CN115226731B - Environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent and preparation method thereof - Google Patents
Environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent and preparation method thereof Download PDFInfo
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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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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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
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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
- A01N59/16—Heavy metals; Compounds thereof
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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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/12—Asteraceae or Compositae [Aster or Sunflower family], e.g. daisy, pyrethrum, artichoke, lettuce, sunflower, wormwood or tarragon
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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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/24—Lauraceae [Laurel family], e.g. laurel, avocado, sassafras, cinnamon or camphor
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P7/00—Arthropodicides
- A01P7/04—Insecticides
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; Derivatives thereof
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- 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 relates to the technical field of archival bacteriostasis, and in particular discloses an environment-friendly slow-release archival antiseptic insect-resistant bacteriostat, which comprises the following raw materials in parts by weight: 45-55 parts of compound antibacterial additive, 2-5 parts of litsea cubeba oil, 3-6 parts of chitosan, 5-10 parts of bentonite regulating modifier, 1-5 parts of sodium alginate and 2-5 parts of gelatin. The bentonite regulating modifier and the compound antibacterial additive can form a synergistic effect, enhance the performance of the product, and simultaneously cooperate with chitosan and sodium alginate to further promote the effects of corrosion resistance, antibacterial and insect prevention of the product.
Description
Technical Field
The invention relates to the technical field of bacteriostats, in particular to an environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostat and a preparation method thereof.
Background
The archives record not only the actual passage of historical activities, but also the development of ideas of people in various activities, experience training in social practice, and creation results of scientific research and cultural arts. Therefore, the method has important reference function for people to examine the past situation, master the history materials, research the development rule of related things, summarize experience and absorb teaching and training. The archives need to be preserved by applying a bacteriostatic agent thereto.
The existing bacteriostatic agent has poor bacteriostatic efficiency, can not perform long-term bacteriostasis, has common anti-corrosion and insect-proof effects, and is further improved based on the conventional bacteriostatic agent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an environment-friendly and slow-release archival anti-corrosion insect-resistant bacteriostatic agent and a preparation method thereof, so as to solve the problems in the background art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides an environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent, which comprises the following raw materials in parts by weight:
45-55 parts of compound antibacterial additive, 2-5 parts of litsea cubeba oil, 3-6 parts of chitosan, 5-10 parts of bentonite regulating modifier, 1-5 parts of sodium alginate and 2-5 parts of gelatin.
Preferably, the bacteriostat comprises the following raw materials in parts by weight:
50 parts of compound antibacterial additive, 3.5 parts of litsea cubeba oil, 4.5 parts of chitosan, 7.5 parts of bentonite regulating modifier, 3 parts of sodium alginate and 3.5 parts of gelatin.
Preferably, the preparation method of the compound antibacterial additive comprises the following steps:
s01: preparation of modified nano zinc oxide:
a. adding 5-10 parts of hydrochloric acid into 10-15 parts of ethanol solvent, then adding 1-5 parts of n-octyl triethoxysilane and 2-4 parts of lanthanum sulfate, stirring and mixing thoroughly, and then adding 5-9 parts of carbon nanotubes to obtain a carbon nanotube agent;
b. stirring the nano zinc oxide and the nano tube agent according to the weight ratio of 1:5 for reaction, then adding hexadecyl trimethyl ammonium bromide accounting for 10-15% of the total amount of the nano zinc oxide, and continuously stirring and uniformly mixing to obtain modified nano zinc oxide;
s02: adding 3-6 parts of pyrethrum extract into 5-9 parts of modified nano zinc oxide, then adding 6-10 parts of beta-cyclodextrin additive, stirring and mixing thoroughly, then spraying under high pressure, and collecting to obtain the compound antibacterial additive.
Preferably, the preparation method of the pyrethrum extract comprises the following steps: pulverizing herba et flos Pyrethri Cinerariifolii, dispersing in 3-5 times ethanol solvent, washing with water, drying, boiling in 6-10 times water for 20-30min, treating with slow fire for 1-2 hr, filtering, and mixing filtrates to obtain herba et flos Pyrethri Cinerariifolii extractive solution.
Preferably, the temperature of the stirring reaction in the step b is 55-65 ℃, the stirring time is 30-40min, and the stirring rotating speed is 500-1000r/min.
Preferably, the specific preparation steps of the beta-cyclodextrin additive are as follows:
mixing 5-10 parts of Span-80 with 3-6 parts of kerosene to obtain an oil phase; the oil phase is firstly added into a magnetic stirrer, the temperature is raised to 60-65 ℃, then 6-12 parts of beta-cyclodextrin aqueous solution is added, the stirring speed is raised to 300-500r/min, the stirring is carried out for 35-45min, then 1-3 parts of potassium peroxide and 0.3-0.6 part of N-methylolacrylamide are added, the stirring is continued for 18-24h, then absolute ethyl alcohol is added for demulsification, and finally absolute ethyl alcohol is used for leaching and drying, thus obtaining the beta-cyclodextrin additive.
Preferably, the beta-cyclodextrin aqueous solution is prepared from beta-cyclodextrin, sodium alginate and deionized water according to a weight ratio of 3:2:5.
Preferably, the preparation method of the bentonite regulating modifier comprises the following steps:
s11: calcining bentonite at 500-550 ℃ for 1-2h, cooling to room temperature, uniformly dispersing in 3-5 times deionized water, washing, filtering and drying to obtain dispersed bentonite;
s12: 1-2 parts of tartaric acid is added into 5-7 parts of sodium dodecyl benzene sulfonate aqueous solution with the mass fraction of 5-10%, then 2-4 parts of silane coupling agent KH560 is added, and the mixture is stirred and mixed fully to obtain modified liquid;
s13: adding the dispersed bentonite into 2-3 times of the modifying liquid, then oscillating in an oscillator, and washing and drying after the treatment is finished to obtain the bentonite regulating modifier.
Preferably, the power of the oscillation treatment is 100-200W, and the treatment time is 20-30min.
The invention also provides a preparation method of the environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent, which comprises the following steps:
step one: weighing a compound antibacterial additive, litsea cubeba oil, chitosan, bentonite regulating modifier, sodium alginate and gelatin raw materials;
step two: uniformly stirring the compound antibacterial additive and the bentonite regulating modifier, adding the mixture into a ball milling tank, and ball milling at a rotating speed of 1000-1500r/min for 10-20min to obtain a ball grinding material;
step three: uniformly mixing litsea cubeba oil, chitosan and sodium alginate to obtain an input material;
step four: the ball grinding material, the input material and the gelatin are uniformly mixed to obtain the bacteriostatic agent.
Compared with the prior art, the invention has the following beneficial effects:
the antibacterial agent is prepared by adopting a compound antibacterial additive and raw materials such as chitosan, litsea cubeba oil, sodium alginate, bentonite regulating modifier and the like, wherein the compound antibacterial additive is prepared by adopting pyrethrum extract and modified nano zinc oxide to be subjected to synergistic modification by a beta-cyclodextrin additive, the extract prepared by pyrethrum extract through pyrethrum extraction has high-efficiency deinsectization efficiency, the modified nano zinc oxide is loaded by a carbon nano tube after being subjected to synergistic modification by nano zinc oxide, cetyltrimethylammonium bromide and a carbon nano tube, and the beta-cyclodextrin additive is prepared by demulsifying an oil phase and a cyclodextrin water phase, so that the nano zinc oxide can be coated, long-acting slow release effect is realized, and long-acting antibacterial and insect-preventing efficiency is achieved; the bentonite regulating modifier has high activity and dispersivity after the bentonite is calcined and dispersed, the tartaric acid, the bentonite regulating modifier and the silane coupling agent are matched with the modified bentonite, the lamellar interlayer spacing structure of the bentonite is inserted in the raw materials of the product, the activity is improved after modification, the antibacterial and antiseptic effects of the product are further regulated, the bentonite regulating modifier and the compound antibacterial additive can form a synergistic effect, the performance of the product is enhanced, and meanwhile, the chitosan and the sodium alginate are matched, so that the antiseptic, antibacterial and insect-preventing effects of the product are further promoted.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following raw materials in parts by weight:
45-55 parts of compound antibacterial additive, 2-5 parts of litsea cubeba oil, 3-6 parts of chitosan, 5-10 parts of bentonite regulating modifier, 1-5 parts of sodium alginate and 2-5 parts of gelatin.
The bacteriostat of the embodiment comprises the following raw materials in parts by weight:
50 parts of compound antibacterial additive, 3.5 parts of litsea cubeba oil, 4.5 parts of chitosan, 7.5 parts of bentonite regulating modifier, 3 parts of sodium alginate and 3.5 parts of gelatin.
The preparation method of the compound antibacterial additive of the embodiment comprises the following steps:
s01: preparation of modified nano zinc oxide:
a. adding 5-10 parts of hydrochloric acid into 10-15 parts of ethanol solvent, then adding 1-5 parts of n-octyl triethoxysilane and 2-4 parts of lanthanum sulfate, stirring and mixing thoroughly, and then adding 5-9 parts of carbon nanotubes to obtain a carbon nanotube agent;
b. stirring the nano zinc oxide and the nano tube agent according to the weight ratio of 1:5 for reaction, then adding hexadecyl trimethyl ammonium bromide accounting for 10-15% of the total amount of the nano zinc oxide, and continuously stirring and uniformly mixing to obtain modified nano zinc oxide;
s02: adding 3-6 parts of pyrethrum extract into 5-9 parts of modified nano zinc oxide, then adding 6-10 parts of beta-cyclodextrin additive, stirring and mixing thoroughly, then spraying under high pressure, and collecting to obtain the compound antibacterial additive.
The preparation method of the pyrethrum extract in the embodiment comprises the following steps: pulverizing herba et flos Pyrethri Cinerariifolii, dispersing in 3-5 times ethanol solvent, washing with water, drying, boiling in 6-10 times water for 20-30min, treating with slow fire for 1-2 hr, filtering, and mixing filtrates to obtain herba et flos Pyrethri Cinerariifolii extractive solution.
In the embodiment b, the temperature of the stirring reaction is 55-65 ℃, the stirring time is 30-40min, and the stirring rotating speed is 500-1000r/min.
The specific preparation steps of the beta-cyclodextrin additive of the embodiment are as follows:
mixing 5-10 parts of Span-80 with 3-6 parts of kerosene to obtain an oil phase; the oil phase is firstly added into a magnetic stirrer, the temperature is raised to 60-65 ℃, then 6-12 parts of beta-cyclodextrin aqueous solution is added, the stirring speed is raised to 300-500r/min, the stirring is carried out for 35-45min, then 1-3 parts of potassium peroxide and 0.3-0.6 part of N-methylolacrylamide are added, the stirring is continued for 18-24h, then absolute ethyl alcohol is added for demulsification, and finally absolute ethyl alcohol is used for leaching and drying, thus obtaining the beta-cyclodextrin additive.
The beta-cyclodextrin aqueous solution of the embodiment is prepared from beta-cyclodextrin, sodium alginate and deionized water according to a weight ratio of 3:2:5.
The preparation method of the bentonite regulating modifier of the embodiment comprises the following steps:
s11: calcining bentonite at 500-550 ℃ for 1-2h, cooling to room temperature, uniformly dispersing in 3-5 times deionized water, washing, filtering and drying to obtain dispersed bentonite;
s12: 1-2 parts of tartaric acid is added into 5-7 parts of sodium dodecyl benzene sulfonate aqueous solution with the mass fraction of 5-10%, then 2-4 parts of silane coupling agent KH560 is added, and the mixture is stirred and mixed fully to obtain modified liquid;
s13: adding the dispersed bentonite into 2-3 times of the modifying liquid, then oscillating in an oscillator, and washing and drying after the treatment is finished to obtain the bentonite regulating modifier.
The power of the oscillation treatment in this embodiment is 100-200W and the treatment time is 20-30min.
The preparation method of the environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following steps:
step one: weighing a compound antibacterial additive, litsea cubeba oil, chitosan, bentonite regulating modifier, sodium alginate and gelatin raw materials:
step two: uniformly stirring the compound antibacterial additive and the bentonite regulating modifier, adding the mixture into a ball milling tank, and ball milling at a rotating speed of 1000-1500r/min for 10-20min to obtain a ball grinding material;
step three: uniformly mixing litsea cubeba oil, chitosan and sodium alginate to obtain an input material;
step four: the ball grinding material, the input material and the gelatin are uniformly mixed to obtain the bacteriostatic agent.
Example 1.
The environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following raw materials in parts by weight:
45 parts of compound antibacterial additive, 2 parts of litsea cubeba oil, 3 parts of chitosan, 5 parts of bentonite regulating modifier, 1 part of sodium alginate and 2 parts of gelatin.
The preparation method of the compound antibacterial additive of the embodiment comprises the following steps:
s01: preparation of modified nano zinc oxide:
a. adding 5 parts of hydrochloric acid into 10 parts of ethanol solvent, then adding 1 part of n-octyl triethoxysilane and 2-parts of lanthanum sulfate, stirring and mixing thoroughly, and then adding 5 parts of carbon nanotubes to obtain a carbon nanotube agent;
b. stirring the nano zinc oxide and the nano tube agent according to the weight ratio of 1:5 for reaction, then adding cetyltrimethylammonium bromide accounting for 10% of the total amount of the nano zinc oxide, and continuously stirring and uniformly mixing to obtain modified nano zinc oxide;
s02: adding 3 parts of pyrethrum extract into 5 parts of modified nano zinc oxide, then adding 6 parts of beta-cyclodextrin additive, stirring and mixing fully, then spraying under high pressure, and collecting to obtain the compound antibacterial additive.
The preparation method of the pyrethrum extract in the embodiment comprises the following steps: pulverizing herba et flos Pyrethri Cinerariifolii, dispersing in 3 times ethanol solvent, washing with water, drying, boiling in 6 times water for 20min, treating with slow fire for 1 hr, filtering, and mixing filtrates to obtain herba et flos Pyrethri Cinerariifolii extractive solution.
In example b, the temperature of the stirring reaction was 55℃and the stirring time was 30min, and the stirring speed was 500r/min.
The specific preparation steps of the beta-cyclodextrin additive of the embodiment are as follows:
mixing 5 parts of Span-80 with 3 parts of kerosene to obtain an oil phase; the oil phase is firstly added into a magnetic stirrer, the temperature is raised to 60 ℃, then 6 parts of beta-cyclodextrin aqueous solution is added, the stirring speed is raised to 300r/min, the stirring is carried out for 35min, then 1 part of potassium peroxide and 0.3 part of N-methylolacrylamide are added, the stirring is continued for 18h, then absolute ethyl alcohol is added for demulsification, and finally the absolute ethyl alcohol is used for leaching and drying, thus obtaining the beta-cyclodextrin additive.
The beta-cyclodextrin aqueous solution of the embodiment is prepared from beta-cyclodextrin, sodium alginate and deionized water according to a weight ratio of 3:2:5.
The preparation method of the bentonite regulating modifier of the embodiment comprises the following steps:
s11: calcining bentonite at 500 ℃ for 1h, cooling to room temperature, uniformly dispersing in 3 times of deionized water, washing with water, filtering, and drying to obtain dispersed bentonite;
s12: 1 part of tartaric acid is added into 5 parts of sodium dodecyl benzene sulfonate aqueous solution with the mass fraction of 5%, then 2 parts of silane coupling agent KH560 is added, and the mixture is stirred and mixed fully to obtain modified liquid;
s13: adding the dispersed bentonite into the 2 times of modifying liquid, then oscillating in an oscillator, and washing and drying after the treatment is finished to obtain the bentonite regulating modifier.
The power of the oscillation treatment in this example was 100W and the treatment time was 20min.
The preparation method of the environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following steps:
step one: weighing the raw materials:
step two: uniformly stirring the compound antibacterial additive and the bentonite regulating modifier, adding the mixture into a ball milling tank, and ball milling for 10min at a rotating speed of 1000r/min to obtain a ball grinding material;
step three: uniformly mixing litsea cubeba oil, chitosan and sodium alginate to obtain an input material;
step four: the ball grinding material, the input material and the gelatin are uniformly mixed to obtain the bacteriostatic agent.
Example 2.
The environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following raw materials in parts by weight:
55 parts of compound antibacterial additive, 5 parts of litsea cubeba oil, 6 parts of chitosan, 10 parts of bentonite regulating modifier, 5 parts of sodium alginate and 5 parts of gelatin.
The preparation method of the compound antibacterial additive of the embodiment comprises the following steps:
s01: preparation of modified nano zinc oxide:
a. adding 10 parts of hydrochloric acid into 15 parts of ethanol solvent, then adding 5 parts of n-octyl triethoxysilane and 4 parts of lanthanum sulfate, stirring and mixing thoroughly, and then adding 9 parts of carbon nanotubes to obtain a carbon nanotube agent;
b. stirring the nano zinc oxide and the nano tube agent according to the weight ratio of 1:5 for reaction, then adding cetyltrimethylammonium bromide accounting for 15% of the total amount of the nano zinc oxide, and continuously stirring and uniformly mixing to obtain modified nano zinc oxide;
s02: adding 6 parts of pyrethrum extract into 9 parts of modified nano zinc oxide, then adding 10 parts of beta-cyclodextrin additive, stirring and mixing thoroughly, then spraying under high pressure, and collecting to obtain the compound antibacterial additive.
The preparation method of the pyrethrum extract in the embodiment comprises the following steps: pulverizing herba et flos Pyrethri Cinerariifolii, dispersing in 5 times ethanol solvent, washing with water, drying, boiling in 10 times water for 30min, treating with slow fire for 2 hr, filtering, and mixing filtrates to obtain herba et flos Pyrethri Cinerariifolii extractive solution.
In example b, the temperature of the stirring reaction was 65℃and the stirring time was 40min, and the stirring speed was 1000r/min.
The specific preparation steps of the beta-cyclodextrin additive of the embodiment are as follows:
mixing 10 parts of Span-80 with 6 parts of kerosene to obtain an oil phase; the oil phase is firstly added into a magnetic stirrer, the temperature is raised to 65 ℃, then 12 parts of beta-cyclodextrin aqueous solution is added, the stirring speed is raised to 500r/min, the stirring is carried out for 45min, then 3 parts of potassium peroxide and 0.6 part of N-methylolacrylamide are added, the stirring is continued for 24h, then absolute ethyl alcohol is added for demulsification, and finally the absolute ethyl alcohol is used for leaching and drying, thus obtaining the beta-cyclodextrin additive.
The beta-cyclodextrin aqueous solution of the embodiment is prepared from beta-cyclodextrin, sodium alginate and deionized water according to a weight ratio of 3:2:5.
The preparation method of the bentonite regulating modifier of the embodiment comprises the following steps:
s11: calcining bentonite at 550 ℃ for 2 hours, cooling to room temperature, uniformly dispersing in 5 times of deionized water, washing with water, filtering, and drying to obtain dispersed bentonite;
s12: adding 2 parts of tartaric acid into 7 parts of 10% sodium dodecyl benzene sulfonate aqueous solution by mass fraction, then adding 4 parts of silane coupling agent KH560, and stirring and mixing thoroughly to obtain a modified liquid;
s13: adding the dispersed bentonite into 3 times of the modifying liquid, then oscillating in an oscillator, and washing and drying after the treatment is finished to obtain the bentonite regulating modifier.
The power of the oscillation treatment in this example was 200W and the treatment time was 30min.
The preparation method of the environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following steps:
step one: weighing the raw materials:
step two: uniformly stirring the compound antibacterial additive and the bentonite regulating modifier, adding the mixture into a ball milling tank, and ball milling for 20min at a rotating speed of 1500r/min to obtain a ball grinding material;
step three: uniformly mixing litsea cubeba oil, chitosan and sodium alginate to obtain an input material;
step four: the ball grinding material, the input material and the gelatin are uniformly mixed to obtain the bacteriostatic agent.
Example 3.
The environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following raw materials in parts by weight:
50 parts of compound antibacterial additive, 3.5 parts of litsea cubeba oil, 4.5 parts of chitosan, 7.5 parts of bentonite regulating modifier, 3 parts of sodium alginate and 3.5 parts of gelatin.
The preparation method of the compound antibacterial additive of the embodiment comprises the following steps:
s01: preparation of modified nano zinc oxide:
a. adding 7.5 parts of hydrochloric acid into 12.5 parts of ethanol solvent, then adding 3 parts of n-octyl triethoxysilane and 3 parts of lanthanum sulfate, stirring and mixing thoroughly, and then adding 7 parts of carbon nanotubes to obtain a carbon nanotube agent;
b. stirring the nano zinc oxide and the nano tube agent according to the weight ratio of 1:5 for reaction, then adding cetyl trimethyl ammonium bromide accounting for 12.5% of the total amount of the nano zinc oxide, and continuously stirring and uniformly mixing to obtain modified nano zinc oxide;
s02: adding 4.5 parts of pyrethrum extract into 7 parts of modified nano zinc oxide, then adding 8 parts of beta-cyclodextrin additive, stirring and mixing thoroughly, then spraying under high pressure, and collecting to obtain the compound antibacterial additive.
The preparation method of the pyrethrum extract in the embodiment comprises the following steps: pulverizing herba et flos Pyrethri Cinerariifolii, dispersing in 4 times ethanol solvent, washing with water, drying, boiling in 8 times water for 25min, treating with slow fire for 1.5 hr, filtering, and mixing filtrates to obtain herba et flos Pyrethri Cinerariifolii extractive solution.
In example b, the temperature of the stirring reaction was 60℃and the stirring time was 35min, and the stirring speed was 750r/min.
The specific preparation steps of the beta-cyclodextrin additive of the embodiment are as follows:
mixing 7.5 parts Span-80 with 4.5 parts kerosene to obtain an oil phase; the oil phase is firstly added into a magnetic stirrer, the temperature is raised to 62.5 ℃, then 9 parts of beta-cyclodextrin aqueous solution is added, the stirring speed is raised to 400r/min, the stirring is carried out for 40min, then 2 parts of potassium peroxide and 0.45 part of N-methylolacrylamide are added, the stirring is continued for 21h, then absolute ethyl alcohol is added for demulsification, and finally the absolute ethyl alcohol is used for leaching and drying, thus obtaining the beta-cyclodextrin additive.
The beta-cyclodextrin aqueous solution of the embodiment is prepared from beta-cyclodextrin, sodium alginate and deionized water according to a weight ratio of 3:2:5.
The preparation method of the bentonite regulating modifier of the embodiment comprises the following steps:
s11: calcining bentonite at 525 ℃ for 1.5 hours, cooling to room temperature, uniformly dispersing in 4 times deionized water, washing with water, filtering, and drying to obtain dispersed bentonite;
s12: 1.5 parts of tartaric acid is added into 6 parts of sodium dodecyl benzene sulfonate aqueous solution with the mass fraction of 7.5%, then 3 parts of silane coupling agent KH560 is added, and stirring and mixing are carried out fully, thus obtaining modified liquid;
s13: adding the dispersed bentonite into 2.5 times of the modifying liquid, then oscillating in an oscillator, and washing and drying after the treatment is finished to obtain the bentonite regulating modifier.
The power of the oscillation treatment in this example was 150W and the treatment time was 25min.
The preparation method of the environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent comprises the following steps:
step one: weighing the raw materials:
step two: uniformly stirring the compound antibacterial additive and the bentonite regulating modifier, adding the mixture into a ball milling tank, and ball milling for 15min at the rotating speed of 1250r/min to obtain a ball grinding material;
step three: uniformly mixing litsea cubeba oil, chitosan and sodium alginate to obtain an input material;
step four: the ball grinding material, the input material and the gelatin are uniformly mixed to obtain the bacteriostatic agent.
Comparative example 1.
The difference from example 3 is that no beta-cyclodextrin additive was added in the preparation of the formulated antimicrobial additive.
Comparative example 2.
The difference from example 3 is that no carbon nanotubes were added in the preparation of the compounded antibiotic additive.
Comparative example 3.
The difference from example 3 is that lanthanum sulfate was not added in the preparation of the carbon nanotube agent.
Comparative example 4.
The difference with the embodiment 3 is that the compound antibiotic additive is prepared by adopting pyrethrum extract and nano zinc oxide according to the weight ratio of 2:1.
Comparative example 5.
The difference from example 3 is that no bentonite conditioning modifier is added.
Comparative example 6.
The difference from example 3 is that bentonite conditioning modifiers are replaced with bentonite.
The results of the performance measurements of examples 1-3 and comparative examples 1-6 are as follows
From examples 1 to 3 and comparative examples 1 to 6,
the insecticidal rate of the embodiment 3 of the invention can realize long-acting and slow-releasing effects after 5 days to 5 months from the instant measurement; meanwhile, the number of black yeast colonies can be kept low for 48 hours, and the long-acting antibacterial effect is achieved; the product prepared by other methods can not realize the effects of slow release and long-acting;
as can be seen from comparative examples 1 to 6, the long-acting antibacterial and insect-preventing efficiency is deteriorated without adding the beta-cyclodextrin additive in the preparation of the compound antibacterial additive, the overall antibacterial and insect-preventing effect is deteriorated without adding the carbon nano tube, in addition, lanthanum sulfate is not added in the preparation of the carbon nano tube agent, the compound antibacterial additive is compounded by using pyrethrum extract and nano zinc oxide according to the weight ratio of 2:1, the performance of the product is deteriorated, the long-acting durability of the antibacterial and insect-preventing effect of the compound antibacterial additive prepared by the method is most obvious, and the effects of the invention are not realized by adopting other methods instead;
in addition, the product is not added with bentonite regulating modifier, the colony number of the black yeast is obviously deteriorated after 48 hours, meanwhile, the insecticidal rate is also greatly reduced after 5 months, and the addition of the bentonite regulating modifier can obviously improve the antibacterial and insect-preventing stability of the product and has important factors for realizing long-acting effect.
The invention further researches and researches the bentonite regulating modifier;
the preparation method of the bentonite regulating modifier comprises the following steps:
s11: calcining bentonite at 525 ℃ for 1.5 hours, cooling to room temperature, uniformly dispersing in 4 times deionized water, washing with water, filtering, and drying to obtain dispersed bentonite;
s12: 1.5 parts of tartaric acid is added into 6 parts of sodium dodecyl benzene sulfonate aqueous solution with the mass fraction of 7.5%, then 3 parts of silane coupling agent KH560 is added, and stirring and mixing are carried out fully, thus obtaining modified liquid;
s13: adding the dispersed bentonite into 2.5 times of the modifying liquid, then oscillating in an oscillator, and washing and drying after the treatment is finished to obtain the bentonite regulating modifier.
Experimental example 1:
the only difference from example 3 is that the bentonite has not been calcined.
Experimental example 2:
the only difference from example 3 is that the bentonite has not been treated with a modifying liquid.
Experimental example 3:
the only difference from example 3 is that no silane coupling agent KH560 was added in the preparation of the modified liquid.
Experimental example 4:
the only difference from example 3 is that tartaric acid was not added in the preparation of the modified liquid.
As can be seen from experimental examples 1 to 4,
the bentonite regulating modifier has the advantages that the bentonite regulating modifier is not treated by a modifying liquid, the performance change trend of the product is most obvious, the use of the modifying liquid has obvious change influence on the antibacterial long-acting stability, the silane coupling agent KH560 is not added and the tartaric acid is not added in the modifying liquid preparation method, the performance of the product is poor, through the research of experimental examples 1-4, the preparing methods of the modifying liquid are different, the performance effects of the product are different, and the bentonite regulating modifier prepared by the method has the most obvious antibacterial long-acting property.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (4)
1. An environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent is characterized by comprising the following raw materials in parts by weight:
45-55 parts of compound antibacterial additive, 2-5 parts of litsea cubeba oil, 3-6 parts of chitosan, 5-10 parts of bentonite regulating modifier, 1-5 parts of sodium alginate and 2-5 parts of gelatin;
the preparation method of the compound antibacterial additive comprises the following steps:
s01: preparation of modified nano zinc oxide:
a. adding 5-10 parts of hydrochloric acid into 10-15 parts of ethanol solvent, then adding 1-5 parts of n-octyl triethoxysilane and 2-4 parts of lanthanum sulfate, stirring and mixing thoroughly, and then adding 5-9 parts of carbon nanotubes to obtain a carbon nanotube agent;
b. stirring the nano zinc oxide and the nano tube agent according to the weight ratio of 1:5 for reaction, then adding hexadecyl trimethyl ammonium bromide accounting for 10-15% of the total amount of the nano zinc oxide, and continuously stirring and uniformly mixing to obtain modified nano zinc oxide; wherein the temperature of the stirring reaction is 55-65 ℃, the stirring time is 30-40min, and the stirring rotating speed is 500-1000r/min;
s02: adding 3-6 parts of pyrethrum extract into 5-9 parts of modified nano zinc oxide, then adding 6-10 parts of beta-cyclodextrin additive, stirring and mixing fully, then spraying under high pressure, and collecting to obtain a compound antibacterial additive;
the preparation method of the pyrethrum extract comprises the following steps: pulverizing herba et flos Pyrethri Cinerariifolii, dispersing in 3-5 times of ethanol solvent, washing with water, drying, boiling in 6-10 times of water for 20-30min, treating with slow fire for 1-2 hr, filtering, and mixing filtrates to obtain herba et flos Pyrethri Cinerariifolii extractive solution;
the specific preparation steps of the beta-cyclodextrin additive are as follows:
mixing 5-10 parts of Span-80 with 3-6 parts of kerosene to obtain an oil phase; adding the oil phase into a magnetic stirrer, heating to 60-65 ℃, then adding 6-12 parts of beta-cyclodextrin aqueous solution, stirring at a speed of 300-500r/min, stirring for 35-45min, then adding 1-3 parts of potassium peroxide and 0.3-0.6 part of N-methylolacrylamide, continuously stirring for 18-24h, then adding absolute ethyl alcohol for demulsification, and finally leaching and drying by absolute ethyl alcohol to obtain the beta-cyclodextrin additive; the beta-cyclodextrin aqueous solution is prepared from beta-cyclodextrin, sodium alginate and deionized water according to a weight ratio of 3:2:5;
the preparation method of the bentonite regulating modifier comprises the following steps:
s11: calcining bentonite at 500-550 ℃ for 1-2h, cooling to room temperature, uniformly dispersing in 3-5 times deionized water, washing, filtering and drying to obtain dispersed bentonite;
s12: 1-2 parts of tartaric acid is added into 5-7 parts of sodium dodecyl benzene sulfonate aqueous solution with the mass fraction of 5-10%, then 2-4 parts of silane coupling agent KH560 is added, and the mixture is stirred and mixed fully to obtain modified liquid;
s13: adding the dispersed bentonite into 2-3 times of the modifying liquid, then oscillating in an oscillator, and washing and drying after the treatment is finished to obtain the bentonite regulating modifier.
2. An environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent according to claim 1, which is characterized by comprising the following raw materials in parts by weight:
50 parts of compound antibacterial additive, 3.5 parts of litsea cubeba oil, 4.5 parts of chitosan, 7.5 parts of bentonite regulating modifier, 3 parts of sodium alginate and 3.5 parts of gelatin.
3. An environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent according to claim 1, which is characterized in that the power of the oscillation treatment is 100-200W and the treatment time is 20-30min.
4. A method for preparing the environment-friendly slow-release archival anti-corrosion insect-resistant bacteriostatic agent according to any one of claims 1-3, which is characterized by comprising the following steps:
step one: weighing a compound antibacterial additive, litsea cubeba oil, chitosan, bentonite regulating modifier, sodium alginate and gelatin raw materials:
step two: uniformly stirring the compound antibacterial additive and the bentonite regulating modifier, adding the mixture into a ball milling tank, and ball milling at a rotating speed of 1000-1500r/min for 10-20min to obtain a ball grinding material;
step three: uniformly mixing litsea cubeba oil, chitosan and sodium alginate to obtain an input material;
step four: and uniformly mixing the ball grinding material, the input material and the gelatin to obtain the bacteriostatic agent.
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