CN110916050A - Microcapsule efficient preservative and preparation method thereof - Google Patents

Microcapsule efficient preservative and preparation method thereof Download PDF

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Publication number
CN110916050A
CN110916050A CN201911192859.6A CN201911192859A CN110916050A CN 110916050 A CN110916050 A CN 110916050A CN 201911192859 A CN201911192859 A CN 201911192859A CN 110916050 A CN110916050 A CN 110916050A
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parts
microcapsule
preservative
efficiency
ester
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李骏
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Nanjing Haipai Enterprise Management Consulting Co Ltd
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Nanjing Haipai Enterprise Management Consulting Co Ltd
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3526—Organic compounds containing nitrogen
    • 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
    • A01N25/26—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 in coated particulate form
    • A01N25/28—Microcapsules or nanocapsules
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
    • A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
    • A01N37/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
    • 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
    • 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
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
    • 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
    • A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
    • A23L3/3517—Carboxylic acid esters
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives

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  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
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  • Pest Control & Pesticides (AREA)
  • Dentistry (AREA)
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  • Agronomy & Crop Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention discloses a microcapsule high-efficiency preservative and a preparation method thereof, wherein the microcapsule high-efficiency preservative comprises the following raw materials in parts by weight: 8-16 parts of fatty acid ester, 5-10 parts of nipagin ester, 10-20 parts of allantoin, 20-36 parts of antibacterial capsule wall component, 2-5 parts of thermosensitive agent, 3-7 parts of cosolvent and 106-152 parts of solvent. The microcapsule high-efficiency preservative adopts environment-friendly raw materials, has obvious effect, can ensure the preservative effect only by using 0.005-0.02 percent of the amount when in use, has no toxicity and little effective amount, thus having no influence on human health, has good preservative performance under different pH values when in use, and can be applied to the field of food due to wide application range of the microcapsule high-efficiency preservative on pH and temperature environmental factors.

Description

Microcapsule efficient preservative and preparation method thereof
Technical Field
The invention relates to the technical field of preservatives, and particularly relates to a microcapsule efficient preservative, a preparation method thereof and application thereof in food.
Background
The bactericidal preservative mainly ensures that the materials do not go bad in the using process by killing bacteria or losing the growth and reproduction capacity of the bacteria. The sterilization preservative has various types, and can be divided into an inorganic preservative and an organic preservative according to different structures.
The inorganic preservative has strong sterilizing capability, but has unstable chemical property, easy decomposition and non-lasting effect; the organic preservative has the characteristics of high efficiency, low toxicity, good biodegradability and the like, has obvious superiority in comparison, but has higher requirements on temperature, pH and the like, and is easy to lose effectiveness under the influence of environment.
The application range of the preservative is not only in the fields of food, cosmetics and the like, but also in the fields of papermaking, weaving, buildings and the like, and the change range of environmental factors such as temperature and the like is large, so that if the organic preservative has high temperature adaptability and even thermal responsiveness, the real-time preservative performance of the preservative can be quantitatively determined according to different use temperatures, and the problem to be solved in the field is urgently solved.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art preservatives.
Therefore, one of the objects of the present invention is to overcome the disadvantages of the existing preservative products and to provide a microcapsule high-efficiency preservative.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions: the microcapsule high-efficiency preservative comprises the following raw materials in parts by weight: 8-16 parts of fatty acid ester, 5-10 parts of nipagin ester, 10-20 parts of allantoin, 20-36 parts of antibacterial capsule wall component, 2-5 parts of thermosensitive agent, 3-7 parts of cosolvent and 106-152 parts of solvent.
As a preferable scheme of the microcapsule high-efficiency preservative, the microcapsule high-efficiency preservative comprises the following components in percentage by weight: the fatty acid ester is one or a combination of more than two of sucrose fatty acid monoester, diglycerol fatty acid ester, ethylhexyl palmitate and isopropyl myristate.
As a preferable scheme of the microcapsule high-efficiency preservative, the microcapsule high-efficiency preservative comprises the following components in percentage by weight: the nipagin ester is one or a combination of two or more of nipagin methyl ester, nipagin ethyl ester, nipagin propyl ester and nipagin butyl ester.
As a preferable scheme of the microcapsule high-efficiency preservative, the microcapsule high-efficiency preservative comprises the following components in percentage by weight: the particle size range of the allantoin is 15-35 mu m, and the average particle size is 20 mu m.
As a preferable scheme of the microcapsule high-efficiency preservative, the antibacterial capsule wall component is one or a composition of more than two of chitosan with deacetylation degree of more than 85%, oxidized dextrin, hardened grease and β -cyclodextrin.
As a preferable scheme of the microcapsule high-efficiency preservative, the microcapsule high-efficiency preservative comprises the following components in percentage by weight: the heat-sensitive agent is a composition of polypropylene glycol-400 and any one or two or more of baking soda, calcium carbonate and soda ash.
As a preferable scheme of the microcapsule high-efficiency preservative, the microcapsule high-efficiency preservative comprises the following components in percentage by weight: the cosolvent is a composition of aminosiloxane and n-propyl acetate.
As a preferable scheme of the microcapsule high-efficiency preservative, the microcapsule high-efficiency preservative comprises the following components in percentage by weight: the solvent is a composition of deionized water, ethanol and triethylene glycol.
The invention also aims to provide a preparation method of the microcapsule high-efficiency preservative.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions: a preparation method of a microcapsule high-efficiency preservative comprises the following specific steps: slowly adding 8-16 parts of fatty acid ester, 5-10 parts of nipagin ester and 10-20 parts of allantoin into 15-27 parts of molten antibacterial capsule wall components, stirring for 10-20 min at 1000-1400 rpm by using a high-speed stirrer, slowly adding the mixed solution into 190-365 parts of aminosiloxane, stirring for 5-15 min at 4500-7500 rpm by using the high-speed stirrer while adding, and cooling to room temperature to obtain a microcapsule-containing earlier-stage mixed solution; mixing 5-9 parts of molten antibacterial capsule wall component with 2-5 parts of heat-sensitive agent and 70-140 parts of aminosiloxane, stirring for 5-15 min at 4000-7000 rpm by using a high-speed stirrer, slowly adding the obtained early-stage mixed solution containing the microcapsules into the mixture, stirring for 5-15 min at 800-1200 rpm by using the stirrer while adding the mixture, allowing the microcapsules to obtain double-layer capsule walls, and cooling to room temperature to obtain a suspension containing the microcapsules; and (2) carrying out suction filtration on the suspension containing the microcapsules through filter paper with the pore diameter of 5-20 mu m, wherein the pump pressure is 0.015-0.045 MPa, so as to obtain microcapsule particles, adding 1.25-3 parts of aminosiloxane, 1.75-4 parts of n-propyl acetate, 18-24 parts of deionized water, 64-95 parts of ethanol and 24-33 parts of triethylene glycol, adjusting the speed to 220-260 rpm, and continuously stirring for 2-5 min, so as to obtain the microcapsule high-efficiency preservative.
The invention further aims to provide application of the microcapsule high-efficiency preservative in food.
The invention has the beneficial effects that:
(1) the microcapsule high-efficiency preservative adopts environment-friendly raw materials, has obvious effect, can ensure the preservative effect by only using 0.005-0.02 percent of the amount when in use, is non-toxic and has little effective amount, thus having no influence on the health of human bodies.
(2) The microcapsule high-efficiency preservative achieves the high-efficiency sterilization and preservation effects by compounding the fatty acid ester, the nipagin ester and the allantoin, and experiments prove that the reasonable compounding effect of the three components is far better than that of any one of the three components which are used independently, so that the synergistic effect is generated.
(3) The microcapsule high-efficiency preservative is formed by two-time feeding and curing of the microcapsule wall in the preparation process to form the microcapsule wall with a double-layer structure, and only the outer-layer capsule wall contains the heat-sensitive agent, so that the microcapsule with the structure has the characteristics of excellent heat stability and thermal response, and the microcapsule with the structure has no effect if the microcapsule wall is formed by one-time curing or the inner-layer capsule wall of the microcapsule contains the heat-sensitive agent and the outer layer does not contain the heat-sensitive agent. Experiments prove that the microcapsule high-efficiency preservative can adapt to the temperature range of minus 80-225 ℃, and the preservative performance within minus 15-80 ℃ has thermal responsiveness.
(4) The microcapsule high-efficiency preservative has good preservative performance under different pH values when in use, and can be applied to the fields of food, cosmetics, textile, papermaking and building industries due to wide application range of the microcapsule high-efficiency preservative to pH and temperature environmental factors.
(5) The microcapsule high-efficiency preservative can be applied by spraying, coating and uniformly mixing with materials, so that the using condition is not limited.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Unless otherwise specified, all materials used in the present invention are commercially available, food grade materials.
The test method comprises the following steps:
and (3) testing the corrosion resistance: referring to CTFA bacteria-adding antiseptic challenge test and evaluation standard, fluid food with 0.01% of antiseptic dosage is tested, and the initial inoculation bacterial amount is 106cfu/g (note: no other ingredients in the food sample that contribute to sterilization, bacteriostasis, preservation), then:
at 28 days, the samples contain bacteria or mould of more than 1000cfu/g, the samples can not pass the bacteria-adding antiseptic challenge test, the antiseptic in the samples can not effectively inhibit the action of microorganism, and the products are easily polluted by the microorganism during production, storage and use.
On day 28, the sample contains 100-1000 cfu/g of bacteria or mold, and the sample conditionally passes the challenge test, namely the protein or other animal and biological material components in the sample are not particularly high, the produced sanitary environment meets the requirement, and the preservative can be used when the package is not easy to generate secondary pollution, otherwise, the preservative cannot be used.
On the 28 th day, the sample contains 10-100 cfu/g of bacteria or mould, and the challenge test of the sample shows that the preservative in the sample has a strong effect of inhibiting and killing microorganisms, so that the product is not easily polluted by the microorganisms during production, storage and use.
From day 7 onwards, the samples contained <10cfu/g of bacteria or mold, and the samples passed challenge tests, which indicated that the preservatives in the samples had a particularly strong killing effect on microorganisms, and the products were not easily contaminated with microorganisms during production, storage and use.
Example 1
(1) Slowly adding 4 parts of sucrose fatty acid monoester, 4.5 parts of diglycerol fatty acid ester, 3.5 parts of ethylhexyl palmitate, 3 parts of ethylparaben, 4.5 parts of propylparaben and 15 parts of allantoin into 7.5 parts of molten chitosan with deacetylation degree of more than 85%, 5.5 parts of hardened grease and 8 parts of β -cyclodextrin, stirring for 15min at 1200rpm by using a high-speed stirrer, slowly adding the mixed solution into 250-305 parts of aminosiloxane while stirring for 10min at 6000rpm, and cooling to room temperature to obtain a mixed solution containing microcapsules at the early stage;
(2) mixing 2.5 parts of molten chitosan with deacetylation degree of more than 85%, 1.8 parts of hardened grease, 2.7 parts of β -cyclodextrin, 1.5 parts of polypropylene glycol-400, 1.5 parts of baking soda, 1 part of calcium carbonate and 90-120 parts of aminosiloxane, stirring for 10min at 5500rpm by using a high-speed stirrer, slowly adding the obtained microcapsule-containing early-stage mixed solution into the mixture, stirring for 10min at 1000rpm by using the stirrer while adding, allowing the microcapsules to obtain a double-layer capsule wall, and cooling to room temperature to obtain a microcapsule-containing suspension;
(3) and (2) carrying out suction filtration on the suspension containing the microcapsules through filter paper with the aperture of 5-20 mu m, wherein the pump pressure is 0.03MPa, so as to obtain microcapsule particles, adding 2.125 parts of aminosiloxane, 2.875 parts of n-propyl acetate, 21 parts of deionized water, 79.5 parts of ethanol and 28.5 parts of triethylene glycol, adjusting the speed to 240rpm, and continuously stirring for 3.5min, so as to obtain the microcapsule high-efficiency preservative.
(4) And (3) testing results: the obtained microcapsule high-efficiency preservative has wide adaptability to various products, excellent broad-spectrum sterilization property and inhibition and killing effect on various bacteria and fungi (bacillus, coccus, spirillum, chytrid, zygomycetes, ascomycetes and basidiomycetes); from day 7 onwards, the samples contained <10cfu/g of bacteria or mold, and through the challenge test, had a particularly strong inhibitory effect on microorganisms.
The food products were tested for preservative performance at different temperatures using the formulations of example 1 and the data are shown in table 1.
TABLE 1
Figure BDA0002294011750000051
As can be seen from the data in Table 1, the temperature of the preservative in use and the preservative performance are regular, namely, the preservative has thermal responsiveness, and controllable preservative performance is realized. The prepared microcapsule high-efficiency preservative can adapt to the temperature range of minus 80-225 ℃, and the preservative performance of the microcapsule high-efficiency preservative at minus 15-80 ℃ has thermal responsiveness.
Example 2
(1) Slowly adding 4.5 parts of sucrose fatty acid monoester, 4.5 parts of ethylhexyl palmitate, 3 parts of isopropyl myristate, 3.5 parts of propylparaben, 4 parts of butylparaben and 15 parts of allantoin into 8 parts of molten chitosan with deacetylation degree of more than 85%, 5.5 parts of hardened grease and 7.5 parts of oxidized dextrin, stirring for 15min at 1200rpm by using a high-speed stirrer, slowly adding the mixed solution into 250-305 parts of aminosiloxane while stirring for 10min at 6000rpm by using the high-speed stirrer, and cooling to room temperature to obtain a primary mixed solution containing microcapsules;
(2) mixing 2.7 parts of molten chitosan with deacetylation degree of more than 85%, 1.8 parts of hardened grease, 2.5 parts of oxidized dextrin, 1.5 parts of polypropylene glycol-400, 1.25 parts of soda ash, 1.25 parts of calcium carbonate and 90-120 parts of aminosiloxane, stirring for 10min at 5500rpm by using a high-speed stirrer, slowly adding the obtained microcapsule-containing early-stage mixed solution into the mixture, stirring for 10min at 1000rpm by using a stirrer while adding, allowing the microcapsules to obtain a double-layer capsule wall, and cooling to room temperature to obtain a microcapsule-containing suspension;
(3) carrying out suction filtration on the suspension containing the microcapsules through filter paper with the aperture of 5-20 microns, and pumping at 0.03MPa to obtain microcapsule particles, adding 2.125 parts of aminosiloxane, 2.875 parts of n-propyl acetate, 21 parts of deionized water, 79.5 parts of ethanol and 28.5 parts of triethylene glycol, adjusting the speed to 240rpm, and continuing stirring for 3.5min to obtain the microcapsule high-efficiency preservative;
(4) and (3) testing results: the obtained microcapsule high-efficiency preservative has wide adaptability to various products, excellent broad-spectrum sterilization property and inhibition and killing effect on various bacteria and fungi (bacillus, coccus, spirillum, chytrid, zygomycetes, ascomycetes and basidiomycetes); from the 7 th day, the sample contains bacteria or mould with the concentration of less than 10cfu/g, and has extremely strong inhibition and killing effects on microorganisms through a challenge test; has good thermal stability and good thermal responsiveness.
Comparative example 1
(1) Adding 11.5 parts of sucrose fatty acid monoester, 12 parts of diglycerol fatty acid ester and 11 parts of ethylhexyl palmitate slowly into 7.5 parts of molten chitosan with deacetylation degree of more than 85%, 5.5 parts of hardened grease and 8 parts of β -cyclodextrin, stirring for 15min at 1200rpm by using a high-speed stirrer, then slowly adding the mixed solution into 250-305 parts of aminosiloxane, stirring for 10min at 6000rpm by using the high-speed stirrer while adding, and cooling to room temperature to obtain a microcapsule-containing early-stage mixed solution (compared with example 1, nipagin ester and allantoin are not added, and the balance is supplemented by fatty acid ester);
(2) mixing 2.5 parts of molten chitosan with deacetylation degree of more than 85%, 1.8 parts of hardened grease, 2.7 parts of β -cyclodextrin, 1.5 parts of polypropylene glycol-400, 1.5 parts of baking soda, 1 part of calcium carbonate and 90-120 parts of aminosiloxane, stirring for 10min at 5500rpm by using a high-speed stirrer, slowly adding the obtained microcapsule-containing early-stage mixed solution into the mixture, stirring for 10min at 1000rpm by using the stirrer while adding, allowing the microcapsules to obtain a double-layer capsule wall, and cooling to room temperature to obtain a microcapsule-containing suspension;
(3) and (2) carrying out suction filtration on the suspension containing the microcapsules through filter paper with the aperture of 5-20 mu m, wherein the pump pressure is 0.03MPa, so as to obtain microcapsule particles, adding 2.125 parts of aminosiloxane, 2.875 parts of n-propyl acetate, 21 parts of deionized water, 79.5 parts of ethanol and 28.5 parts of triethylene glycol, adjusting the speed to 240rpm, and continuously stirring for 3.5min, so as to obtain the microcapsule high-efficiency preservative.
(4) And (3) testing results: the obtained microcapsule high-efficiency preservative has poor adaptability to cosmetics, fabrics and the like, general broad-spectrum sterilization, small inhibition and killing range on bacterial species and only has inhibition and killing effects on bacilli, cocci, chytrid and ascomycetes; on the 28 th day, the sample contains 100-1000 cfu/g of bacteria or mold, and conditionally passes a challenge test, so that the inhibition and killing effect on microorganisms is general; the thermal stability is general and has a certain thermal responsiveness.
Comparative example 2
(1) 4 parts of sucrose fatty acid monoester, 4.5 parts of diglycerol fatty acid ester, 3.5 parts of ethylhexyl palmitate, 3 parts of ethylparaben, 4.5 parts of propylparaben, 15 parts of allantoin, 1.5 parts of polypropylene glycol-400, 1.5 parts of baking soda and 1 part of calcium carbonate are slowly added into 10 parts of molten chitosan with deacetylation degree of more than 85%, 7.3 parts of hardened grease and 10.7 parts of β -cyclodextrin, stirred for 15min at 1200rpm by using a high-speed stirrer, then the mixed solution is slowly added into 340-425 parts of aminosiloxane, stirred for 10min at 6000rpm by using the high-speed stirrer while adding, and cooled to room temperature to obtain a suspension containing microcapsules;
(2) and (3) carrying out suction filtration on the suspension containing the microcapsules through filter paper with the aperture of 5-20 microns, wherein the pump pressure is 0.03MPa, so as to obtain microcapsule particles, adding 2.125 parts of aminosiloxane, 2.875 parts of n-propyl acetate, 21 parts of deionized water, 79.5 parts of ethanol and 28.5 parts of triethylene glycol, adjusting the speed to 240rpm, and continuously stirring for 3.5min, so as to obtain the microcapsule high-efficiency preservative (compared with the embodiment 1, after one-time addition of microcapsule wall components is finished, a single-layer wall containing the thermosensitive agent is formed through solidification).
(3) And (3) testing results: the obtained microcapsule high-efficiency preservative has wide adaptability to various products, good broad-spectrum sterilization property and wide inhibition and killing range to bacterial species (bacillus, spirillum, chytrid, ascomycete and basidiomycete); on the 28 th day, the sample contains 10-100 cfu/g of bacteria or mould, and the inhibition and killing effect on microorganisms is strong through a challenge test; but the thermal stability was poor and there was no significant thermal responsiveness.
Comparative example 3
(1) 4 parts of sucrose fatty acid monoester, 4.5 parts of diglycerol fatty acid ester, 3.5 parts of ethylhexyl palmitate, 3 parts of ethylparaben, 4.5 parts of propylparaben, 15 parts of allantoin, 1.5 parts of polypropylene glycol-400, 1.5 parts of baking soda, 1 part of calcium carbonate and 90-120 parts of aminosiloxane are slowly added into 7.5 parts of molten chitosan with deacetylation degree of more than 85%, 5.5 parts of hardened grease and 8 parts of β -cyclodextrin, the mixture is stirred at 1200rpm for 15min by using a high-speed stirrer, then the mixture is slowly added into 250-305 parts of aminosiloxane, the mixture is stirred at 6000rpm for 10min while being added, and the mixture is cooled to room temperature to obtain a pre-stage mixed solution containing microcapsules;
(2) mixing 2.5 parts of molten chitosan with deacetylation degree of more than 85%, 1.8 parts of hardened grease and 2.7 parts of β -cyclodextrin, stirring for 10min at 5500rpm by using a high-speed stirrer, slowly adding the obtained microcapsule-containing early-stage mixed solution into the mixture, stirring for 10min at 1000rpm by using a stirrer while adding the mixture to obtain a double-layer capsule wall of the microcapsule, and cooling to room temperature to obtain a microcapsule-containing suspension (compared with example 1, the inner layer of the capsule wall of the microcapsule contains a thermosensitive agent, and the outer layer does not contain the thermosensitive agent);
(3) and (2) carrying out suction filtration on the suspension containing the microcapsules through filter paper with the aperture of 5-20 mu m, wherein the pump pressure is 0.03MPa, so as to obtain microcapsule particles, adding 2.125 parts of aminosiloxane, 2.875 parts of n-propyl acetate, 21 parts of deionized water, 79.5 parts of ethanol and 28.5 parts of triethylene glycol, adjusting the speed to 240rpm, and continuously stirring for 3.5min, so as to obtain the microcapsule high-efficiency preservative.
(4) And (3) testing results: the obtained microcapsule high-efficiency preservative has wide adaptability to various products, good broad-spectrum sterilization property and wide inhibition and killing range to bacterial species (bacillus, spirillum, chytrid, ascomycete and basidiomycete); on the 28 th day, the sample contains 10-100 cfu/g of bacteria or mould, and the inhibition and killing effect on microorganisms is strong through a challenge test; the thermal stability is good, but the thermal responsiveness is not good.
Comparative example 4
A commercially available preservative.
And (3) testing results: the product has wide adaptability to various products, good broad-spectrum sterilization, and wide inhibition and killing range to bacterial species (bacillus, spirillum, chytrid, ascomycete); on the 28 th day, the sample contains 10-100 cfu/g of bacteria or mould, and the inhibition and killing effect on microorganisms is strong through a challenge test; the thermal stability is poor and the thermal responsiveness is not good.
Comparative example 5
On the basis of the example 1, the influence of the addition amounts of different fatty acid esters, nipagin ester and allantoin on the sterilization effect of the microcapsule high-efficiency preservative is shown in the test design and the results in tables 2 and 3.
TABLE 2
Figure BDA0002294011750000081
Figure BDA0002294011750000091
TABLE 3
Figure BDA0002294011750000092
Figure BDA0002294011750000101
Most fatty acid esters have the functions of fresh keeping and antibiosis, and are particularly used for coating and fresh keeping of meat, eggs, vegetables, fruits and the like; the nipagin ester can destroy the cell membrane of the microorganism, denature the protein in the cell and inhibit the activity of the respiratory enzyme system and the electron transfer enzyme system of the microorganism cell; allantoin is an amphoteric compound, can combine with multiple substances to form double salt, and has light-shielding, antibacterial, antiseptic, analgesic, and antioxidant effects. The microcapsule wall maintains the heat stability of the preservative and endows the preservative with the heat responsiveness, the wall with a double-layer structure is formed by two times of feeding and curing, and only the outer layer wall contains the heat-sensitive agent, so that the microcapsule wall has the characteristics of excellent heat stability and heat responsiveness, and if the microcapsule wall is formed by one-time curing, or the inner layer wall of the microcapsule contains the heat-sensitive agent and the outer layer does not contain the heat-sensitive agent, the effect is not achieved. The efficient sterilization and preservation effects are achieved through the compounding of the fatty acid ester, the nipagin ester and the allantoin, and experiments prove that the reasonable compounding effect of the three components is far better than that of any one of the three components which are used independently, so that the synergistic effect is generated among the three components.
In conclusion, the microcapsule high-efficiency preservative adopts environment-friendly raw materials, has obvious effect, can ensure the preservative effect by only using 0.005-0.02 percent of the amount when in use, is non-toxic and has little effective amount, thus having no influence on the health of human bodies. The microcapsule high-efficiency preservative achieves the high-efficiency sterilization and preservation effects by compounding the fatty acid ester, the nipagin ester and the allantoin, and experiments prove that the reasonable compounding effect of the three components is far better than that of any one of the three components which are used independently, so that the synergistic effect is generated.
The microcapsule high-efficiency preservative is formed by twice charging and curing of the microcapsule wall in the preparation process to form a double-layer structure capsule wall, and only the outer-layer capsule wall contains a heat-sensitive agent. It has been surprisingly found that microcapsules of this structure have excellent thermal stability and thermal response, which is not the case if they are cured at one time to form the microcapsule wall or if the inner wall of the microcapsule contains a heat-sensitive agent and the outer wall does not. Experiments prove that the microcapsule high-efficiency preservative can adapt to the temperature range of minus 80-225 ℃, and the preservative performance within minus 15-80 ℃ has thermal responsiveness.
The microcapsule high-efficiency preservative has good preservative performance under different pH values when in use, and can be applied to various industrial fields of food, cosmetics, textile, papermaking, building and the like due to wide application range of environmental factors such as pH, temperature and the like. The microcapsule high-efficiency preservative can be applied by spraying, coating, uniformly mixing with materials and the like, so that the using condition is not limited.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (10)

1. A microcapsule high-efficiency preservative is characterized in that: the microcapsule high-efficiency preservative comprises the following raw materials in parts by weight: 8-16 parts of fatty acid ester, 5-10 parts of nipagin ester, 10-20 parts of allantoin, 20-36 parts of antibacterial capsule wall component, 2-5 parts of thermosensitive agent, 3-7 parts of cosolvent and 106-152 parts of solvent.
2. The microcapsule high-efficiency preservative according to claim 1, wherein: the fatty acid ester is one or a combination of more than two of sucrose fatty acid monoester, diglycerol fatty acid ester, ethylhexyl palmitate and isopropyl myristate.
3. The microcapsule high-efficiency preservative according to claim 1, wherein: the nipagin ester is one or a combination of two or more of nipagin methyl ester, nipagin ethyl ester, nipagin propyl ester and nipagin butyl ester.
4. The microcapsule high-efficiency preservative according to claim 1, wherein: the particle size range of the allantoin is 15-35 mu m, and the average particle size is 20 mu m.
5. The microcapsule high-efficiency preservative according to claim 1, wherein the antibacterial capsule wall component is one or a combination of two or more of chitosan with a degree of deacetylation of > 85%, oxidized dextrin, hardened oil and β -cyclodextrin.
6. The microcapsule high-efficiency preservative according to claim 1, wherein: the heat-sensitive agent is a composition of polypropylene glycol-400 and any one or two or more of baking soda, calcium carbonate and soda ash.
7. The microcapsule high-efficiency preservative according to claim 1, wherein: the cosolvent is a composition of aminosiloxane and n-propyl acetate.
8. The microcapsule high-efficiency preservative according to claim 1, wherein: the solvent is a composition of deionized water, ethanol and triethylene glycol.
9. The preparation method of the microcapsule high-efficiency preservative according to any one of claims 1 to 8, which is characterized by comprising the following specific steps:
slowly adding 8-16 parts of fatty acid ester, 5-10 parts of nipagin ester and 10-20 parts of allantoin into 15-27 parts of molten antibacterial capsule wall components, stirring for 10-20 min at 1000-1400 rpm by using a high-speed stirrer, slowly adding the mixed solution into 190-365 parts of aminosiloxane, stirring for 5-15 min at 4500-7500 rpm by using the high-speed stirrer while adding, and cooling to room temperature to obtain a microcapsule-containing earlier-stage mixed solution;
mixing 5-9 parts of molten antibacterial capsule wall component with 2-5 parts of heat-sensitive agent and 70-140 parts of aminosiloxane, stirring for 5-15 min at 4000-7000 rpm by using a high-speed stirrer, slowly adding the obtained early-stage mixed solution containing the microcapsules into the mixture, stirring for 5-15 min at 800-1200 rpm by using the stirrer while adding the mixture, allowing the microcapsules to obtain double-layer capsule walls, and cooling to room temperature to obtain a suspension containing the microcapsules;
and (2) carrying out suction filtration on the suspension containing the microcapsules through filter paper with the pore diameter of 5-20 mu m, wherein the pump pressure is 0.015-0.045 MPa, so as to obtain microcapsule particles, adding 1.25-3 parts of aminosiloxane, 1.75-4 parts of n-propyl acetate, 18-24 parts of deionized water, 64-95 parts of ethanol and 24-33 parts of triethylene glycol, adjusting the speed to 220-260 rpm, and continuously stirring for 2-5 min, so as to obtain the microcapsule high-efficiency preservative.
10. The method for preparing the microcapsule high-efficiency preservative according to claim 1 or 5, wherein: the melting point range of the antibacterial capsule wall component is 60-80 ℃, the particle size range of the microcapsule is 20-50 mu m, and the average particle size is 35 mu m.
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