mixed solution of a compound 2, and filtering to remove the catalyst; 3) reducing the temperature to 110 +/-2.5 ℃, adding sodium hydroxide in the step 2) to adjust the pH value to 7, then adding 4mol of sodium bisulfite (sodium bisulfite water solution with the mass concentration of 35%) and reacting for 50min to obtain the sodium hydrogen sulfite. Wherein the solid acid catalyst is purchased from south university synthetic chemistry, ltd.
Example 5
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the reducing agent is glycerol and n-amyl alcohol; the weight ratio of the glycerol to the n-amyl alcohol is 7: 3.
example 6
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the reducing agent is glycerol and n-dodecanol; the weight ratio of the glycerol to the n-dodecanol is 7: 1.
example 7
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the reducing agent is n-amyl alcohol or n-dodecanol; the weight ratio of the n-pentanol to the n-dodecanol is 3: 1.
example 8
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the reducing agent is glycerol, n-amyl alcohol and n-dodecanol; the weight ratio of the glycerol to the n-amyl alcohol to the n-dodecanol is 1: 3: 1.
example 9
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the reducing agent is glycerol, n-amyl alcohol and n-dodecanol; the weight ratio of the glycerol to the n-amyl alcohol to the n-dodecanol is 10: 3: 1.
example 10
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the weight ratio of the 6, 7-dihydroxy-2-quinoxaline carboxylic acid to p-hydroxyacetanilide is 1: 1.
example 11
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the weight ratio of the 6, 7-dihydroxy-2-quinoxaline carboxylic acid to p-hydroxyacetanilide is 1: 5.
example 12
The specific implementation mode of the disinfectant containing hydrogen peroxide silver ions is the same as that of the disinfectant in the example 1, and the differences are that: the 6, 7-dihydroxy-2-quinoxaline carboxylic acid is replaced by sodium dodecylbenzenesulfonate.
Performance testing
Antibacterial property: escherichia coli and staphylococcus aureus are used as tested strains, antibacterial performance of the bactericide prepared in different embodiments is inspected through a bacteriostatic ring antibacterial test method, and the specific operation is as follows: 0.1ml of test suspension (10) was aspirated7cfu/ml) is placed in a plate containing nutrient agar, a cotton swab is used for uniformly smearing, then a disinfectant to be tested (20ul) diluted by 5 times is dripped on the surface of the culture medium coated with the tested bacteria, the culture medium is covered and inverted and cultivated in a thermostat at 37 ℃ for 14h, and the size of the bacteriostatic ring is observed.
And (3) testing the inhibition zone: according to the judgment standard of the diameter of the inhibition zone, the diameter of not less than 15mm is highly sensitive, the diameter of not less than 10mm is less than 15mm is moderately sensitive, the diameter of less than 10mm is lowly sensitive, and the larger the diameter is, the stronger the antibacterial activity is.
Stability the disinfectant described in the examples was tested for hydrogen peroxide content after 4 hours at 50 ℃ by the potassium permanganate titration method and the rate of decrease (%) was calculated as × 100%/initial hydrogen peroxide content (initial hydrogen peroxide content-hydrogen peroxide content after 4 hours of standing), where rates of decrease of less than 15% were recorded as good, rates of greater than 15% and less than 30% were recorded as medium and rates of greater than 40% were recorded as bad.
The corrosion inhibition performance is that magnesium alloy with the model of AZ31 is soaked in a disinfectant for 4 days, the corrosion inhibition rate is calculated, the weight of the magnesium alloy is × 100 percent/the weight of the initial magnesium alloy after the magnesium alloy is placed for 4 days, wherein the corrosion inhibition rate is recorded as excellent when being more than 98 percent, recorded as medium when being less than 98 percent and 80 percent, recorded as poor when being less than 80 percent.
Figure BDA0002476472970000111
The disinfectant described in example 1 was tested for corrosion inhibition efficiency on magnesium alloy AZ91 in the same manner, and found to be of moderate corrosion inhibition efficiency.
The disinfectant described in the present application meets the relevant requirements of the disinfection technical code in all other aspects.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.

Claims (10)

1. A disinfectant containing silver hydroperoxide ions, which is characterized in that the raw materials comprise: 8-12mL of reducing agent, 8-10mL of silver salt, 3-5g of lactam-containing polymer and/or sodium alkyl sulfosuccinate, 70-90mL of hydrogen peroxide, 2-4g of polyethylene glycol and fatty alcohol condensate, and supplementing water to 1000 mL.
2. The disinfectant of claim 1 wherein said reducing agent is selected from at least one of hydrazine hydrate, sodium borohydride, glucose, and organic alcohols.
3. The disinfectant of claim 2 wherein said reducing agent is selected from the group consisting of at least one of glycerol, lactitol, n-pentanol, n-hexanol, and n-dodecanol.
4. The disinfectant of claim 1, wherein said lactam-containing polymer and sodium sulfosuccinate are present in a mass ratio of (3-4): 1.
5. the disinfectant of claim 4 wherein said lactam-group containing polymer has a lactam-group dipole moment of from 30 to 42.
6. The disinfectant of claim 5 wherein said lactam-group containing polymer further comprises methylene groups in the long chain; the environments of two ends of the lactam group-containing polymer are different, one end of an oxygen atom is exposed, and one end containing an N atom is surrounded by methyl and methylene.
7. The disinfectant of claim 1 wherein said polyethylene glycol and fatty alcohol condensate has a hydroxyl number of 90 to 110mgKOH/g and an HLB of 12 to 14.
8. The disinfectant according to claim 1, wherein said disinfectant further comprises a quinoxaline compound and/or p-hydroxyacetanilide in an amount of 8 to 12 mg.
9. The disinfectant according to claim 8, wherein the weight ratio of said quinoxaline compound to p-hydroxyacetanilide is 1: (2-4).
10. A method of preparing a disinfectant as claimed in claim 8 or 9, comprising the steps of:
(1) sequentially adding a reducing agent, a lactam group-containing polymer and/or sodium sulfosuccinate alkyl ester into 800mL of water at the rotation speed of 1000-1500r/min, and stirring until the mixture is transparent and clear; heating to 20-30 ℃, adding silver salt, continuing heating and stirring, and reacting for 2-4 hours; (2) and (2) adding a polyethylene glycol and fatty alcohol condensation product, hydrogen peroxide, a quinoxaline compound and/or p-hydroxyacetanilide into the step (1), and supplementing the residual amount of water to 1000mL to obtain the compound.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112136809A (en) * 2020-10-12 2020-12-29 浙江施维康生物医学材料有限公司 Compound solid fumigation disinfectant and using method thereof
CN112931527A (en) * 2021-02-05 2021-06-11 天天向上(宁波)医疗科技有限公司 Hydrogen peroxide silver ion disinfectant and preparation process thereof
CN114532359A (en) * 2021-04-22 2022-05-27 北京洁尔爽高科技有限公司 Stable composition, application thereof and product containing same

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112136809A (en) * 2020-10-12 2020-12-29 浙江施维康生物医学材料有限公司 Compound solid fumigation disinfectant and using method thereof
CN112931527A (en) * 2021-02-05 2021-06-11 天天向上(宁波)医疗科技有限公司 Hydrogen peroxide silver ion disinfectant and preparation process thereof
CN114532359A (en) * 2021-04-22 2022-05-27 北京洁尔爽高科技有限公司 Stable composition, application thereof and product containing same
CN114532359B (en) * 2021-04-22 2024-01-30 北京洁尔爽高科技有限公司 Stable composition, application thereof and product containing composition

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