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CN113749090B - Abamectin composition, fermentation process and preparation method thereof - Google Patents

Abamectin composition, fermentation process and preparation method thereof Download PDF

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Publication number
CN113749090B
CN113749090B CN202111140504.XA CN202111140504A CN113749090B CN 113749090 B CN113749090 B CN 113749090B CN 202111140504 A CN202111140504 A CN 202111140504A CN 113749090 B CN113749090 B CN 113749090B
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fermentation tank
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CN113749090A (en
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刘丽虹
刘进峰
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Hebei Xingbai Agricultural Technology Co ltd
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Hebei Xingbai Agricultural Science And Technology Co ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • 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
    • A01N25/24—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients to enhance the sticking of the active ingredients
    • 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
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • 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
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/44—Preparation of O-glycosides, e.g. glucosides
    • C12P19/60—Preparation of O-glycosides, e.g. glucosides having an oxygen of the saccharide radical directly bound to a non-saccharide heterocyclic ring or a condensed ring system containing a non-saccharide heterocyclic ring, e.g. coumermycin, novobiocin
    • C12P19/62—Preparation of O-glycosides, e.g. glucosides having an oxygen of the saccharide radical directly bound to a non-saccharide heterocyclic ring or a condensed ring system containing a non-saccharide heterocyclic ring, e.g. coumermycin, novobiocin the hetero ring having eight or more ring members and only oxygen as ring hetero atoms, e.g. erythromycin, spiramycin, nystatin
    • C12P19/623—Avermectin; Milbemycin; Ivermectin; C-076
    • 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

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  • Engineering & Computer Science (AREA)
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  • Agronomy & Crop Science (AREA)
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  • Microbiology (AREA)
  • Dispersion Chemistry (AREA)
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Abstract

The invention provides an abamectin composition, a fermentation process and a preparation method thereof. The stable suspending agent can be prepared by selecting the auxiliary agent and the sand grinding process and equipment; the novel hypha fermentation process is adopted, the preparation is uniform, and the content of active ingredients is stable; the suspending agent prepared by the invention can keep long-term stability, and can quickly recover to a better suspension state when partial precipitation is generated.

Description

Abamectin composition, fermentation process and preparation method thereof
Technical Field
The invention belongs to the field of pesticides, and particularly relates to an abamectin composition, a fermentation process and a preparation method thereof.
Background
The abamectin is fermented by a strain to obtain hypha, and then is extracted by a solvent to obtain a raw drug with higher content, and then is processed into a preparation. Such an operation brings about many problems. 1, the use of a large amount of solvent brings about many problems of environment and life safety even if the solvent can be recycled. 2, solvent extraction or other extraction followed by further processing of the formulation, which brings about a lot of costs. Therefore, the invention is based on the characteristics of hypha and can be processed into the suspending agent. Saves the processing cost, reduces the use of solvents, ensures the environmental protection and the life safety, and has excellent effect of field experiments.
The pesticide raw materials are prepared into different formulations according to different characteristics, such as more than ten formulations, such as missible oil, suspending agent, wettable powder, granules, water agent, poison bait, mother liquor, mother powder and the like. The suspending agent is a preparation prepared by uniformly dispersing a solid pesticide raw material in water in the form of particles with the particle size of less than 4 microns, and the international code is SC. Because SC does not have the problem of dust flying like Wet Powder (WP), is nonflammable and explosive, has small particle size, high biological activity, larger specific gravity and smaller packaging volume, and is safe and environment-friendly compared with other pesticide formulations, SC becomes a pesticide variety with larger tonnage in a novel water-based pesticide formulation.
Disclosure of Invention
The invention provides an abamectin composition, which comprises the following components in part by weight:
Figure GDA0003745390010000021
as an embodiment of the present invention, the hydroxypolyethylene oxide block copolymer has an EO/PO ratio of 1: 1.71.
in one embodiment of the present invention, the hydroxyl value of the hydroxypolyethylene oxide block copolymer is 18 to 20mg KOH/g.
In one embodiment of the present invention, the HLB value of the dispersant is 16.5 to 17.
As an embodiment of the present invention, the dispersant further comprises a polymeric polycarboxylate.
In one embodiment of the present invention, the thickener is lithium magnesium silicate.
As an embodiment of the invention, the bacteriostatic agent is selected from one or two of dodecyl benzyl ammonium chloride, isothiazolinone, chlorine dioxide, sodium monochloride, benzoic acid and sodium benzoate.
An abamectin preparation is prepared from the abamectin composition.
As an embodiment of the present invention, the formulation is in the form of a suspension.
As an embodiment of the invention, the preparation process of the abamectin comprises the following steps:
s01 mixing of raw materials
Adding corn starch, soybean cake powder, yeast powder, a defoaming agent, caustic soda flakes, cobalt chloride, sodium molybdate, manganese sulfate, amylase and water into a feeding pool, and stirring until the mixture is milky;
s02 fermentation
Pumping the milky mixture obtained in the step S01 into a fermentation tank, pressing actinomycetes into the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, introducing steam, maintaining the pressure, continuously sterilizing for 0.5h, cooling to 28.5 ℃, introducing compressed air into the fermentation tank, operating for 540h, sampling, inspecting and discharging to the fermentation tank after the sampling is qualified;
preparation of S03 preparation
And (4) adding the rest components into the fermentation liquor obtained in the step (S02), crushing, and steaming out excessive water from the crushed material.
Has the advantages that:
1. the stable suspending agent can be prepared by selecting the auxiliary agent and the sand grinding process and equipment;
2. the novel hypha fermentation process is adopted, the preparation is uniform, and the content of active ingredients is stable;
3. the suspending agent prepared by the invention can keep long-term stability, and can quickly recover to a better suspension state when partial precipitation is generated.
Detailed Description
Abamectin, english name Abamaectin, accession number: 65195-55-3 and 65195-56-4; it is a macrolide compound with insecticidal, acaricidal and nematicidal activities.
The abamectin has stomach toxicity and contact killing effect on mites and insects, and can not kill eggs. The action mechanism is different from that of the common pesticide in that the action mechanism interferes with the neurophysiological activity and stimulates the release of gamma-aminobutyric acid, and the aminobutyric acid has an inhibition effect on the nerve conduction of arthropods. After the mite adults, nymphs and insect larvae are contacted with the abamectin, paralysis symptoms appear, and the mites die after 2-4 days without moving or taking food. The killing effect of abamectin is slow because the abamectin does not cause rapid dehydration of insects. The abamectin has direct contact killing effect on predatory insects and parasitic natural enemies, but has little damage to beneficial insects because of little residue on the surface of the plant. The abamectin is adsorbed by soil in soil and cannot move and is decomposed by microorganisms, so that the abamectin has no accumulation effect in the environment and can be used as a component of comprehensive control. The preparation is easy to prepare, can be used after being poured into water and slightly stirred, and is safe to crops.
The abamectin is fermented by a strain to obtain hypha, and then the hypha is extracted by a solvent to obtain a raw pesticide with higher content, and then the raw pesticide is processed into a preparation. Such an operation brings about many problems. 1, the use of a large amount of solvent brings about many problems of environment and life safety even if the solvent can be recycled. 2, solvent extraction or other means of extraction followed by further processing of the preparation, comes at a considerable cost.
The invention provides a novel avermectin fermentation method and a preparation process, which solve the problems and comprise the following steps:
s01 raw material mixing
Adding corn starch, soybean cake powder, yeast powder, a defoaming agent, caustic soda flakes, cobalt chloride, sodium molybdate, manganese sulfate, amylase and water into a feeding pool, and stirring until the mixture is milky;
s02 fermentation
Pumping the milky mixture obtained in the step S01 into a fermentation tank, pressing actinomycetes into the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, introducing steam, maintaining the pressure, continuously sterilizing for 0.5h, cooling to 28.5 ℃, introducing compressed air into the fermentation tank, operating for 540h, sampling, inspecting and discharging to the fermentation tank after the sampling is qualified;
preparation of S03 preparation
And (4) adding the rest components into the fermentation liquor obtained in the step (S02), crushing, and steaming out excessive water from the crushed material.
The specific detailed preparation method is as follows:
s01 raw material mixing
15.5t of corn starch, 2.5t of soybean cake powder, 950kg of yeast powder, 600kg of defoaming agent, 25kg of caustic soda flakes, 1.5kg of cobalt chloride, 2kg of sodium molybdate, 500g of manganese sulfate, 3.5kg of amylase and 40m of water are put into a feeding pool 3 Stirring to be milky;
s02 fermentation
Pumping actinomycetes into a fermentation tank by using a feeding pump, pressing actinomycetes to the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, opening front and rear valves of a steam filter to introduce steam, adjusting the opening of a valve to enable a pressure gauge on a precision filter to display 0.13MPa, then directly introducing steam of 0.4MPa and 150 ℃ into the fermentation tank, maintaining the pressure and continuously sterilizing for 0.5h when the temperature on the fermentation tank displays 120 ℃ and the pressure gauge displays 0.13MPa, then introducing circulating water into an inner coil and an outer coil of the fermentation tank to enable the temperature in the fermentation tank to reach 28.5 ℃, introducing compressed air into the fermentation tank, operating for 540h, sampling, inspecting and discharging to the fermentation tank after the temperature is qualified;
preparation of S03 preparation
Adding the rest components into the fermentation liquor, pulverizing, and evaporating excessive water from the pulverized material by a double-effect falling film evaporator according to the content requirement.
Hydroxy polyethylene oxide block copolymers
In the present invention, the EO/PO ratio of the hydroxypolyethylene oxide block copolymer is 1: 1.71; in particular to the brand of Ethylan NS-500 LQ.
As an embodiment of the present invention, the hydroxyl value of the hydroxypolyethylene oxide block copolymer is 18 to 20mg KOH/g; the specific brand is 1603# of Nantong de-Yi chemical industry Co.
In one embodiment of the present invention, the hydroxypolyethylene oxide block copolymer is a hydroxypolyethylene oxide block copolymer of a brand number of ethyllan NS-500LQ and a hydroxypolyethylene oxide block copolymer of a brand number of 1603# in a mass ratio of 7: 2, or a mixture thereof.
Dispersing agent
As the name suggests, the dispersant acts as a dispersing agent. A Dispersant (Dispersant) is a surfactant that has both lipophilic and hydrophilic properties in opposite directions within a molecule. The amphiphilic agent is capable of uniformly dispersing solid and liquid particles of inorganic and organic pigments which are difficult to dissolve in liquids, and also preventing settling and agglomeration of the particles to form stable suspensions.
Common dispersing agents for pesticides are surfactants whose function is to keep the particles dispersed and prevent agglomeration. As the alkyl aryl sulfonate, a formaldehyde condensate thereof, a lignosulfonate, an alkylphenol polyoxyethylene ether formaldehyde condensate, a sulfate, etc. are usually used.
In one embodiment of the invention, the dispersant is selected from dispersants having an HLB value of 16.5 to 17, more preferably a dispersant having an HLB value of 16.9, and more particularly Wacker Germany VOK-G5000.
As an embodiment of the invention, the dispersant also comprises polymeric polycarboxylate, specifically GY-D series carboxylate dispersant of Beijing Guangyuan Yinong Chemicals, Inc., and specifically GY-D800 of Beijing Guangyuan Yinong Chemicals, Inc.
As an embodiment of the present invention, the dispersant further comprises calatlox 4913.
As an embodiment of the invention, the dispersant is prepared from German Wolk VOK-G5000, Guangyuan Yinong GY-D800 and Daatlox 4913 according to the weight ratio of 1: 1: 2.
Defoaming agent
Common defoamers can reduce the surface tension of water, solutions, suspensions, etc., prevent foam formation, or reduce or eliminate the original foam.
The defoamer should have the following properties: the defoaming power is strong, and the dosage is less; adding the product into a foaming system does not influence the basic properties of the system, namely does not react with a system to be defoamed; surface tension is small; the balance between the surface and the surface is good; the heat resistance is good; sixthly, the diffusivity and the permeability are good, and the positive spreading coefficient is higher; the chemical stability and the oxidation resistance are strong; the gas has good solubility and permeability; ninthly, small solubility in the foaming solution; the red (R) has no physiological activity and high safety.
The agricultural chemicals include herbicide, insecticide, bactericide, etc., generally are complex organic matters, and in order to make them uniformly distributed on crops, surfactant must be added to make them into wettable powder or oil-in-water emulsion. Upon dilution, a foam will be produced. The flotation of the foam reduces the uniformity of the pesticide water dispersion, influences the pesticide effect and simultaneously disturbs the spraying operation.
In the invention, the defoaming agent is an organic silicon defoaming agent, and the specific mark is Mi image SAG 672.
In the invention, the specific use method of the defoaming agent is that the organic silicon defoaming agent is firstly mixed with deionized water, and the weight ratio of the two is 10: 1, and then mixed into the whole system.
Thickening agent
The thickener is also called gelatinizer, is a substance capable of increasing the viscosity of latex and liquid, and is also called paste when being used for food. The thickening agent can improve the viscosity of the system, so that the system is kept in a uniform and stable suspension state or an emulsion state, or forms gel; most thickeners have an emulsifying effect. Can be divided into two main categories of natural and synthetic. The natural products are mostly prepared from plants and seaweed containing polysaccharide viscous substances, such as starch, acacia, pectin, agar, gelatin, seaweed gel, carrageenan, dextrin, etc., and general gelatin, soluble starch, polysaccharide derivatives, etc. can be used in cosmetics; the synthetic product includes carboxymethyl cellulose, propylene glycol alginate, methyl cellulose, sodium starch phosphate, sodium carboxymethyl cellulose, sodium alginate, casein, sodium polyacrylate, polyoxyethylene, and polyvinylpyrrolidone.
In one embodiment of the present invention, the thickener is lithium magnesium silicate.
Bacteriostatic agent
Bacteriostatic agents are substances that inhibit the growth of bacteria. The bacteriostatic agent may not kill bacteria, but it can inhibit the growth of bacteria, prevent the bacteria from breeding too much and endanger health.
As an embodiment of the invention, the bacteriostatic agent is selected from one or two of dodecyl dimethyl benzyl ammonium chloride, isothiazolinone, chlorine dioxide, sodium perchlorate, benzoic acid and sodium benzoate.
In a preferred mode of the invention, the bacteriostatic agent is isothiazolinone.
The invention is further described with reference to the following examples:
example 1
This example provides an avermectin composition comprising:
Figure GDA0003745390010000091
the embodiment provides an avermectin suspending agent, and the preparation process of the suspending agent is as follows:
s01 raw material mixing
15.5t of corn starch, 2.5t of soybean cake powder, 950kg of yeast powder, 600kg of defoaming agent, 25kg of caustic soda flakes and cobalt chloride are added into a feeding pool1.5kg, 2kg of sodium molybdate, 500g of manganese sulfate, 3.5kg of amylase and 40m of water 3 Stirring to be milky;
s02 fermentation
Pumping into a fermentation tank by using a feeding pump, pressing 8000 units of actinomycetes into the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, opening front and rear valves of a steam filter to feed steam, adjusting the opening of a valve to enable a pressure gauge on a precision filter to display 0.13MPa, then directly feeding steam with 0.4MPa and 150 ℃ into the fermentation tank, keeping the pressure and continuously sterilizing for 0.5h when the temperature on the fermentation tank is 120 ℃ and the pressure gauge displays 0.13MPa, then feeding circulating water into an inner coil and an outer coil of the fermentation tank to enable the temperature in the fermentation tank to be 28.5 ℃, feeding compressed air into the fermentation tank, sampling and discharging the materials into the fermentation tank after the sampling and the inspection are qualified after the operation is carried out for 540 h;
preparation of S03 preparation
Adding the rest components into the fermentation liquor, then crushing, and distilling off the redundant water by adopting a double-effect falling film evaporator according to the requirement of 1 percent of the abamectin content in the crushed material.
In the invention, an ultrasonic nano crusher is used for crushing treatment, and the type of the ultrasonic nano crusher is JY-3500.
In this example, the hydroxypolyethylene oxide block copolymer is a hydroxypolyethylene oxide block copolymer of a brand number of ethyl lan NS-500LQ and a hydroxypolyethylene oxide block copolymer of a brand number of 1603# in a mass ratio of 7: 2, or a mixture thereof.
In this example, the dispersant was prepared from German Wolk VOK-G5000, Guangyuan Yinong GY-D800, and Daatlox 4913 in the proportions of 1: 1: 2.
In the embodiment, the defoaming agent is an organic silicon defoaming agent, and the specific brand mai chart SAG 672; the specific using method of the defoaming agent is that the organic silicon defoaming agent is mixed with deionized water firstly, and the weight ratio of the organic silicon defoaming agent to the deionized water is 10: 1, and then mixed into the whole system.
In this embodiment, the thickener is lithium magnesium silicate.
In this embodiment, the bacteriostatic agent is isothiazolinone.
Example 2
This example provides an avermectin composition comprising:
Figure GDA0003745390010000101
Figure GDA0003745390010000111
the embodiment provides an avermectin suspending agent, and the preparation process of the suspending agent comprises the following steps:
s01 raw material mixing
15.5t of corn starch, 2.5t of soybean cake powder, 950kg of yeast powder, 600kg of defoaming agent, 25kg of caustic soda flakes, 1.5kg of cobalt chloride, 2kg of sodium molybdate, 500g of manganese sulfate, 3.5kg of amylase and 40m of water are put into a feeding pool 3 Stirring to be milky;
s02 fermentation
Pumping into a fermentation tank by using a feeding pump, pressing 8000 units of actinomycetes to the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, opening front and rear valves of a steam filter to introduce steam, adjusting the opening of a valve to enable a pressure gauge on a precision filter to display 0.13MPa, then directly introducing steam with 0.4MPa and 150 ℃ into the fermentation tank, maintaining the pressure and continuously sterilizing for 0.5h when the temperature on the fermentation tank displays 120 ℃ and the pressure gauge displays 0.13MPa, then introducing circulating water into an inner coil and an outer coil of the fermentation tank to enable the temperature in the fermentation tank to reach 28.5 ℃, introducing compressed air into the fermentation tank, and discharging to the fermentation tank after sampling and checking are qualified after running for 540 h;
preparation of S03 preparation
Adding the rest components into the fermentation liquor, then crushing, and evaporating redundant water from the crushed material by adopting a double-effect falling film evaporator according to the requirement of 1 percent of the abamectin content.
In the invention, an ultrasonic nano grinder is used for grinding treatment, and the model is JY-3500.
In this example, the hydroxypolyethylene oxide block copolymer was a hydroxypolyethylene oxide block copolymer having a trade name of Ethylan NS-500 LQ.
In this example, the dispersant was prepared from Guangyuan Yinong GY-D800 and Daatlox 4913 in the ratio of 1: 1 in a mixed combination.
In the embodiment, the defoaming agent is an organic silicon defoaming agent, and the specific mark is Mi image SAG 672; the specific use method of the defoaming agent is that the organic silicon defoaming agent is mixed with deionized water firstly, and the weight ratio of the two is 10: 1, and then mixed into the whole system.
In this embodiment, the thickener is lithium magnesium silicate.
In this embodiment, the bacteriostatic agent is isothiazolinone.
Example 3
This example provides an avermectin composition comprising:
Figure GDA0003745390010000121
the embodiment provides an avermectin suspending agent, and the preparation process of the suspending agent is as follows:
s01 raw material mixing
15.5t of corn starch, 2.5t of soybean cake powder, 950kg of yeast powder, 600kg of defoaming agent, 25kg of caustic soda flakes, 1.5kg of cobalt chloride, 2kg of sodium molybdate, 500g of manganese sulfate, 3.5kg of amylase and 40m of water are put into a feeding pool 3 Stirring to be milky;
s02 fermentation
Pumping into a fermentation tank by using a feeding pump, pressing 8000 units of actinomycetes to the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, opening front and rear valves of a steam filter to introduce steam, adjusting the opening of a valve to enable a pressure gauge on a precision filter to display 0.13MPa, then directly introducing steam with 0.4MPa and 150 ℃ into the fermentation tank, maintaining the pressure and continuously sterilizing for 0.5h when the temperature on the fermentation tank displays 120 ℃ and the pressure gauge displays 0.13MPa, then introducing circulating water into an inner coil and an outer coil of the fermentation tank to enable the temperature in the fermentation tank to reach 28.5 ℃, introducing compressed air into the fermentation tank, and discharging to the fermentation tank after sampling and checking are qualified after running for 540 h;
preparation of S03 preparation
Adding the rest components into the fermentation liquor, then crushing, and distilling off the redundant water by adopting a double-effect falling film evaporator according to the requirement of 1 percent of the abamectin content in the crushed material.
In the invention, an ultrasonic nano crusher is used for crushing treatment, and the type of the ultrasonic nano crusher is JY-3500.
In this example, the hydroxypolyethylene oxide block copolymer is a hydroxypolyethylene oxide block copolymer of a brand number of ethyl lan NS-500LQ and a hydroxypolyethylene oxide block copolymer of a brand number of 1603# in a mass ratio of 7: 2, or a mixture thereof.
In the embodiment, the dispersant is prepared from German Wolkel VOK-G5000, Guangyuan Yinong GY-D800 according to the weight ratio of 1: 1 in combination.
In the embodiment, the defoaming agent is an organic silicon defoaming agent, and the specific trademark is Mitu SAG 672.
In this embodiment, the thickener is lithium magnesium silicate.
In this embodiment, the bacteriostatic agent is isothiazolinone.
Example 4
This example provides an avermectin composition comprising:
Figure GDA0003745390010000141
the embodiment provides an avermectin suspending agent, and the preparation process of the suspending agent is as follows:
s01 raw material mixing
15.5t of corn starch, 2.5t of soybean cake powder, 950kg of yeast powder, 600kg of defoaming agent, 25kg of caustic soda flakes, 1.5kg of cobalt chloride, 2kg of sodium molybdate, 500g of manganese sulfate, 3.5kg of amylase and 40m of water are put into a feeding pool 3 Stirring to be milky;
s02 fermentation
Pumping into a fermentation tank by using a feeding pump, pressing 8000 units of actinomycetes to the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, opening front and rear valves of a steam filter to introduce steam, adjusting the opening of a valve to enable a pressure gauge on a precision filter to display 0.13MPa, then directly introducing steam with 0.4MPa and 150 ℃ into the fermentation tank, maintaining the pressure and continuously sterilizing for 0.5h when the temperature on the fermentation tank displays 120 ℃ and the pressure gauge displays 0.13MPa, then introducing circulating water into an inner coil and an outer coil of the fermentation tank to enable the temperature in the fermentation tank to reach 28.5 ℃, introducing compressed air into the fermentation tank, and discharging to the fermentation tank after sampling and checking are qualified after running for 540 h;
preparation of S03 preparation
Adding the rest components into the fermentation liquor, then crushing, and evaporating redundant water from the crushed material by adopting a double-effect falling film evaporator according to the requirement of 1 percent of the abamectin content.
In the invention, an ultrasonic nano grinder is used for grinding treatment, and the model is JY-3500.
In this example, the hydroxypolyethylene oxide block copolymer was a hydroxypolyethylene oxide block copolymer having a trade name of Ethylan NS-500 LQ.
In this example, the dispersant was prepared from Guangyuan Yinong GY-D800 and Daatlox 4913 in the ratio of 1: 1 in a mixed combination.
In the embodiment, the defoaming agent is an organic silicon defoaming agent, and the specific brand mai chart SAG 672; the specific use method of the defoaming agent is that the organic silicon defoaming agent is mixed with deionized water firstly, and the weight ratio of the two is 10: 1, and then mixed into the whole system.
In this example, the thickener is xanthan gum.
In this embodiment, the bacteriostatic agent is isothiazolinone.
Performance testing
Test 1: and (3) suspension rate determination: measurements were carried out according to GB/T14825-2006.
And (3) testing 2: the deposition conditions after standing at high temperature (40 ℃) for 6 months are divided into non-deposition, partial deposition and total deposition.
And (3) testing: the examples after being placed at high temperature (40 ℃) for 6 months are stirred, the stirring mode is wood stick stirring, stirring is carried out for 6 circles in one minute, stirring is carried out for one minute, the uniform dispersion condition after stirring is checked, and the examples are divided into dispersion, most of uniform dispersion and small of uniform dispersion.
TABLE 1 Performance test
Figure GDA0003745390010000161
According to the embodiment, the magnesium lithium silicate is selected as the thickening agent, and the specific suspending agent, the defoaming agent and the like are matched, so that the prepared suspending agent has good suspension property, but the magnesium lithium silicate can be penetrated by water molecules in water and has strong stability, so that the inventor finds that when the suspending agent prepared by the magnesium lithium silicate is used immediately or stored for a short time, the product has good stability and the suspension property is beneficial; however, after long-term standing, the suspension stability of the pesticide is gradually transferred to the precipitation stability, and once the precipitation is generated, the difficulty of transferring the pesticide to the suspension is far greater than that of pesticide preparations using lithium magnesium silicate. The present inventors have found that a preparation method using a specific dispersant and a specific suspending agent can solve this problem; the colloid structure is firm and the yield value is large because of the existence of moisture before the finished product is prepared; the performance is stable; however, with the loss of water and the combination of the specific dispersant, the comb-shaped structure of the dispersant can reduce the flexibility value of the magnesium lithium silicate colloid because the acting force of the dispersant is greater than that of the magnesium lithium silicate with the loss of water, thereby alleviating the problems.
Indoor bioassay test report for pesticides
1.0% Abamectin SC on diamondback moth
Indoor biological activity assay
1 purpose of the test:
virulence of 1.0% avermectin suspension SC on Lepidoptera Plutella xylostella (Plutella xylostella L.) larvae
2 conditions of the test
2.1 test targets:
diamondback moth (Plutella xylostella L.) larva with substantially consistent size and health, and average weight of 0.0015 + -0.0001 g/head.
2.2 culture conditions:
the insect rearing room conditions are as follows: feeding fresh radish seedlings at the temperature of 24-26 ℃ and the relative humidity of 70-80% in an illumination period of L: D ═ 14: 10.
2.3 instruments and equipment:
electronic balance (sensing 0.0001), volumetric flask, beaker, pipettor, tweezers, filter paper, marker pen, stopwatch, temperature and humidity control equipment, etc.
Design of the experiment
3.1 reagents
3.1.1 test agents:
the 1.0% avermectin suspending agent SC is the present invention example 1.
3.1.2 other reagents:
acetone, tween 80, distilled water, and the like.
3.2 test treatment
3.2.1 dose settings:
the test agent is directly diluted into 1500 times of solution and 3000 times of solution respectively by using clear water. Clear water was used as a blank control.
3.2.2 test replicates:
each concentration was tested in 4 replicates, each replicate treating 15 test insects.
3.3 mode of treatment
3.3.1 treatment time and number:
test treatments were performed on 24 days at 5 months 2021.
3.3.2 instruments used and methods of administration:
the instruments used include beaker, forceps, stopwatch, finger tube (diameter 1.8cm, length 8cm), etc., and the soaking time is 30 seconds respectively by the leaf soaking method.
4 test method:
the leaf soaking method comprises soaking fresh caulis et folium Brassicae Capitatae in medicinal liquid for 30 s, air drying on absorbent paper, placing into insect box, and inoculating 15 heads of insect test. And (3) feeding and observing under the conditions that the temperature is 24-26 ℃, the relative humidity is 70-80% and the illumination period is L: D ═ 14: 10.
Referring to the agricultural industry standard NYT 1154.14-2008 of the people's republic of China, part 14 of the indoor bioassay test criteria for pesticides: insecticidal activity test, leaf soaking method.
5 data investigation and statistical analysis
5.1 survey methods and grading standards:
the test investigation method is that a skilled technician lightly touches the insect body with a writing brush, and the person who does not move or can not normally crawl is counted as death.
5.2 investigation time and number of surveys:
the test was investigated twice, i.e. 24 and 48 hours after treatment to check for test insect mortality.
5.3 statistical analysis of data
The survival of the test insects is investigated, and the corrected mortality rate is calculated according to the Abbott formula (1).
Figure GDA0003745390010000191
In the formula: mm-corrected mortality
Mt-treatment group mortality
Mc-mortality of control group
The results of the statistical analysis are shown in Table 1.
5.4 other cases
None.
6 results analysis and discussion
6.1 evaluation of drug
TABLE 21.0% Abamectin SC Table of indoor bioassay results for diamondback moth
2021.5.
Figure GDA0003745390010000192
From the indoor bioassay result of the 1.0% avermectin suspending agent SC on the diamondback moth larvae, no matter the dilution is 1500 times or 3000 times after the administration for 24 hours, the toxicity to the diamondback moth larvae is not obviously different. After the two agents are diluted by 1500 times and 3000 times for 48 hours, the toxicity of the two agents to the test insects reaches more than 85 percent.
6.2 problem analysis
The leaf soaking method adopted in the test reflects the main effects of contact toxicity and partial stomach toxicity of the medicament.

Claims (3)

1. An avermectin preparation, which is characterized in that the dosage form is a suspending agent and comprises:
1.0 to 15 percent of abamectin
1-4% of hydroxy polyethylene oxide block copolymer
2 to 8 percent of dispersant
0.1 to 1 percent of defoaming agent
0.2 to 1 percent of thickening agent
0.05 to 0.5 percent of bacteriostatic agent
Water is added to make up to 100 percent;
wherein the hydroxyl polyethylene oxide block copolymer is a hydroxyl polyethylene oxide block copolymer with the trade name of Ethylan NS-500LQ and a hydroxyl polyethylene oxide block copolymer with the trade name of 1603# according to the mass ratio of 7: 2; the dispersant is prepared from German Wolk VOK-G5000, Guangyuan Yinong GY-D800 and Daatlox 4913 according to the weight ratio of 1: 1: 2; the defoaming agent is an organic silicon defoaming agent; the thickener is lithium magnesium silicate.
2. An abamectin formulation according to claim 1, wherein the bacteriostatic agent is selected from one or a combination of dodecyl benzyl ammonium chloride, isothiazolinone, chlorine dioxide, chlordiazepoxide, benzoic acid and sodium benzoate.
3. The avermectin preparation of claim 1, which is prepared by the following process:
s01 raw material mixing
Adding corn starch, soybean cake powder, yeast powder, a defoaming agent, caustic soda flakes, cobalt chloride, sodium molybdate, manganese sulfate, amylase and water into a feeding pool, and stirring until the mixture is milky;
s02 fermentation
Pumping the milky mixture obtained in the step S01 into a fermentation tank, pressing actinomycetes into the fermentation tank from a distributor, adjusting the pH value in the fermentation tank to 6.8, introducing steam, maintaining the pressure, continuously sterilizing for 0.5h, cooling to 28.5 ℃, introducing compressed air into the fermentation tank, operating for 540h, sampling, inspecting and discharging to the fermentation tank after the sampling is qualified;
preparation of S03 preparation
And (4) adding the rest components into the fermentation liquor obtained in the step (S02), crushing, and steaming out excessive water from the crushed material.
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