CN114145311B - Diflubenzuron particles, and preparation method and application thereof - Google Patents

Diflubenzuron particles, and preparation method and application thereof Download PDF

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Publication number
CN114145311B
CN114145311B CN202111454369.6A CN202111454369A CN114145311B CN 114145311 B CN114145311 B CN 114145311B CN 202111454369 A CN202111454369 A CN 202111454369A CN 114145311 B CN114145311 B CN 114145311B
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particles
diflubenzuron
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water
peroxide
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CN114145311A (en
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王海坤
张永丹
李硕
郭坤坤
黄银斌
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WUHAN HVSEN BIOTECHNOLOGY CO Ltd
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WUHAN HVSEN BIOTECHNOLOGY CO Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N63/00Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
    • A01N63/20Bacteria; Substances produced thereby or obtained therefrom
    • A01N63/22Bacillus
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01MCATCHING, TRAPPING OR SCARING OF ANIMALS; APPARATUS FOR THE DESTRUCTION OF NOXIOUS ANIMALS OR NOXIOUS PLANTS
    • A01M1/00Stationary means for catching or killing insects
    • A01M1/02Stationary means for catching or killing insects with devices or substances, e.g. food, pheronones attracting the insects
    • A01M1/023Attracting insects by the simulation of a living being, i.e. emission of carbon dioxide, heat, sound waves or vibrations
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/12Powders or granules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, 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
    • A01N47/08Biocides, 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
    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/34Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the groups, e.g. biuret; Thio analogues thereof; Urea-aldehyde condensation products
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N63/00Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
    • A01N63/20Bacteria; Substances produced thereby or obtained therefrom
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N63/00Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
    • A01N63/20Bacteria; Substances produced thereby or obtained therefrom
    • A01N63/27Pseudomonas
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N63/00Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
    • A01N63/30Microbial fungi; Substances produced thereby or obtained therefrom
    • A01N63/32Yeast
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01MCATCHING, TRAPPING OR SCARING OF ANIMALS; APPARATUS FOR THE DESTRUCTION OF NOXIOUS ANIMALS OR NOXIOUS PLANTS
    • A01M2200/00Kind of animal
    • A01M2200/01Insects
    • A01M2200/012Flying insects
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against 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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Abstract

The invention discloses a diflubenzuron particle, a preparation method and application thereof, wherein the diflubenzuron particle is prepared from the following raw materials in percentage by mass: 4 to 10 percent of diflubenzuron, 0.2 to 0.4 percent of adhesive, 0.5 to 1.5 percent of wetting agent, 1 to 3 percent of dispersing agent, 1 to 2 percent of anti-adhesive, 0.5 to 1 percent of carbon black, 0.5 to 0.8 percent of peroxide, 0.1 to 0.5 percent of microbial powder and the balance of water-soluble carrier. 1) The granules prepared by the invention have stable properties, high temperature resistance, difficult moisture absorption and agglomeration, rapid sinking when meeting water, and disintegration within 2 minutes to form a water-dispersible suspension; when the fly-swathing agent is directly and dried and scattered in a septic tank or a sewage ditch, particles sink under water, are rapidly disintegrated and dispersed, and are more easily contacted with fly larvae in excrement; the granule has simple process, is stirred and granulated at normal temperature, and is convenient for large-scale industrialized production; 2) Carbon black, peroxide and microbial powder are also added in the particles, and the insecticidal performance of the particles is greatly improved through the synergistic effect of the materials.

Description

Diflubenzuron particles, and preparation method and application thereof
Technical Field
The invention belongs to the technical field of preparation of mosquito killers, and particularly relates to a diflubenzuron granule, a preparation method and application thereof.
Background
The fly belongs to a fully allergic insect, the life history comprises four stages of eggs, larvae (maggots), pupae and adults (flies), the fertility is extremely strong, the sex is mature after the pupae is feathered into the adult fly for 3 to 5 days, and male and female flies mate and spawn. 1 female fly can spawn 100-200 eggs each time, each pair of female flies can reproduce 10-20 generations within one year, and 1 hundred million-2 hundred million offspring can be produced according to biological statistics measurement. Most of the fly, wild fly, black fly and the like are distributed in livestock farms. The domestic fly has great influence and harm to livestock and poultry cultivation, not only pollutes animal feed, drinking water and environmental sanitation, but also can disturb livestock and poultry rest, reduce animal production performance, and more seriously, can spread livestock and poultry diseases. It has been reported that flies can spread several tens of human and animal diseases such as cholera, typhoid, paratyphoid, dysentery, salmonellosis, escherichia coli disease, leptospirosis, etc., which are also great threats to human health.
Because the fly larvae (fly maggots) have light-shading property, when light irradiates in the daytime, the light always drills to the bottom of the excrement storage tank, the pupa body is harder before the pupa emerges into adults, the trouble is brought to the work of eliminating fly eggs, maggots and pupas, and the common spray, wettable powder is difficult to reach all parts in the deep part of the septic tank, so that the ideal effect cannot be achieved. The existing medicines for controlling fly maggots in livestock and poultry manure mainly comprise traditional pesticides such as organic phosphorus, amitraz and pyrethrin pesticides, insect growth regulator cyromazine and the like, and the medicines have the problems of high toxicity, high residue, poor efficacy or drug resistance and the like at present. Therefore, the animal husbandry in China is urgently required to search a novel and efficient fly-resistant medicament which is safe to people and livestock, low in toxicity and environment-friendly.
The diflubenzuron is a specific low-toxicity pesticide, and belongs to the benzoic acid phenyl urea pesticide. Because of its high safety to human, livestock and environment, it has less influence to natural enemies and has outstanding selectivity, and is called "third generation pesticide" and "ideal environmental chemical". It is neither nerve agent nor cholinesterase inhibitor, and has the main effects of inhibiting chitin synthesis of insect epidermis, and simultaneously has damage and destruction effects on endocrine and gland such as fat body, pharyngeal side body, etc., thereby preventing insect from smooth molting and metamorphosis. The main action mode of the diflubenzuron on pests is stomach toxicity and contact poisoning, the pests eat the diflubenzuron to cause accumulated poisoning, and larvae cannot form new epidermis, molting is difficult and pupation is blocked due to the lack of chitin; adults are difficult to eclosion and spawn; eggs do not develop normally and hatched larva cuticle lacks rigidity to die, thereby affecting the pest's entire generation. At present, the diflubenzuron preparation is not deeply developed in animal husbandry for controlling fly larvae in feces, and the development and application of the diflubenzuron preparation are beneficial to the popularization and application of novel high-efficiency and safe fly maggot resistant medicaments in the breeding industry, are beneficial to the improvement of food safety and breeding environment safety, and have important technical, economic and social benefits.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a diflubenzuron particle, and a preparation method and application thereof. The granules prepared by the invention have stable properties, high temperature resistance, difficult moisture absorption and agglomeration, rapid sinking when meeting water, and disintegration within 2 minutes to form a water-dispersible suspension; when the fly-swathing agent is directly and dried and scattered in a septic tank or a sewage ditch, particles sink under water, are rapidly disintegrated and dispersed, and are more easily contacted with fly larvae in excrement; the granule has simple process, is stirred and granulated at normal temperature, and is convenient for large-scale industrialized production.
It is an object of the present invention to provide a diflubenzuron particle.
The diflubenzuron particles are prepared from the following raw materials in percentage by mass: 4 to 10 percent of diflubenzuron, 0.2 to 0.4 percent of adhesive, 0.5 to 1.5 percent of wetting agent, 1 to 3 percent of dispersing agent, 1 to 2 percent of anti-adhesive, 0.5 to 1 percent of carbon black, 0.5 to 0.8 percent of peroxide, 0.1 to 0.5 percent of microbial powder and the balance of water-soluble carrier.
Further, the water-soluble carrier is water-soluble crystal particles, and the water-soluble crystal particles are selected from one or more of sodium chloride, potassium chloride, calcium chloride, magnesium chloride, sodium sulfate, potassium sulfate, calcium sulfate and magnesium sulfate.
Further, the binder is selected from one or more of microcrystalline cellulose, low-substituted hydroxypropyl cellulose, cross-linked polyvinylpyrrolidone, pregelatinized starch, and polyvinylpyrrolidone-K30.
Further, the wetting agent is selected from one or more of sodium dodecyl sulfate, alkyl sulfate, sulfonate, fatty acid ester sulfate, carboxylic acid soap, phosphate ester, polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene block copolymer.
Further, the dispersing agent is selected from one or more of ethanol, propylene glycol, glycerol and dimethyl sulfoxide.
Further, the anti-adhesion agent is micro silica gel.
Further, the peroxide is selected from one or more of sodium peroxide, magnesium peroxide, zinc peroxide, calcium peroxide and potassium peroxide.
Further, the microbial powder can produce aroma or lactic acid, for example, the microbial powder can be fungi (dry yeast, aroma-producing yeast E-36, aroma-enhancing effect, aroma-producing yeast, producing special fruit-flavored main sunflower lactone); may be actinomycetes (thermophilic actinomycetes, producing a pleasant aroma); bacteria (thermophilic bacteria, which produce pleasant fragrances; bacillus, ammonia nitrogen and amide nitrogen content increase; pseudomonas, which produce fragrance substances); pseudomonas is preferred.
The diflubenzuron particles are prepared from the following raw materials in percentage by mass: 4 to 10 percent of diflubenzuron, 0.2 to 0.4 percent of adhesive, 0.5 to 1.5 percent of wetting agent, 1 to 3 percent of dispersing agent, 1 to 2 percent of anti-adhesive, 0.5 to 1 percent of carbon black, 0.5 to 0.8 percent of peroxide, 0.1 to 0.5 percent of microbial powder and the balance of water-soluble carrier. Wherein, water-soluble crystal particles are taken as a carrier and an inner core, and the outer layer is adhered with the drug diflubenzuron, and the prepared particles sink under water and disintegrate and disperse rapidly, so that the drug is distributed to all corners of the excrement urinal and fully contacts with fly larvae; the adhesive is dissolved in the dispersing agent, so that on one hand, the adhesive effect is exerted, and on the other hand, the particles can exert a disintegrating effect when dissolved in water, so that the medicine is released rapidly; the dispersing agent enables the water-insoluble diflubenzuron to be uniformly dispersed; the wetting agent further promotes disintegration of the granules; the anti-adhesive agent makes the particles less prone to binding.
In addition, carbon black, peroxide and microbial powder are also added into the particles, wherein the carbon black mainly has the following three functions: 1) When the particles are applied to the excrement pool, the particles sink rapidly and are distributed to each corner of the excrement pool, and the particles are fully contacted with fly larvae; 2) Carbon black is a black substance, and has a certain attracting effect on fly larvae, so that the fly larvae are attracted to the periphery of particles and then killed; 3) Carbon black is a porous substance, so that microorganisms colonize the pores to grow and reproduce, and fragrance substances are continuously generated, thereby attracting fly larvae to the periphery of the particles to be eliminated; peroxide is quickly decomposed when meeting water, a large amount of oxygen is generated while heat is released, the heat has a certain attraction effect on fly larvae, the oxygen can be used for microorganism growth, propagation and utilization, and the insecticidal performance of the particles is greatly improved through the mutual synergistic effect among the materials.
Another object of the present invention is to provide a method for preparing the diflubenzuron particles.
The process for preparing the diflubenzuron particles as claimed in any one of the above, comprising the steps of:
s1, pretreatment of raw and auxiliary materials: after the diflubenzuron is crushed by air flow, the particles with the particle diameter of less than 15 mu m are not less than 80%, the binder and the wetting agent are crushed by a 100-120 mesh screen, the water-soluble crystal particles are crushed by a 30-50 mesh screen, and the water-soluble crystal particles are pretreated for standby;
S2, granulating: in the multifunctional granulator, firstly adding a water-soluble carrier, starting a pressure pump, spraying a dispersing agent under the pressure condition of 0.05-0.08 bar, and then stirring for 2-10 min under the condition of 50-80 r/min to uniformly mix materials, so that the surface of the water-soluble carrier uniformly covers the dispersing agent; adding the diflubenzuron, the adhesive, the wetting agent, the carbon black, the peroxide and the microbial powder into the multifunctional granulator, and continuously stirring and mixing for 2-10 min to enable the auxiliary materials to be adhered to the surface of the water-soluble carrier; finally adding an anti-adhesive agent, stirring and granulating for 5-15 min, and discharging;
S3, drying: drying the particles prepared in the step S2 for 1-2 hours at the temperature of 40-60 ℃;
S4, finishing: and (3) sieving the dried granules in the step (S3) with a 24-60-mesh screen to obtain the diflubenzuron granules.
It is a final object of the present invention to provide the use of diflubenzuron particles.
Use of the diflubenzuron particles of any one of the above in pest control.
Further, the diflubenzuron particles are used for killing fly larvae in a livestock and poultry farm manure pit and a sewage ditch.
Compared with the prior art, the invention has the following advantages:
1) The granules prepared by the invention have stable properties, high temperature resistance, difficult moisture absorption and agglomeration, rapid sinking when meeting water, and disintegration within 2 minutes to form a water-dispersible suspension; when the fly-swathing agent is directly and dried and scattered in a septic tank or a sewage ditch, particles sink under water, are rapidly disintegrated and dispersed, and are more easily contacted with fly larvae in excrement; the granule has simple process, is stirred and granulated at normal temperature, and is convenient for large-scale industrialized production;
2) The particle of the invention is also particularly added with carbon black, peroxide and microbial powder, the carbon black plays a multiple role, the peroxide is rapidly decomposed when meeting water, a large amount of oxygen is generated when the peroxide emits heat, the heat has a certain attraction effect on fly larvae, the oxygen can be used for microorganism growth and propagation, and the insecticidal performance of the particle is greatly improved through the mutual synergistic effect of the materials.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the preparation of the diflubenzuron particles of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments, and that all other embodiments obtained by persons of ordinary skill in the art without making creative efforts based on the embodiments in the present invention are within the protection scope of the present invention.
Conventional reagents and equipment used in the present invention are commercially available unless otherwise specified.
The performance index of the particles of the present invention was determined according to the method in literature (Ling Shihai. Solid preparation [ M ]. Chemical industry Press, 2003.) and is specifically as follows:
Wettability measurement method (graduated cylinder test method) of water dispersible granule: 500mL of 360 mg/L of hardness water is added into a 500mL graduated cylinder; 1.0g of sample was poured quickly into the measuring cylinder with a weighing dish, without stirring, a stopwatch was immediately recorded, and the time for 99% of the sample to sink into the bottom of the cylinder was recorded.
The dispersibility determination is carried out by a measuring cylinder mixing method of the water dispersible granule: adding 98mL of deionized water into a 100mL graduated cylinder, weighing 2g of sample, adding into the graduated cylinder, reversing for 10 times after about 2s each time and 60min, and standing for 24 hours after complete redispersion; after 24 hours the cylinder was inverted and the number of inversions to redisperse the sediment was recorded, with inversions below 10 times generally being considered acceptable.
The method for measuring the disintegration of the water dispersible granule comprises the following steps: sample particles 0.5g were added to a 100mL stoppered graduated cylinder containing 90mL distilled water at 25℃and then the cylinder was clamped in the middle, the cylinder mouth was stoppered, and the cylinder was rotated about the center at a speed of 8 revolutions until the sample completely disintegrated in water and the time was recorded.
Suspension rate measurement: 0.5000g of sample was weighed, slowly put into a beaker containing 50mL of standard hard water, rotated by hand for 2min at (30+ -1) deg.C, 120 times per minute, and the suspension was allowed to stand in a water bath at the same temperature for 13min. Then quantitatively transferring to a measuring cylinder preheated to 30 ℃, supplementing the measuring cylinder to 250mL by standard water with the temperature of (30+/-1) DEG C, and plugging the measuring cylinder. The cylinder was inverted 30 times in 1min, turned upside down 180 ° and returned to the original position once again. The measuring cylinder is vertically placed in a water bath, cannot vibrate, and has no direct sunlight. After 30min, 225mL (9/10) of the suspension was aspirated with a pipette over 10-15 s, taking care not to shake or agitate the sediment in the cylinder, ensuring that the tube was always a few millimeters below the liquid surface. The active ingredient content in the sample and in 25mL of suspension in the measuring cylinder was determined by high performance liquid chromatography. The suspension ratio is expressed as a percentage of the amount of the active ingredient suspended in water to the amount of the active ingredient in the base sample.
The content determination method of the diflubenzuron comprises the following steps: 0.25g of diflubenzuron sample is taken and dissolved in methanol to a volume of 50mL. The column was a C18 column, the mobile phase was methanol: acetonitrile: water=56:24:20 (v/v), flow rate: 2mL min -1; sample injection amount: 5. Mu.L; column temperature: 18 ℃; relative humidity 40%; detection wavelength: 254nm. The content of the diflubenzuron is measured by an external standard method, and the high performance liquid chromatograph is Shimadzu LC-20AD.
Example 1
The diflubenzuron particles are prepared from the following raw materials in percentage by mass: 8% of diflubenzuron, 0.3% of microcrystalline cellulose, 1.0% of sodium dodecyl sulfate, 2% of ethanol, 2% of micro-powder silica gel, 0.7% of carbon black, 0.7% of sodium peroxide and 0.3% of pseudomonas and 85% of sodium chloride.
The preparation method of the diflubenzuron particles comprises the following steps:
S1, pretreatment of raw and auxiliary materials: after the diflubenzuron is crushed by air flow, the particles below 15 mu m are not less than 80%, microcrystalline cellulose and sodium dodecyl sulfate are crushed and pass through a 100-120 mesh screen, sodium chloride is crushed and pass through a 30-50 mesh screen, and the pretreatment is finished for later use;
S2, granulating: in the multifunctional granulator, firstly adding sodium chloride, starting a pressure pump, spraying ethanol under the pressure condition of 0.05-0.08 bar, and then stirring for 2-10 min under the condition of 50-80 r/min to uniformly mix materials, so that the surface of the sodium chloride uniformly covers the ethanol; adding the diflubenzuron, microcrystalline cellulose, sodium dodecyl sulfate, carbon black, sodium peroxide and pseudomonas into the multifunctional granulator, and continuously stirring and mixing for 2-10 min to enable the auxiliary materials to be adhered to the surface of the sodium chloride; finally adding the superfine silica powder, stirring and granulating for 5-15 min, and discharging;
S3, drying: drying the particles prepared in the step S2 for 1-2 hours at the temperature of 40-60 ℃;
S4, finishing: and (3) sieving the dried granules in the step (S3) with a 24-60-mesh screen to obtain the diflubenzuron granules.
The content of the diflubenzuron particles is 7.88%, the yield is 93%, the wettability time is 8s, the disintegration time is 45s, the redispersibility is 4 times, and the suspension rate is 94.7%.
Example 2
The diflubenzuron particles are prepared from the following raw materials in percentage by mass: 10% of diflubenzuron, 0.4% of low-substituted hydroxypropyl cellulose, 1.5% of sulfonate, 3% of propylene glycol, 2% of micro silica gel, 1% of carbon black, 0.8% of zinc peroxide and 0.5% of bacillus, and 80.8% of magnesium chloride.
The preparation method of the diflubenzuron particles comprises the following steps:
S1, pretreatment of raw and auxiliary materials: after the diflubenzuron is crushed by air flow, the particles below 15 mu m are not less than 80%, the low-substituted hydroxypropyl cellulose and sulfonate are crushed by a 100-120 mesh screen, the magnesium chloride is crushed by a 30-50 mesh screen, and the pretreated product is reserved;
S2, granulating: firstly adding magnesium chloride into a multifunctional granulator, starting a pressure pump, spraying propylene glycol under the pressure condition of 0.05-0.08 bar, and stirring for 2-10 min under the condition of 50-80 r/min to uniformly mix materials, so that the surface of the magnesium chloride uniformly covers the propylene glycol; adding diflubenzuron, low-substituted hydroxypropyl cellulose, sulfonate, carbon black, zinc peroxide and bacillus into the multifunctional granulator, and continuously stirring and mixing for 2-10 min to enable the auxiliary materials to be adhered to the surface of magnesium chloride; finally adding the superfine silica powder, stirring and granulating for 5-15 min, and discharging;
S3, drying: drying the particles prepared in the step S2 for 1-2 hours at the temperature of 40-60 ℃;
S4, finishing: and (3) sieving the dried granules in the step (S3) with a 24-60-mesh screen to obtain the diflubenzuron granules.
The content of the diflubenzuron particles is 9.64%, the yield is 91%, the wettability time is 11s, the disintegration time is 1min, the redispersibility is 7 times, and the suspension rate is 93.5%.
Example 3
The diflubenzuron particles are prepared from the following raw materials in percentage by mass: 6% of diflubenzuron, 0.25% of crosslinked polyvinylpyrrolidone, 0.8% of fatty acid ester sulfate, 2% of glycerol, 2% of micro silica gel, 1% of carbon black, 0.8% of calcium peroxide and 86.65% of aroma-producing saccharomyces cerevisiae.
The preparation method of the diflubenzuron particles comprises the following steps:
S1, pretreatment of raw and auxiliary materials: after the diflubenzuron is crushed by air flow, particles with the particle diameter of less than 15 mu m are not less than 80%, the cross-linked polyvinylpyrrolidone and fatty acid ester sulfate are crushed by a 100-120 mesh screen, the potassium sulfate is crushed by a 30-50 mesh screen, and the pretreatment is finished for later use;
S2, granulating: in the multifunctional granulator, firstly adding potassium sulfate, starting a pressure pump, spraying glycerol under the pressure condition of 0.05-0.08 bar, and then stirring for 2-10 min under the condition of 50-80 r/min to uniformly mix materials, so that the surface of the potassium sulfate uniformly covers the glycerol; adding diflubenzuron, crosslinked polyvinylpyrrolidone, fatty acid ester sulfate, carbon black, calcium peroxide and aroma-controlling sporotrichum into the multifunctional granulator, and continuously stirring and mixing for 2-10 min to enable the auxiliary materials to be adhered to the surface of the potassium sulfate; finally adding the superfine silica powder, stirring and granulating for 5-15 min, and discharging;
S3, drying: drying the particles prepared in the step S2 for 1-2 hours at the temperature of 40-60 ℃;
S4, finishing: and (3) sieving the dried granules in the step (S3) with a 24-60-mesh screen to obtain the diflubenzuron granules.
The content of the diflubenzuron particles is 5.78%, the yield is 94%, the wettability time is 10s, the disintegration time is 52s, the redispersibility is 5 times, and the suspension rate is 96.4%.
Example 4
The diflubenzuron particles are prepared from the following raw materials in percentage by mass: 4% of diflubenzuron, 0.2% of pregelatinized starch, 0.5% of polyoxyethylene fatty alcohol ether, 1% of dimethyl sulfoxide, 1% of micro silica gel, 0.5% of carbon black, 0.5% of potassium peroxide and 0.1% of thermophilic actinomycetes, and 92.2% of magnesium sulfate.
The preparation method of the diflubenzuron particles comprises the following steps:
S1, pretreatment of raw and auxiliary materials: after the diflubenzuron is crushed by air flow, the particles with the particle diameter of less than 15 mu m are not less than 80%, pregelatinized starch and polyoxyethylene fatty alcohol ether are crushed by a 100-120-mesh screen, magnesium sulfate is crushed by a 30-50-mesh screen, and the pre-treatment is finished for later use;
S2, granulating: firstly adding magnesium sulfate into a multifunctional granulator, starting a pressure pump, spraying dimethyl sulfoxide under the pressure condition of 0.05-0.08 bar, and stirring for 2-10 min under the condition of 50-80 r/min to uniformly mix materials, so that the surface of the magnesium sulfate uniformly covers the dimethyl sulfoxide; adding the diflubenzuron, pregelatinized starch, polyoxyethylene fatty alcohol ether, carbon black, potassium peroxide and thermophilic actinomycetes into the multifunctional granulator, and continuously stirring and mixing for 2-10 min to enable the auxiliary materials to be adhered to the surface of the magnesium sulfate; finally adding the superfine silica powder, stirring and granulating for 5-15 min, and discharging;
S3, drying: drying the particles prepared in the step S2 for 1-2 hours at the temperature of 40-60 ℃;
S4, finishing: and (3) sieving the dried granules in the step (S3) with a 24-60-mesh screen to obtain the diflubenzuron granules.
The content of the diflubenzuron particles is 3.92%, the yield is 96%, the wettability time is 9s, the disintegration time is 38s, the redispersibility is 3 times, and the suspension rate is 93.7%.
Comparative example 1
The diflubenzuron particles were substantially identical to the preparation method of example 1, except that no carbon black was added in step S2.
Comparative example 2
The diflubenzuron particles were substantially identical to the preparation method of example 1, except that sodium peroxide was not added in step S2.
Comparative example 3
The diflubenzuron particles were substantially identical to the preparation method of example 1, except that in step S2, no Pseudomonas was added.
Example 5 stability test
5.1 High temperature test
The sample was exposed to the culture dish and left to stand at a high temperature of 60.+ -. 2 ℃ for 10 days, sampled on the 5 th and 10 th days, and examined for indexes such as properties, contents and fluidity, and compared with the data of the sample on the 0 th day, and the results are shown in Table 1 below:
TABLE 1 results of high temperature test
As can be seen from the data in the table, the properties of the diflubenzuron particles in examples 1-4 are not changed in the high-temperature test period, the diflubenzuron particles have no caking phenomenon, have good fluidity and no obvious change in content, and all indexes meet the requirements, so that the results show that the diflubenzuron particles prepared by the invention are very stable at high temperature.
5.2 Accelerated test
In order to determine the stability of the preparation, according to the requirements of the "veterinary drug stability test technical Specification", an acceleration test under the following conditions is specially set, the prepared granules of examples 1 to 4 are placed under the conditions of 40+/-2 ℃ and 75+/-5% relative humidity for 6 months, and are sampled once in 0, 1,2, 3 and 6 months, and are respectively examined according to stability key examination items, and the performance indexes such as properties, content and fluidity are examined, and the results are shown in the following tables 2 to 5:
TABLE 2 accelerated stability test results of diflubenzuron particles in example 1
Time of Content (% w/w) Appearance characteristics Fluidity of the product
0 Month 7.88 White-like dispersion particles Good (good)
1 Month 7.81 White-like dispersion particles Good (good)
2 Months of 7.79 White-like dispersion particles Good (good)
3 Months of 7.83 White-like dispersion particles Good (good)
6 Months of 7.80 White-like dispersion particles Good (good)
TABLE 3 accelerated stability test results of diflubenzuron particles in example 2
Time of Content of Appearance characteristics Fluidity of the product
0 Month 9.64 White-like dispersion particles Good (good)
1 Month 9.56 White-like dispersion particles Good (good)
2 Months of 9.58 White-like dispersion particles Good (good)
3 Months of 9.57 White-like dispersion particles Good (good)
6 Months of 9.57 White-like dispersion particles Good (good)
TABLE 4 accelerated stability test results for diflubenzuron particles in example 3
Time of Content of Appearance characteristics Fluidity of the product
0 Month 5.78 White-like dispersion particles Good (good)
1 Month 5.73 White-like dispersion particles Good (good)
2 Months of 5.74 White-like dispersion particles Good (good)
3 Months of 5.69 White-like dispersion particles Good (good)
6 Months of 5.68 White-like dispersion particles Good (good)
TABLE 5 accelerated stability test results for diflubenzuron particles in example 4
Time of Content of Appearance characteristics Fluidity of the product
0 Month 3.92 White-like dispersion particles Good (good)
1 Month 3.90 White-like dispersion particles Good (good)
2 Months of 3.88 White-like dispersion particles Good (good)
3 Months of 3.87 White-like dispersion particles Good (good)
6 Months of 3.86 White-like dispersion particles Good (good)
As can be seen from the data in tables 2 to 5, the properties of the diflubenzuron particles in examples 1 to 4 are not changed in the accelerated stability test period, the diflubenzuron particles have no caking phenomenon, good fluidity and no obvious change in content, and various indexes meet the requirements, so that the results show that the diflubenzuron particles prepared by the invention have better stability.
Example 6 test of the effect of the diflubenzuron particles on killing fly larvae in feces
A test is carried out by selecting a manure pit of a large pig farm in Guangdong province, according to the application amount of 15g/m 2, the diflubenzuron particles prepared in examples 1-4 and comparative examples 1-3 are uniformly put into a manure pit, meanwhile, a blank control is arranged, the drug is taken from day 6, only one time is taken every day, the manure is collected in the early treatment period (days 1, 3 and 5), the drug use period (days 6, 8, 10 and 12) and the drug stopping period (days 13, 15, 17 and 19), the collection points are uniformly distributed, the manure at different sampling points is mixed and uniformly stirred, and the total sampling amount of each time is 1L.
The evaluation method comprises the following steps: the samples were divided into 6 portions and placed in 6 200mL beakers, the cup mouth was closed with gauze, and the beakers were placed in an environment with a temperature of 25 ℃ and a humidity of about 60% for 3 weeks, during which the occurrence of live and dead maggots were counted, and the average mortality of the fly maggots in the 6 beakers of the samples was calculated, and the mortality = dead fly maggots/(dead maggots + live maggots) ×100%, the results are shown in table 6 below:
TABLE 6 mortality of fly larvae in feces (%)
For 1 day For 3 days For 5 days For 6 days For 8 days For 10 days For 12 days 13 Days For 15 days For 17 days For 19 days
Example 1 5 6 7 100 100 100 100 100 70 30 18
Example 2 7 5 8 100 100 100 100 100 60 25 15
Example 3 7 5 6 100 100 100 100 100 80 20 12
Example 4 5 7 6 100 100 100 100 100 65 23 17
Comparative example 1 6 8 7 85 84 83 85 82 55 15 9
Comparative example 2 7 5 6 90 91 92 91 93 60 18 12
Comparative example 3 5 7 8 92 91 92 92 91 61 17 10
Blank control 6 7 6 8 7 9 6 7 8 7 6
As can be seen from the results in the table, the insecticidal urea particles prepared in examples 1-4 have good effect of killing fly maggots, and the insecticidal performance of the insecticidal urea particles prepared in the invention is greatly improved when the fly maggots are killed to 100% in the period of using the insecticide (days 6,8, 10 and 12);
Comparative example 1 differs from example 1 in that no carbon black was added in step S2. As a result, it was found that during the period of administration (days 6, 8, 10, 12), there was a significant drop in the fly larvae killing effect, because the carbon black of the present invention has mainly the following three effects: 1) When the particles are applied to the excrement pool, the particles sink rapidly and are distributed to each corner of the excrement pool, and the particles are fully contacted with fly larvae; 2) Carbon black is a black substance, and has a certain attracting effect on fly larvae, so that the fly larvae are attracted to the periphery of particles and then killed; 3) Carbon black is a porous substance, so that microorganisms colonize the pores to grow and reproduce, and fragrance substances are continuously generated, thereby attracting fly larvae to the periphery of the particles to be eliminated; therefore, if carbon black is not added, on one hand, particles cannot uniformly permeate into all corners of the septic tank, and meanwhile, fly maggots cannot be quickly attracted to the vicinity of the particles to be killed, so that some fly maggots in the septic tank are not killed, and the importance of the carbon black is further illustrated;
Comparative example 2 and comparative example 3 differ from example 1 in that sodium peroxide or pseudomonas is not added in step S2. As a result, it was found that the effect of killing fly larvae was reduced to some extent during the period of administration (days 6, 8, 10, 12) because sodium peroxide was decomposed rapidly by water to give off heat and a large amount of oxygen was generated, and the heat was also attracted to fly larvae to some extent, and oxygen was available for growth and reproduction of Pseudomonas, and if sodium peroxide or Pseudomonas were not added, the trapping of fly larvae was reduced and a part of fly larvae survived, and therefore the effect of killing fly larvae was reduced to some extent.
In conclusion, the granules prepared by the invention have stable properties, high temperature resistance, difficult moisture absorption and agglomeration, rapid sinking when meeting water, and disintegration within 2 minutes to form a water-dispersible suspension; when the fly-swathing agent is directly and dried and scattered in a septic tank or a sewage ditch, particles sink under water, are rapidly disintegrated and dispersed, and are more easily contacted with fly larvae in excrement; the granule has simple process, is stirred and granulated at normal temperature, and is convenient for large-scale industrialized production.
The above examples are only specific embodiments of the present invention for illustrating the technical solution of the present invention, but not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the foregoing examples, it will be understood by those skilled in the art that the present invention is not limited thereto: any person skilled in the art may modify or easily conceive of the technical solution described in the foregoing embodiments, or perform equivalent substitution of some of the technical features, while remaining within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention, and are intended to be included in the scope of the present invention.

Claims (9)

1. The diflubenzuron particles are characterized by being prepared from the following raw materials in percentage by mass: 4 to 10 percent of diflubenzuron, 0.2 to 0.4 percent of adhesive, 0.5 to 1.5 percent of wetting agent, 1 to 3 percent of dispersing agent, 1 to 2 percent of anti-adhesive, 0.5 to 1 percent of carbon black, 0.5 to 0.8 percent of peroxide, 0.1 to 0.5 percent of microbial powder and the balance of water-soluble carrier;
the peroxide is selected from one or more of sodium peroxide, magnesium peroxide, zinc peroxide, calcium peroxide and potassium peroxide;
the microorganism is Pseudomonas, bacillus, sporobusta or thermophilic actinomycetes.
2. The diflubenzuron particles of claim 1, wherein the water soluble carrier is a water soluble crystalline particle selected from one or more of sodium chloride, potassium chloride, calcium chloride, magnesium chloride, sodium sulfate, potassium sulfate, calcium sulfate and magnesium sulfate.
3. The diflubenzuron particles of claim 1, wherein the binder is selected from one or more of microcrystalline cellulose, low substituted hydroxypropyl cellulose, cross-linked polyvinylpyrrolidone, pregelatinized starch, and polyvinylpyrrolidone-K30.
4. The avermectin particles of claim 1, wherein the wetting agent is selected from one or more of alkyl sulfates, sulfonates, fatty acids, fatty acid ester sulfates, carboxylic acid soaps, phosphate esters, polyoxyethylene alkylphenol ethers, polyoxyethylene fatty alcohol ethers, and polyoxyethylene polyoxypropylene block copolymers.
5. The diflubenzuron particles of claim 1, wherein the dispersant is selected from one or more of ethanol, propylene glycol, glycerol and dimethyl sulfoxide.
6. The diflubenzuron particles of claim 1, wherein the anti-blocking agent is a colloidal silica.
7. The diflubenzuron particles of claim 1, wherein the microbial powder is capable of producing a fragrance or lactic acid.
8. A process for the preparation of the diflubenzuron particles as claimed in any one of claims 1 to 7, comprising the steps of:
S1, pretreatment of raw and auxiliary materials: after the diflubenzuron is crushed by air flow, the particles with the particle diameter of less than 15 mu m are not less than 80%, the binder and the wetting agent are crushed by a 100-120 mesh screen, the water-soluble crystal particles are crushed by a 30-50 mesh screen, and the water-soluble crystal particles are pretreated for standby;
S2, granulating: in the multifunctional granulator, firstly adding a water-soluble carrier, starting a pressure pump, spraying a dispersing agent under the pressure condition of 0.05-0.08 bar, and then stirring for 2-10 min under the condition of 50-80 r/min to uniformly mix materials, so that the surface of the water-soluble carrier uniformly covers the dispersing agent; adding the diflubenzuron, the adhesive, the wetting agent, the carbon black, the peroxide and the microbial powder into the multifunctional granulator, and continuously stirring and mixing for 2-10 min to enable the auxiliary materials to be adhered to the surface of the water-soluble carrier; finally adding an anti-adhesive agent, stirring and granulating for 5-15 min, and discharging; the microorganism is pseudomonas, bacillus, aroma sporotrichum or thermophilic actinomycetes;
S3, drying: drying the particles prepared in the step S2 for 1-2 hours at the temperature of 40-60 ℃;
S4, finishing: and (3) sieving the dried granules in the step (S3) with a 24-60-mesh screen to obtain the diflubenzuron granules.
9. Use of the diflubenzuron particles as claimed in any one of claims 1 to 7 for fly maggot killing.
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1679392A (en) * 2004-12-08 2005-10-12 西北农林科技大学无公害农药研究服务中心 Preparation method of pesticide water dispersible soft particles
WO2007046650A1 (en) * 2005-10-22 2007-04-26 Se Joon Park Microorganisms having bad smell removal activity of organic waste and use thereof
KR100847905B1 (en) * 2007-05-19 2008-07-23 백도현 Deodorizer of domestic animal
CN102550578A (en) * 2010-12-30 2012-07-11 安阳市安林生物化工有限责任公司 Emamectin benzoate-diflubenzuron compound pesticide
CN105028461A (en) * 2015-08-24 2015-11-11 江阴苏利化学股份有限公司 Insecticidal composition containing diflubenzuron and deltamethrin and application thereof
CN107372590A (en) * 2017-06-26 2017-11-24 安徽省黄淮兽药有限公司 A kind of aquaculture insecticide and preparation method thereof
CN108902135A (en) * 2018-06-15 2018-11-30 刘长德 A kind of diflubenzuron urea granules and preparation method thereof
CN110122501A (en) * 2019-06-14 2019-08-16 青岛润农化工有限公司 A kind of diflubenzuron water dispersible granules and preparation method thereof
CN111903701A (en) * 2020-06-28 2020-11-10 武汉轻工大学 Fly-killing premix for animals and preparation method and application thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1679392A (en) * 2004-12-08 2005-10-12 西北农林科技大学无公害农药研究服务中心 Preparation method of pesticide water dispersible soft particles
WO2007046650A1 (en) * 2005-10-22 2007-04-26 Se Joon Park Microorganisms having bad smell removal activity of organic waste and use thereof
KR100847905B1 (en) * 2007-05-19 2008-07-23 백도현 Deodorizer of domestic animal
CN102550578A (en) * 2010-12-30 2012-07-11 安阳市安林生物化工有限责任公司 Emamectin benzoate-diflubenzuron compound pesticide
CN105028461A (en) * 2015-08-24 2015-11-11 江阴苏利化学股份有限公司 Insecticidal composition containing diflubenzuron and deltamethrin and application thereof
CN107372590A (en) * 2017-06-26 2017-11-24 安徽省黄淮兽药有限公司 A kind of aquaculture insecticide and preparation method thereof
CN108902135A (en) * 2018-06-15 2018-11-30 刘长德 A kind of diflubenzuron urea granules and preparation method thereof
CN110122501A (en) * 2019-06-14 2019-08-16 青岛润农化工有限公司 A kind of diflubenzuron water dispersible granules and preparation method thereof
CN111903701A (en) * 2020-06-28 2020-11-10 武汉轻工大学 Fly-killing premix for animals and preparation method and application thereof

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