CN115137035B - Preparation method of montmorillonite mildew inhibitor - Google Patents

Preparation method of montmorillonite mildew inhibitor Download PDF

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CN115137035B
CN115137035B CN202210831162.4A CN202210831162A CN115137035B CN 115137035 B CN115137035 B CN 115137035B CN 202210831162 A CN202210831162 A CN 202210831162A CN 115137035 B CN115137035 B CN 115137035B
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reaction
montmorillonite
aqueous solution
montmorillonite powder
citric acid
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CN115137035A (en
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陆军
于琴
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Zhejiang Weijing Technology 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
    • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
    • A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
    • A23L5/273—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption using adsorption or absorption agents, resins, synthetic polymers, or ion exchangers
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/105—Aliphatic or alicyclic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/20—Inorganic substances, e.g. oligoelements
    • A23K20/24—Compounds of alkaline earth metals, e.g. magnesium
    • 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
    • A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
    • 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
    • A23L3/3499—Organic compounds containing oxygen with doubly-bound oxygen
    • 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
    • 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
    • A23L3/358—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a preparation method of a montmorillonite mildew preventive, which comprises the following steps: (a) Uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, adding polylysine aqueous solution for hydrothermal reaction after the reaction is finished, and filtering, centrifuging and drying after the reaction is finished to obtain a solid mixture; (b) Mixing the solid mixture with 6-gingerol and water chestnut peel extract proportionally. The invention can prepare the nontoxic broad-spectrum mildew inhibitor by a simple and low-cost method, has good and durable mildew-proof effect, is beneficial to the stable storage of feed and prevents the loss of nutrient components.

Description

Preparation method of montmorillonite mildew inhibitor
Technical Field
The invention relates to the technical field of mildew inhibitors, in particular to a preparation method of a montmorillonite mildew inhibitor.
Background
Mycotoxins are toxic metabolites produced by moulds in their contaminated food products and they can pass through the feed into the animal. The mildew of the feed is easy to occur during the storage, transportation, sale and use processes, and a large amount of mould for growth and reproduction pollutes the feed, so that not only is the nutrition substances in the feed consumed and the quality of the feed reduced and the feed return reduced, but also diarrhea, enteritis and the like caused by the feed can cause the symptoms of reduced digestion capacity, reduced lymphatic function and the like after the feed is eaten by livestock and poultry, the tissues such as the liver, the kidney, the nerves, the hematopoiesis, the skin and the like of the organism are damaged, and serious death can even be caused.
Montmorillonite is an aluminosilicate mineral containing crystal water in a ratio of 2:1, and is formed by sandwiching an aluminum oxide octahedral sheet between two layers of silicon oxide tetrahedral sheets; the most basic structural layer is constructed by linking a silicon oxygen tetrahedral sheet with an aluminum oxygen octahedral sheet through a common oxygen atom, all top oxygen atoms of the silicon oxygen tetrahedral being directed to the aluminum oxygen octahedron. Based on the special structural composition, the montmorillonite has larger surface area and cation exchange capacity, and the addition of montmorillonite becomes the first choice of mould-proof mould-release measures suitable for large-scale feed production; the strong adsorption capacity of montmorillonite comes from ultra-large surface area and electrostatic adsorption, but the interlayer spacing of natural montmorillonite is limited, so that the montmorillonite has selectivity on adsorption of mycotoxin, has good adsorption performance on strong-polarity aflatoxin, and has poor adsorption and removal effects on hydrophobic and weak-polarity mold (such as zearalenone and vomitoxin) and the like, so that the montmorillonite is required to be modified to improve the service performance, expand the application range and improve the application value.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a preparation method of the montmorillonite mildew inhibitor, which can prepare a nontoxic broad-spectrum mildew inhibitor by a simple and low-cost method, has good and durable mildew-proof effect, is beneficial to stable storage of feed and prevents nutrient loss.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of a montmorillonite mildew preventive comprises the following steps:
(a) Uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, adding polylysine aqueous solution for hydrothermal reaction after the reaction is finished, and filtering, centrifuging and drying after the reaction is finished to obtain a solid mixture;
in the step, calcium peroxide reacts with water to generate oxygen and calcium hydroxide, the generated oxygen is collected and can be applied to other fields as byproducts, and meanwhile, the generation of the oxygen can expand the interlayer spacing of montmorillonite, so that the adsorption performance is improved; the calcium citrate is generated by the reaction of calcium hydroxide and excessive citric acid, and the calcium citrate is added into the feed, so that the calcium citrate is not only an acidulant but also a calcium source, can promote gastric acid secretion of animals, reduce the emptying speed of gastrointestinal tracts, promote nutrient absorption, enhance the anti-stress capability of animals, improve animal body shape and meat color, and improve meat quality; in addition, the redundant citric acid can acidify the montmorillonite to promote the cation between montmorillonite layers to be converted into acid soluble salt, so that the binding force between original montmorillonite layers is weakened, the interlayer lattice of the montmorillonite is favorably cracked, the interlayer spacing is further enlarged, the subsequent intercalation of polylysine is favorably realized, and the specific surface area and the adsorption capacity of the montmorillonite are increased; the citric acid remained in the solid mixture is also a natural mildew inhibitor, which can reduce the pH of the feed, inhibit the proliferation of harmful microorganisms and the generation of toxins, and can be used as a synergist of antioxidant, and can be mixed with the feed antioxidant for use, thereby improving the antioxidation effect, preventing or delaying the oxidation of the feed, improving the stability of the compound feed and prolonging the storage period.
(b) Mixing the solid mixture with 6-gingerol and water chestnut peel extract at a certain proportion.
In the step (a), the dosage ratio of the montmorillonite powder to the deionized water is 1g when the montmorillonite powder is dispersed: 100mL.
In the step (a), the addition amount of the calcium peroxide is 3-5% of the mass of the montmorillonite powder.
In the step (a), the concentration of the citric acid aqueous solution is 0.1mol/L, and the molar ratio of the calcium peroxide to the citric acid in the citric acid aqueous solution is 3:2.5-4.
In the step (a), the concentration of the polylysine aqueous solution is 0.1mol/L, and the mass ratio of montmorillonite powder to polylysine in the polylysine aqueous solution is 1:0.07-0.15.
In the step (a), the hydrothermal reaction temperature is 50-60 ℃ and the reaction time is 4-8h.
In the step (b), the addition amount of the 6-gingerol is 3-5.5% of the mass of montmorillonite powder.
In the step (b), the addition amount of the chufa peel extract is 2-5% of montmorillonite powder.
The beneficial effects of the invention are as follows: the interlayer distance of the montmorillonite is enlarged by utilizing oxygen generated by the reaction of calcium peroxide and water, then the montmorillonite is acidized by citric acid, the bonding force between montmorillonite layers is further weakened, the intercalation of polylysine is promoted, and meanwhile, the interlayer is provided with hydrophilic and lipophilic properties by utilizing the intercalation of polylysine, so that the adsorption capacity is obviously increased, and particularly, the adsorption and removal of hydrophobic and weak-polarity mould are realized; the mold-proof capability is further improved and the feed is prolonged by the synergistic effect of substances through the compounding of polylysine, 6-gingerol, chufa peel extract and montmorillonite; the mildew preventive is nontoxic and harmless, the safety of feed can be improved, the calcium citrate can promote the absorption of nutrient substances, the healthy growth of animals can be promoted, oxygen generated in the production process can be used as a byproduct, and the economic benefit of production and preparation can be improved.
Detailed Description
The invention is further described in connection with the following detailed description:
example 1
A preparation method of a montmorillonite mildew preventive comprises the following steps:
(a) Uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, adding polylysine aqueous solution for hydrothermal reaction at 60 ℃ for 4 hours after the reaction is finished, and filtering, centrifuging and drying at 60 ℃ after the reaction is finished to obtain a solid mixture;
wherein, the dosage ratio of montmorillonite powder to deionized water is 1g when the montmorillonite powder is dispersed: 100mL; the addition amount of the calcium peroxide is 3% of the mass of the montmorillonite powder; the concentration of the aqueous solution of citric acid is 0.1mol/L, and the molar ratio of the calcium peroxide to the citric acid in the aqueous solution of citric acid is 3:2.5; the concentration of the polylysine aqueous solution is 0.1mol/L, and the mass ratio of montmorillonite powder to polylysine in the polylysine aqueous solution is 1:0.15.
(b) Mixing the solid mixture with 6-gingerol and water chestnut peel extract at a certain proportion. Wherein the addition amount of 6-gingerol is 5% of the mass of montmorillonite powder; the addition amount of the chufa peel extract is 3.6% of montmorillonite powder.
Example 2
A preparation method of a montmorillonite mildew preventive comprises the following steps:
(a) Uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, adding polylysine aqueous solution for hydrothermal reaction at 60 ℃ for 6 hours after the reaction is finished, and filtering, centrifuging and drying at 60 ℃ after the reaction is finished to obtain a solid mixture;
wherein, the dosage ratio of montmorillonite powder to deionized water is 1g when the montmorillonite powder is dispersed: 100mL; the addition amount of the calcium peroxide is 5% of the mass of the montmorillonite powder; the concentration of the aqueous solution of citric acid is 0.1mol/L, and the molar ratio of the calcium peroxide to the citric acid in the aqueous solution of citric acid is 3:3, a step of; the concentration of the polylysine aqueous solution is 0.1mol/L, and the mass ratio of montmorillonite powder to polylysine in the polylysine aqueous solution is 1:0.1.
(b) Mixing the solid mixture with 6-gingerol and water chestnut peel extract at a certain proportion. Wherein the addition amount of 6-gingerol is 4.7% of the mass of montmorillonite powder; the addition amount of the chufa peel extract is 2% of that of montmorillonite powder.
Example 3
A preparation method of a montmorillonite mildew preventive comprises the following steps:
(a) Uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, adding polylysine aqueous solution for hydrothermal reaction at 50 ℃ for 8 hours after the reaction is finished, and filtering, centrifuging and drying at 60 ℃ after the reaction is finished to obtain a solid mixture;
wherein, the dosage ratio of montmorillonite powder to deionized water is 1g when the montmorillonite powder is dispersed: 100mL; the addition amount of the calcium peroxide is 4% of the mass of the montmorillonite powder; the concentration of the aqueous solution of citric acid is 0.1mol/L, and the molar ratio of the calcium peroxide to the citric acid in the aqueous solution of citric acid is 3:4, a step of; the concentration of the polylysine aqueous solution is 0.1mol/L, and the mass ratio of montmorillonite powder to polylysine in the polylysine aqueous solution is 1:0.1.
(b) Mixing the solid mixture with 6-gingerol and water chestnut peel extract at a certain proportion. Wherein the 6-gingerol addition amount is 3% of the montmorillonite powder mass; the addition amount of the chufa peel extract is 5% of that of montmorillonite powder.
Example 4
A preparation method of a montmorillonite mildew preventive comprises the following steps:
(a) Uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, adding polylysine aqueous solution for hydrothermal reaction at 55 ℃ for 7 hours after the reaction is finished, and filtering, centrifuging and drying at 60 ℃ after the reaction is finished to obtain a solid mixture;
wherein, the dosage ratio of montmorillonite powder to deionized water is 1g when the montmorillonite powder is dispersed: 100mL; the addition amount of the calcium peroxide is 3.5% of the mass of the montmorillonite powder; the concentration of the aqueous solution of citric acid is 0.1mol/L, and the molar ratio of the calcium peroxide to the citric acid in the aqueous solution of citric acid is 3:3, a step of; the concentration of the polylysine aqueous solution is 0.1mol/L, and the mass ratio of montmorillonite powder to polylysine in the polylysine aqueous solution is 1:0.07.
(b) Mixing the solid mixture with 6-gingerol and water chestnut peel extract at a certain proportion. Wherein the addition amount of 6-gingerol is 5.5% of the mass of montmorillonite powder; the addition amount of the chufa peel extract is 4.2% of montmorillonite powder.
Comparative example 1
A montmorillonite mildewproof agent was prepared according to the method and the proportions of example 4, except that step (a) was changed to: uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding a polylysine aqueous solution, carrying out hydrothermal reaction for 7 hours at 55 ℃, and carrying out filtration, centrifugation and drying at 60 ℃ after the reaction is finished; the dosage ratio of montmorillonite powder to deionized water is 1g when dispersing montmorillonite powder: 100mL; the concentration of the polylysine aqueous solution is 0.1mol/L, and the mass ratio of montmorillonite powder to polylysine in the polylysine aqueous solution is 1:0.07.
comparative example 2
A montmorillonite mildewproof agent was prepared according to the method and the proportions of example 4, except that step (a) was changed to: uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, and filtering, centrifuging and drying at 60 ℃ after the reaction is finished to obtain a solid mixture; wherein, the dosage ratio of montmorillonite powder to deionized water is 1g when the montmorillonite powder is dispersed: 100mL; the addition amount of the calcium peroxide is 3.5% of the mass of the montmorillonite powder; the concentration of the aqueous solution of citric acid is 0.1mol/L, and the molar ratio of the calcium peroxide to the citric acid in the aqueous solution of citric acid is 3:3.
comparative example 3
The montmorillonite mold inhibitor was prepared according to the method and the mixture ratio of example 4, except that: step (b) does not add 6-gingerol.
Comparative example 4
The montmorillonite mold inhibitor was prepared according to the method and the mixture ratio of example 4, except that: and (b) adding no chufa peel extract.
The test of the adsorption performance of mycotoxins was performed on the montmorillonite mold inhibitors of examples 1 to 4 and comparative examples 1 to 4, and the results are shown in Table 1. The comparison example 4 and the comparison examples 1-4 show that the oxygen expansion layer modification and the polylysine intercalation modification have a synergistic amplification effect on interlayer spacing of montmorillonite, can effectively improve mildew resistance, has better mildew resistance effect than simple blending, and meanwhile, the polylysine, 6-gingerol and chufa peel extract are compounded to have a synergistic effect, and the lack of any component can reduce the performance of the mildew inhibitor.
TABLE 1
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (2)

1. A preparation method of a montmorillonite mildew preventive is characterized by comprising the following steps: the method comprises the following steps:
(a) Uniformly dispersing montmorillonite powder in deionized water in a reaction kettle, adding calcium peroxide solid, stirring for reaction, adding excessive citric acid aqueous solution after no gas is generated, continuing stirring for reaction, adding polylysine aqueous solution for hydrothermal reaction after the reaction is finished, and filtering, centrifuging and drying after the reaction is finished to obtain a solid mixture; the hydrothermal reaction temperature is 50-60 ℃ and the reaction time is 4-8h;
the addition amount of the calcium peroxide is 3-5% of the mass of the montmorillonite powder; the concentration of the aqueous solution of citric acid is 0.1mol/L, and the molar ratio of the calcium peroxide to the citric acid in the aqueous solution of citric acid is 3:2.5-4; the concentration of the polylysine aqueous solution is 0.1mol/L, and the mass ratio of montmorillonite powder to polylysine in the polylysine aqueous solution is 1:0.07-0.15;
(b) Mixing the solid mixture with 6-gingerol and water chestnut peel extract at a certain proportion; the adding amount of 6-gingerol is 3-5.5% of the mass of montmorillonite powder; the additive amount of the water chestnut peel extract is 2-5% of the mass of montmorillonite powder.
2. The method for preparing the montmorillonite mildew preventive as claimed in claim 1, wherein: in the step (a), the dosage ratio of the montmorillonite powder to the deionized water is 1g when the montmorillonite powder is dispersed: 100mL.
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