CN113455517B - Environment-friendly slow-release antibacterial disinfection emulsion and preparation method thereof - Google Patents

Environment-friendly slow-release antibacterial disinfection emulsion and preparation method thereof Download PDF

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CN113455517B
CN113455517B CN202110743772.4A CN202110743772A CN113455517B CN 113455517 B CN113455517 B CN 113455517B CN 202110743772 A CN202110743772 A CN 202110743772A CN 113455517 B CN113455517 B CN 113455517B
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peroxide
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antibacterial
suspending agent
deionized water
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CN113455517A (en
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徐强
吴群绒
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Wuhan Huaxin Meikang New Material Technology Co ltd
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Wuhan Huaxin Meikang New Material Technology Co ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • 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
    • A01N25/02—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 liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • 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
    • A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
    • A01N31/02—Acyclic compounds
    • Y—GENERAL 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
    • 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

Abstract

The invention discloses a preparation method of an environment-friendly slow-release antibacterial disinfection emulsion, belonging to the field of antibacterial disinfection. The preparation method of the antibacterial disinfectant comprises the following steps: firstly, preparing nano peroxide with hydroxyl-rich surface, adding the nano peroxide into deionized water containing a suspending agent, wherein the suspending agent is a suspending agent containing polyhydroxy, and adding a proper amount of dispersing agent to uniformly and stably suspend the nano peroxide with hydroxyl-rich surface in a solvent to obtain the antibacterial disinfection emulsion. The invention also discloses an environment-friendly slow-release antibacterial disinfection emulsion. The antibacterial disinfectant disclosed by the invention does not contain flammable high-concentration alcohol and toxic chloride ions, has the characteristics of small irritation to a human body and environmental friendliness, is simple in preparation process condition, excellent in sterilization effect and has a lasting sterilization effect; and a small amount of other antibacterial agents can be added for compounding so as to achieve wider application range and better antibacterial performance.

Description

Environment-friendly slow-release antibacterial disinfection emulsion and preparation method thereof
Technical Field
The invention belongs to the technical field of antibacterial disinfectants, and particularly relates to an environment-friendly slow-release antibacterial disinfection emulsion and a preparation method thereof.
Background
In recent years, infectious diseases caused by rapid transmission of harmful microorganisms such as mutated bacteria and germs have caused great harm to human health and life and production. Since the outbreak of new coronary pneumonia, antibacterial and disinfectant products have become hot spots for research. Disinfectant and antibacterial hand sanitizer have become necessary cleaning products in daily life. However, the components of the traditional disinfectant and bactericide are mainly ethanol and chlorine-containing compounds, so that the traditional disinfectant and bactericide has short antibacterial duration, pungent smell, volatility and certain toxicity, and can cause certain damage to human skin. Nanometer metal ions such as silver and zinc ions are hot spots in the antibacterial field due to their high surface energy and broad-spectrum bacteriostatic activity.
For example, chinese patent CN102860923A discloses a nano-silver bacteriostatic hand sanitizer and a preparation method thereof, which has a long-acting bactericidal effect. However, silver, as a noble metal, is expensive to produce and is also oxidized to change color; and the silver is used as a heavy metal, does not participate in human metabolism, and can affect human health after being used for a long time. Therefore, the macromolecular antibacterial liquid with good biocompatibility can be produced. CN106491633A discloses an antimicrobial disinfectant with good biocompatibility, which is based on biological macromolecules, and a series of antimicrobial disinfectants are obtained by adjusting the types of active groups and mixing the active groups with auxiliary agents, however, the disinfectant has high price, needs a plurality of auxiliary agents and is complicated to operate. Therefore, the peroxide with low cost, broad-spectrum antibacterial property, high efficiency, no toxicity, no color and no odor is favored in the antibacterial field. For example, chinese patent publication No. CN102696674A discloses a low-concentration hydrogen peroxide disinfectant with a simple preparation process, which has a rapid and significant bactericidal effect. However, hydrogen peroxide has poor stability and is easily decomposed into oxygen and water, so that the disinfection effect is influenced; moreover, the oxydol has strong oxidability and has severe stimulation to human skin when the concentration is too high. Therefore, the development of a broad-spectrum antibacterial emulsion of nano peroxide, which is environment-friendly, low in cost and simple in preparation process, is needed.
Disclosure of Invention
Aiming at one or more of the defects or the improvement requirements of the prior art, the invention provides the environment-friendly slow-release antibacterial disinfection emulsion and the preparation method thereof, and the environment-friendly antibacterial emulsion with low cost, lasting antibacterial property, broad-spectrum antibacterial activity and environment friendliness is prepared.
In order to achieve the above objects, according to one aspect of the present invention, there is provided a method for preparing an environment-friendly slow-release antibacterial sterilizing emulsion, comprising the steps of:
s1: preparing nano peroxide;
dissolving metal salt in deionized water, adding a precipitator, uniformly stirring, adding hydrogen peroxide for peroxidation, and washing and filtering to obtain nano peroxide with a surface rich in hydroxyl after the reaction is finished;
s2: adding a proper amount of the nano peroxide which is prepared in the step S1 and has rich hydroxyl on the surface into deionized water containing a suspending agent, wherein the suspending agent is a suspending agent containing polyhydroxy; adding a proper amount of dispersant to ensure that the nano peroxide with rich hydroxyl on the surface is evenly and stably suspended in the solvent to obtain the antibacterial disinfection emulsion;
the nano peroxide is one or more of magnesium peroxide, calcium peroxide and zinc peroxide.
As a further improvement of the invention, in step S1, the metal salt is one or more of nitrate, chloride, acetate or sulfate containing calcium, magnesium and zinc; the precipitator is ammonia water, sodium hydroxide or potassium hydroxide;
and the molar ratio of the metal salt to the precipitant is 1: 2-1: 4, the molar ratio of the metal salt to the hydrogen peroxide is 1: 1-1: 10.
as a further improvement of the invention, in step S2, the suspending agent is one or more of ethylene glycol, propylene glycol and glycerol; the dispersing agent is one or more of polyethylene glycol, tween-80, polyvinylpyrrolidone, sodium alginate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
As a further improvement of the invention, the mass volume ratio of the suspending agent to the deionized water in the deionized water containing the suspending agent is 5-10%.
As a further improvement of the invention, the mass-volume ratio of the nano peroxide to the deionized water containing the suspending agent is 1: 50-1: 900, the mass ratio of the dispersing agent to the nano peroxide is 1: 1-1: 15.
as a further improvement of the invention, in the antibacterial and disinfectant emulsion prepared in step S2, a compound antibacterial agent is continuously added, wherein the compound antibacterial agent is at least one of magnesium oxide, titanium dioxide, hydrogen peroxide or ethanol, and the addition ratio of the compound antibacterial agent is 0-20%.
According to a second aspect of the present invention, there is provided an environmentally friendly slow-release antibacterial disinfectant emulsion prepared by mixing a nano peroxide, deionized water containing a polyhydroxy suspending agent, and a dispersing agent; wherein the content of the first and second substances,
the nano peroxide is obtained by dissolving metal salt in deionized water, adding a precipitator, uniformly stirring, adding hydrogen peroxide for peroxidation, and washing and filtering after the reaction is finished to obtain the nano peroxide with the surface rich in hydroxyl;
the peroxide with rich hydroxyl groups on the surface is uniformly and stably suspended in the solvent by adding the peroxide into the deionized water containing the polyhydroxy suspending agent and adding the dispersing agent.
As a further improvement of the invention, the nano peroxide is one or more of magnesium peroxide, calcium peroxide and zinc peroxide; the polyhydroxy suspending agent is one or more of ethylene glycol, propylene glycol and glycerol; the dispersing agent is one or more of polyethylene glycol, tween-80, polyvinylpyrrolidone, sodium alginate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
As a further improvement of the invention, the mass volume ratio of the nano peroxide to the deionized water containing the suspending agent is 1: 50-1: 900, the mass ratio of the dispersing agent to the nano peroxide is 1: 1-1: 15; the mass volume ratio of the suspending agent to the deionized water in the deionized water containing the suspending agent is 5-10%.
In a preferred embodiment, the environment-friendly slow-release antibacterial disinfection emulsion can be used in combination with a compound antibacterial agent, the compound antibacterial agent is at least one of magnesium oxide, titanium dioxide, hydrogen peroxide or ethanol, and the addition ratio of the compound antibacterial agent is 0-20%.
According to a third aspect of the present invention, there is provided an environmentally friendly slow-release antibacterial disinfectant emulsion, which is prepared from raw materials including nano peroxide with a surface rich in hydroxyl groups, suspending agent containing polyhydroxy group, deionized water and dispersing agent; wherein the content of the first and second substances,
the nano peroxide is one or more of magnesium peroxide, calcium peroxide and zinc peroxide; the suspending agent containing polyhydroxy is one or more of ethylene glycol, propylene glycol and glycerol; the dispersing agent is one or more of polyethylene glycol, tween-80, polyvinylpyrrolidone, sodium alginate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate; and the number of the first and second electrodes,
the mass volume ratio of the nano peroxide to the deionized water containing the suspending agent is 1: 50-1: 900, the mass of the dispersing agent and the nano peroxide is 1: 1-1: 15; the mass volume ratio of the suspending agent to the deionized water in the deionized water containing the suspending agent is 5-10%.
In a preferred embodiment, the environment-friendly slow-release antibacterial disinfection emulsion can be used in combination with a compound antibacterial agent, the compound antibacterial agent is at least one of magnesium oxide, titanium dioxide, hydrogen peroxide or ethanol, and the addition ratio of the compound antibacterial agent is 0-20%.
Generally, compared with the prior art, the above technical solution conceived by the present invention has the following beneficial effects:
(1) the preparation method of the environment-friendly slow-release antibacterial disinfection emulsion takes the nano metal peroxide as the main antibacterial active ingredient, has high stability and slow release property, and has little stimulation and harm to human body; the surface of the nano metal peroxide adopted by the invention is rich in hydroxyl, and the nano metal peroxide is added into a dispersing agent and a suspending agent containing polyhydroxy, so that the nano peroxide rich in hydroxyl on the surface can be uniformly and stably suspended in the dispersing agent and the suspending agent, and the antibacterial effect can be sustained. The antibacterial emulsion disclosed by the invention is simple in preparation process condition, environment-friendly, strong in practicability, excellent in antibacterial effect and long-lasting in antibacterial action.
(2) The environment-friendly slow-release antibacterial disinfection emulsion does not contain inflammable high-concentration alcohol and toxic chloride ions, and has the characteristics of small irritation to human bodies and environment friendliness; after being compounded with other antibacterial agents, the nano peroxide can stabilize the performance, thereby greatly reducing the addition of other antibacterial agents, having good effect and being capable of obtaining wider application range and better antibacterial performance.
Drawings
FIG. 1 is a schematic diagram illustrating the interparticle force effect of the nano-peroxide-rich particles in the environmentally-friendly slow-release antibacterial disinfecting emulsion according to the embodiment of the present invention;
FIG. 2 is an XRD representation of the nano-sized magnesium peroxide prepared in example 1 of the present invention;
FIG. 3 is a SEM representation of the nano-sized magnesium peroxide prepared in example 1 of the present invention;
FIG. 4 is a comparison of the antibacterial disinfectant emulsion prepared by using the nano magnesium peroxide of the present invention and the antibacterial disinfectant prepared by using the commercial magnesium peroxide of the comparative example.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The preparation method of the environment-friendly slow-release antibacterial disinfection emulsion provided by the invention specifically comprises the following steps:
(1) preparing nano peroxide;
dissolving metal salt in deionized water, adding a precipitator, uniformly stirring, adding hydrogen peroxide for peroxidation, and washing and filtering to obtain nano peroxide with a surface rich in hydroxyl after the reaction is finished;
(2) adding a proper amount of the nano peroxide rich in hydroxyl on the surface prepared in the step (1) into deionized water containing a suspending agent, wherein the suspending agent is a suspending agent containing polyhydroxy; adding a proper amount of dispersant to ensure that the nano peroxide with rich hydroxyl on the surface is evenly and stably suspended in the solvent to obtain the antibacterial disinfection emulsion;
in a preferred embodiment, the nanoperoxide is one or more of magnesium peroxide, calcium peroxide and zinc peroxide, but is not limited thereto, and is not limited to the specific raw material used in the embodiment.
In the step (1), the metal salt is one or more of nitrate, chloride, acetate or sulfate containing calcium, magnesium and zinc; the precipitator is one or more of ammonia water, sodium hydroxide or potassium hydroxide. But is not limited thereto and is more limited to the specific kind used in the examples. Specifically, the molar ratio of the metal salt to the precipitant is 1: 2-1: 4, the molar ratio of the metal salt to the hydrogen peroxide is 1: 1-1: 10.
in addition, in the step (1), a stirring device or other blending methods available in the prior art may be used, and the mixing may be performed at normal temperature and normal pressure, for example, magnetic stirring or ultrasonic mixing may be used, and the method is not particularly limited.
Further, in the step (2), the suspending agent is one or more of ethylene glycol, propylene glycol and glycerol; the dispersant is one or more of polyethylene glycol, tween-80, polyvinylpyrrolidone, sodium alginate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate. However, the kinds of the suspending agent and the dispersing agent are not limited thereto, and are more limited to the specific kinds used in the examples.
Further, the mass volume ratio of the nano peroxide to the deionized water containing the suspending agent is 1: 50-1: 900, the mass ratio of the dispersing agent to the nano peroxide is 1: 1-1: 15; the proportion of the suspending agent in the deionized water containing the suspending agent is 5-10% (mass volume ratio).
Because the dispersant is mainly organic matter, excessive dispersant is added in the preparation process, which can cause the problems of flocculation, aggregation and precipitation of products, even colloid formation and the like, thereby leading the fluidity of the nanometer peroxide particle suspension to be poor; in addition, too much dispersant may cause problems such as increased product cost, flammability of the product, and the like. When the addition ratio of the dispersant is too low, the nano peroxide particles cannot be uniformly suspended in the solvent due to the addition of too little dispersant, and upper and lower layers may be formed after long-term storage.
In addition, the antibacterial and disinfectant emulsion prepared by the method can be compounded with other antibacterial agents. In some embodiments, the compound antibacterial agent is continuously added into the antibacterial and disinfectant emulsion prepared in step (2), the compound antibacterial agent is preferably an inorganic or organic antibacterial agent such as magnesium oxide, titanium dioxide, hydrogen peroxide or ethanol, and the addition ratio of the compound antibacterial agent is 0-20%. In the prior art, more than 65% of ethanol is generally added for compounding, but the compound antibacterial agent prepared by the preparation method disclosed by the invention has the use amount of less than 20% and can effectively reduce the addition amount of other antibacterial agents.
In the step (1), the nano peroxide is only washed and filtered, and a drying process is not needed, so that the nano peroxide adopted by the invention is a wet product. As shown in the figure 1, the principle diagram of the action of particles rich in nano-peroxide shows that the surface of a wet product of nano-magnesium peroxide is rich in OH — On the one hand, agglomeration of the nanoparticles can be prevented; on the other hand, the dispersion in the water phase is uniform; furthermore, the suspending agent adopted by the invention is a suspending agent containing polyhydroxy group, and the interaction between the nano peroxide rich in hydroxyl group and the suspending agent containing polyhydroxy group can further ensure that the nano peroxide is uniformly and stably suspended in the solvent.
The commercial (nano) magnesium peroxide powder has OH on the surface due to drying treatment — Greatly reduces and even generates particle agglomeration, is not beneficial to uniform dispersion in solution, and the antibacterial disinfectant prepared by adopting commercial nano peroxide can cause serious emulsion aggregation and precipitation, thereby affecting the performance of products.
In addition, the nano magnesium peroxide prepared by the invention is a solid material, and is more stable than other liquid antibacterial components such as volatile ethanol or easily-decomposed hydrogen peroxide, so that the solid nano magnesium peroxide particles can be fully contacted with water after meeting water, thereby effectively and slowly releasing active oxygen species and playing a role in continuous and long-term sterilization and disinfection. The active oxygen species is a substance with stronger activity generated by oxygen in the process of electron transfer, has stronger oxidability and can effectively kill bacteria.
To better illustrate the product and method of preparation of the present invention, the following specific examples are provided:
example 1
(1) Preparing nano magnesium peroxide;
15.6g Mg (NO) are weighed out 3 ) 2 ·6H 2 Dissolving O in 70mL of deionized water, adding 18mL of ammonia water (25-28 wt%), stirring for reaction for 30min, adding 50mL of hydrogen peroxide (30 wt%), continuously stirring for reaction for 1h, separating and washing the mixed solution to obtain nano peroxideMagnesium.
(2) Weighing 2g of prepared nano magnesium peroxide, adding the nano magnesium peroxide into 100mL of deionized water containing 10g of glycerol, then adding 0.2g of polyvinylpyrrolidone, stirring, and uniformly dispersing by ultrasonic to obtain the magnesium peroxide emulsion.
The antibacterial disinfection emulsion of the embodiment is tested according to the disinfection technical specification (2.1.3) standard, and the disinfection effect on air is 1m 3 Spraying 10mL of emulsion in the experimental cabin, and detecting that the killing rate of the staphylococcus albus is more than 99% after 1h of action; the 1h inactivation rate of the antibacterial disinfection emulsion of the embodiment on poliovirus is detected to be more than 50% according to the disinfection technical specification (2.1.1.10);
and after standing, the emulsion is uniformly dispersed without layering.
Example 2
(1) Preparing nano magnesium peroxide; the preparation procedure is the same as in example 1;
(2) adding 0.2g of prepared nano magnesium peroxide into 180mL of deionized water containing 5g of ethylene glycol and 5g of glycerol, then adding 0.04g of sodium alginate, 0.06g of tween-80 and 0.1g of polyvinylpyrrolidone, stirring, ultrasonically dispersing uniformly, adding 20mL of hydrogen peroxide, and mixing to obtain the magnesium peroxide-hydrogen peroxide compound antibacterial emulsion.
The sterilization effect of the antibacterial sterilization emulsion of the embodiment on escherichia coli is detected according to the sterilization technical specification (2.1.1), and the detection sterilization rate reaches more than 99% after 1 h;
and after standing, the emulsion is uniformly dispersed without layering.
Example 3
(1) Preparing nano magnesium peroxide; the preparation procedure is the same as example 1;
(2) adding 2g of prepared nano magnesium peroxide into 160mL of deionized water containing 2g of ethylene glycol, 2g of propylene glycol and 8g of glycerol, then adding 0.05g of sodium dodecyl sulfate, 0.05g of sodium dodecyl benzene sulfonate and 0.2g of polyvinylpyrrolidone, stirring, ultrasonically dispersing uniformly, adding 40mL of absolute ethyl alcohol, and mixing to obtain the magnesium peroxide-ethanol compound antibacterial emulsion.
The sterilization effect of the antibacterial sterilization emulsion of the embodiment on escherichia coli is detected according to the sterilization technical specification (2.1.1), and the detection sterilization rate reaches more than 99% after 1 h;
and after standing, the emulsion is uniformly dispersed without layering.
Example 4
(1) Preparing nano magnesium peroxide;
15.6g Mg (NO) are weighed out 3 ) 2 ·6H 2 Dissolving O in 70mL of deionized water, adding 13.5mL of ammonia water (25-28 wt%), stirring for reaction for 30min, adding 31mL of hydrogen peroxide (30 wt%), continuing stirring for reaction for 1h, and separating and washing the mixed solution to obtain the nano magnesium peroxide.
(2) 1.5g of prepared nano magnesium peroxide is weighed and added into 750mL of deionized water containing 45g of glycerol, and then 0.1g of polyvinylpyrrolidone is added, stirred and uniformly dispersed by ultrasonic waves to obtain the magnesium peroxide emulsion.
The sterilization effect of the antibacterial sterilization emulsion of the embodiment on escherichia coli is detected according to the sterilization technical specification (2.1.1), and the detection sterilization rate reaches more than 99% after 1 h;
and after standing, the emulsion is uniformly dispersed without layering.
Example 5
(1) Preparing nano magnesium peroxide;
15.6g Mg (NO) are weighed out 3 ) 2 ·6H 2 Dissolving O in 70mL of deionized water, adding 13.5mL of ammonia water (25-28 wt%), stirring for reaction for 30min, adding 62mL of hydrogen peroxide (30 wt%), continuing stirring for reaction for 1h, and separating and washing the mixed solution to obtain the nano magnesium peroxide.
(2) Weighing 1g of prepared nano magnesium peroxide, adding the nano magnesium peroxide into 100mL of deionized water containing 8g of glycerol, then adding 0.2g of polyvinylpyrrolidone, stirring, and uniformly dispersing by ultrasonic to obtain the magnesium peroxide emulsion.
The sterilization effect of the antibacterial sterilization emulsion of the embodiment on escherichia coli is detected according to the sterilization technical specification (2.1.1), and the detection sterilization rate reaches more than 99% after 1 h;
and after standing, the emulsion is uniformly dispersed without layering.
Example 6
(1) Preparing nano calcium peroxide;
weighing 10g Ca (NO) 3 ) 2 ·4H 2 And O, dissolving in 70mL of deionized water, adding 11mL of 8M sodium hydroxide solution, stirring for reaction for 30min, adding 6mL of hydrogen peroxide, continuously stirring for reaction for 5h, and separating and washing the mixed solution to obtain the nano calcium peroxide.
(2) 0.5g of prepared nano calcium peroxide is weighed and added into 30mL of deionized water containing 2g of glycerol and 1g of glycol, then 0.1g of polyvinylpyrrolidone is added, and the mixture is stirred and ultrasonically dispersed uniformly to obtain calcium peroxide emulsion.
The sterilization effect of the antibacterial sterilization emulsion of the embodiment on escherichia coli is detected according to the sterilization technical specification (2.1.1), and the detection sterilization rate reaches more than 99% after 4 hours of action;
and after standing, the emulsion is uniformly dispersed without layering.
Example 7
(1) Preparing nano zinc peroxide;
weighing 12g Zn (NO) 3 ) 2 ·6H 2 And dissolving O in 70mL of deionized water, adding 6.4mL of ammonia water, stirring for reaction for 30min, adding 6mL of hydrogen peroxide, continuing stirring for reaction for 4h, and separating and washing the mixed solution to obtain the nano zinc peroxide.
(2) Weighing 2g of prepared nano zinc peroxide, 1g of magnesium oxide and 1g of titanium dioxide (P25), adding into 100mL of deionized water containing 10g of glycerol, then adding 0.3g of polyvinylpyrrolidone, stirring, and ultrasonically dispersing uniformly to obtain the zinc peroxide-magnesium oxide-titanium dioxide compound antibacterial emulsion.
After the visible light is irradiated for 30min, the killing effect of the antibacterial and disinfectant emulsion of the embodiment on escherichia coli is detected according to the disinfection technical specification (2.1.1) standard, and the killing rate on the escherichia coli reaches more than 99%;
and after standing, the emulsion is uniformly dispersed without layering.
Example 8
2g of the nano magnesium peroxide prepared in the embodiment 1 and 1g of the nano zinc peroxide prepared in the embodiment 7 are added into 180mL of deionized water containing 3g of propylene glycol and 7g of glycerol, then 0.2g of polyvinylpyrrolidone is added, after stirring and ultrasonic dispersion, 20mL of absolute ethyl alcohol is added, and the magnesium peroxide-zinc peroxide-ethyl alcohol compound antibacterial emulsion is obtained after mixing.
The killing effect of the compound on escherichia coli is detected according to the disinfection technical specification (2.1.1), and the killing rate is over 99 percent after 1 hour of action;
and after standing, the emulsion is uniformly dispersed without layering.
Example 9
And (3) taking 1g of the nano magnesium peroxide prepared in the example 1, 1g of the nano zinc peroxide prepared in the example 7 and 1g of the nano calcium peroxide prepared in the example 6, adding the obtained mixture into 600mL of deionized water containing 12g of propylene glycol and 36g of glycerol, then adding 0.2g of polyvinylpyrrolidone, stirring and ultrasonically dispersing the mixture uniformly to obtain the magnesium peroxide-zinc peroxide-calcium peroxide antibacterial emulsion.
The killing effect of the compound on escherichia coli is detected according to the disinfection technical specification (2.1.1), and the killing rate is over 99 percent after 1 hour of action;
and after standing, the emulsion has no layering phenomenon.
It should be noted that the metal salt used for preparing the nano metal peroxide particles is not limited to Mg (NO) in the above examples 3 ) 2 ·6H 2 O、Ca(NO 3 ) 2 ·4H 2 O、Zn(NO 3 ) 2 ·6H 2 Specific metal salts such as O, etc., and may be selected from other nitrates, chlorides, sulfates, acetates and their hydrates of magnesium, calcium and zinc.
Comparative example
Weighing 2g of commercial nano magnesium peroxide, adding the commercial nano magnesium peroxide into 100mL of deionized water containing 10g of glycerol, then adding 0.2g of polyvinylpyrrolidone, stirring, and performing ultrasonic dispersion to obtain a magnesium peroxide emulsion.
The air disinfection effect of the product is detected according to the disinfection technical specification (2.1.3) standard, and is 1m 3 Spraying 10mL of emulsion in the experimental cabin, and detecting that the killing rate of the emulsion on the white staphylococcus is less than 50% after 1 h;
and upon standing, the emulsion appeared to separate into layers.
In combination with the test results shown in the above examples, comparative examples and figures, the analysis was as follows:
FIG. 2 is an XRD representation of the nano-sized magnesium peroxide prepared in example 1 of the present invention; FIG. 3 is a SEM representation of the nano-sized magnesium peroxide prepared in example 1 of the present invention. As can be seen from FIG. 2, the XRD peak of the magnesium peroxide particles prepared by the present invention corresponds to that of the magnesium peroxide card JCPDS 01-076-1363; as can be seen from FIG. 3, the nano magnesium peroxide particles prepared by the embodiment of the invention are spheroidal nano particles with regular shapes and uniform particle sizes, and the particle sizes of the nano magnesium peroxide particles are about 30-70 nm. In the invention, the used nano peroxide particles are stable solid particles, and have higher stability compared with volatile organic or hydrogen peroxide antibacterial agents, so that active oxygen species can be continuously and slowly released after contacting water, thereby achieving the effect of slow-release and long-acting sterilization.
For the bactericidal effect of the antibacterial sterilizing emulsion prepared in each example and comparative example, it can be seen that: from examples 1-3, it can be seen that the antibacterial and disinfectant emulsions prepared by using the nano magnesium peroxide particles with rich hydroxyl groups on the surfaces have strong bactericidal effects, wherein the antibacterial emulsion compounded by magnesium peroxide and hydrogen peroxide is used in example 2, and the antibacterial emulsion compounded by magnesium peroxide and ethanol is used in example 3, the bactericidal effects of the antibacterial and disinfectant emulsions on escherichia coli are detected according to the standards of disinfection technical specifications (2.1.3), and the detected bactericidal rates after 1 hour of action are both more than 99%. It is known from examples 6 and 7 that the antibacterial and disinfectant emulsion prepared by using the nano calcium peroxide and the nano zinc peroxide with rich hydroxyl groups on the surface has stronger bactericidal effect, and the effect is slightly inferior to that of the nano magnesium peroxide antibacterial emulsion. Further, it is seen from example 7 that, in addition to adding a liquid-state complex antimicrobial agent (hydrogen peroxide, absolute ethyl alcohol, or the like), the antimicrobial agent can be also complex-formulated with a solid-state antimicrobial component, but the amount of the complex antimicrobial agent used is low. From example 8, it can be seen that the antibacterial and disinfectant emulsion prepared by using the hydroxyl-rich nano magnesium peroxide particles and the hydroxyl-rich nano zinc peroxide particles simultaneously or the three kinds of nano magnesium peroxide particles simultaneously (example 9) also has a strong bactericidal effect, indicating that the effect may achieve a certain additive effect after mixing.
In addition, as can be seen from the comparative example, the antibacterial and disinfectant emulsion prepared by using the commercial nano magnesium peroxide particles has poor bactericidal effect, and the bactericidal effect described in the embodiment of the present invention is difficult to achieve, and as shown in fig. 4 (the left side uses the commercial nano magnesium peroxide particles, and the right side uses the nano magnesium peroxide particles of the present invention), the antibacterial and disinfectant emulsion prepared by using the commercial nano magnesium peroxide particles has a layering phenomenon after standing, while the antibacterial and disinfectant emulsion of the present invention, the hydroxyl-rich nano peroxide is uniformly and stably suspended in the solvent, and the industrial nano magnesium peroxide particles cannot achieve the stable dispersion effect of the present invention. Further indicates that the antibacterial disinfection emulsion prepared by the nano peroxide particles with rich hydroxyl on the surface is a product with excellent antibacterial performance, mildness and long lasting effect.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (4)

1. The preparation method of the environment-friendly slow-release antibacterial disinfection emulsion is characterized by comprising the following steps:
s1: preparing nano peroxide;
dissolving metal salt in deionized water, adding a precipitator, uniformly stirring, adding hydrogen peroxide for peroxidation, and washing and filtering to obtain nano peroxide with a surface rich in hydroxyl after the reaction is finished; the metal salt is one or more of nitrate, chloride, acetate or sulfate containing calcium, magnesium and zinc; the precipitator is ammonia water, sodium hydroxide or potassium hydroxide;
s2: adding a proper amount of the nano peroxide which is prepared in the step S1 and has rich hydroxyl on the surface into deionized water containing a suspending agent, wherein the suspending agent is a suspending agent containing polyhydroxy; adding a proper amount of dispersant to enable the nano peroxide with rich hydroxyl on the surface to be evenly and stably suspended in the solvent to obtain the antibacterial disinfection emulsion; the suspending agent is one or more of ethylene glycol, propylene glycol and glycerol; the dispersing agent is one or more of polyethylene glycol, tween-80, polyvinylpyrrolidone, sodium alginate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate;
the nano peroxide is one or more of magnesium peroxide, calcium peroxide and zinc peroxide;
the mass volume ratio of the suspending agent to the deionized water in the deionized water containing the suspending agent is 5-10 percent; the mass volume ratio of the nano peroxide to the deionized water containing the suspending agent is 1: 50-1: 900, the mass ratio of the dispersing agent to the nano peroxide is 1: 1-1: 15.
2. the method for preparing an environmentally friendly sustained-release antibacterial disinfectant emulsion according to claim 1, wherein in step S1, the molar ratio of the metal salt to the precipitant is 1: 2-1: 4, the molar ratio of the metal salt to the hydrogen peroxide is 1: 1-1: 10.
3. the preparation method of the environment-friendly slow-release antibacterial and disinfectant emulsion according to claim 1 or 2, wherein a compound antibacterial agent is continuously added to the antibacterial and disinfectant emulsion prepared in step S2, wherein the compound antibacterial agent is at least one of magnesium oxide, titanium dioxide, hydrogen peroxide or ethanol, and the addition ratio of the compound antibacterial agent is 0-20%.
4. An environment-friendly slow-release antibacterial disinfection emulsion is characterized in that the antibacterial disinfection emulsion is prepared by mixing nano peroxide, deionized water containing polyhydroxy suspending agent and dispersing agent; wherein the content of the first and second substances,
the nano peroxide is obtained by dissolving metal salt in deionized water, adding a precipitator, uniformly stirring, adding hydrogen peroxide for peroxidation, and washing and filtering after the reaction is finished to obtain the nano peroxide with the surface rich in hydroxyl; the metal salt is one or more of nitrate, chloride, acetate or sulfate containing calcium, magnesium and zinc; the precipitator is ammonia water, sodium hydroxide or potassium hydroxide;
the peroxide with the surface rich in hydroxyl groups is uniformly and stably suspended in the solvent by adding the peroxide into the deionized water containing the polyhydroxy suspending agent and adding the dispersing agent;
the nano peroxide is one or more of magnesium peroxide, calcium peroxide and zinc peroxide; the polyhydroxy suspending agent is one or more of ethylene glycol, propylene glycol and glycerol; the dispersing agent is one or more of polyethylene glycol, tween-80, polyvinylpyrrolidone, sodium alginate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate;
the mass volume ratio of the nano peroxide to the deionized water containing the suspending agent is 1: 50-1: 900, the mass of the dispersing agent and the nano peroxide is 1: 1-1: 15; the mass volume ratio of the suspending agent to the deionized water in the deionized water containing the suspending agent is 5-10%.
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