CN107372516B - Sanitary insecticidal granules and preparation method thereof - Google Patents
Sanitary insecticidal granules and preparation method thereof Download PDFInfo
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- CN107372516B CN107372516B CN201710616294.4A CN201710616294A CN107372516B CN 107372516 B CN107372516 B CN 107372516B CN 201710616294 A CN201710616294 A CN 201710616294A CN 107372516 B CN107372516 B CN 107372516B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- 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
- A01N25/12—Powders or granules
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
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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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/14—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing aromatic radicals
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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
- A01N63/00—Biocides, 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
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Abstract
The invention relates to a sanitary insecticidal granule and a preparation method thereof, wherein the sanitary insecticidal granule comprises the following components in parts by weight: 0.1-10% of active component A, 0.1-40% of active component B, 0.2-20% of solvent, 0.1-5.0% of emulsifier, 0.1-5.0% of dispersant, 0.1-5.0% of slow-release film-forming agent, 0.1-5.0% of quick-release film-forming agent, 0.1-10% of adsorbent and porous carrier which are complemented to 100%. The active component A is slow-acting medicament Bti or pyriproxyfen of Bacillus thuringiensis subspecies Israel; the active component B is quick-acting neurotoxic medicament fenthion, parathion, chlorpyrifos, pirimiphos-methyl, abamectin, ivermectin and emamectin benzoate selected from the following group; the active ingredient A is used for being adsorbed in the porous carrier, and the active ingredient B is wrapped outside the porous carrier; the slow-release film-forming agent is a hydrophobic high-molecular polymer; the quick-release film-forming agent is a water-soluble high-molecular polymer. The special slow-release film-forming agent and the quick-release film-forming agent selected by the invention are particularly further compounded in a special proportion, and the compound slow-release film-forming agent and the compound quick-release film-forming agent have excellent compatibility with corresponding insecticidal active ingredients, and can play a better role in quick release and slow release.
Description
Technical Field
The invention relates to the field of sanitary insecticides, in particular to a composition for sanitary killing of mosquito and fly larvae and application thereof.
Background
The Bacillus thuringiensis Israeli subspecies (Bti) is a Bacillus thuringiensis subspecies with earlier research time, deeper research content and wider application range, and is widely used for controlling the quantity of mosquitoes and flies as a biological mosquito killer. Bti is a gram-positive aerobic bacillus capable of forming spores, can produce a crystal protein, becomes a toxic protein after being ingested by larvae, leads to cell membrane perforation and finally death by combining with special receptors on epithelial cell walls, and can secrete various active ingredients such as thuringiensis, exotoxin, chitinase and the like, has a plurality of action sites and cannot generate drug resistance.
The specific action mechanism of the juvenile hormone analogue pyriproxyfen is not well understood at present, but the pyriproxyfen has the characteristics of high efficiency, safety and long duration, can interfere ecdysis and reproduction, thoroughly blocks the eclosion of larvae, and has almost no drug resistance.
Organophosphorus insecticides such as fenthion, parathion, chlorpyrifos and pirimiphos-methyl are acetylcholinesterase inhibitors, macrolide insecticides such as abamectin, ivermectin and emamectin benzoate are r-aminobutyric acid inhibitors, and the two are nerve toxicants, have high action speed, can inhibit the activity of larvae within 24 hours and die quickly.
For a long time, the dosage forms for preventing and controlling the sanitary mosquito and fly larvae are mainly single preparation types such as single-dose granules, missible oil, emulsion in water, wettable powder and the like, and the organophosphorus insecticide or macrolide insecticide is used independently, so that the defects of short lasting period and quick development of drug resistance exist although the insecticidal speed is high; and the insect growth regulator used alone has long lasting period and low drug resistance, but can not quickly reduce the population density.
In the granule part, the prior art also does not relate to the granule that two-layer set up, wherein CN201510456298.1 discloses a sustained and controlled release pesticide granule, its structure includes inside and outside two-layer structure, its core part is the sustained release granule, and the quick release layer of cladding outside the sustained release layer, the active ingredient of pesticide is organic phosphorus class, nicotine class etc., it wraps up the active ingredient of pesticide in the sustained release nuclear layer (diameter 1.2-2 mm) first, adopt the residual material to throw the circle with the sustained release nuclear layer and form the quick release layer (the layer thickness is 0.3-0.5 mm) afterwards, namely in this prior art, do not distinguish the active ingredient of different release layers, select different sustained release film formers to the controlled release speed of different release layers more. CN201610353235.8 discloses a slow-release pesticide granule and a preparation method thereof, wherein 3 active ingredient layers are arranged, the active ingredients of the pesticide in each layer can be the same or different, different cross-linking agents are adopted in each layer, the cross-linking agent in the first layer is a water-soluble high polymer such as polyvinylpyrrolidone, the cross-linking agent in the second layer is cellulose or cellulose salt such as sodium carboxymethylcellulose, carboxyethyl cellulose, methyl cellulose and the like, the cross-linking agent in the third layer is borax, and the release of the active ingredients of the pesticide is promoted by adopting different cross-linking agents and setting a proper proportion in each layer, so that quick-acting, medium-acting and long-acting release is finally achieved.
It can be seen that the prior art, although it relates to the presence of immediate release and sustained release layers in granules, does not concern which active ingredient is used in each release layer, let alone the use of different adjuvants for different active ingredients.
The applicant finds that different quick-acting medicaments and slow-acting medicaments are matched with respective adaptive specific film forming agents and are compounded in granules, so that the quick-acting medicaments can quickly exert a quick-killing effect, the dosage is reduced, and the heavy mouth density is quickly reduced; the slow-release agent can exert the slow-release effect for a longer time, thoroughly kill residual larvae or block the emergence of the residual larvae, reduce the development of the drug resistance of the organophosphorus pesticide or macrolide pesticide, is convenient to apply and realizes more ideal insecticidal effect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provide the sanitary insecticidal granules which can simultaneously achieve the quick-release effect and the slow-release effect according to the needs, realize the effects of simultaneously and quickly killing mosquito and fly larvae to reduce the population density, inhibiting the growth of the larvae for a long time, thoroughly killing residual larvae or preventing the residual larvae from feathering, and reducing the drug resistance.
In order to achieve the purpose of the invention, the invention provides a sanitary insecticidal granule which is characterized by comprising the following components in parts by weight:
active ingredient A0.1-10%
0.1 to 10 percent of active ingredient B
0.2 to 20 percent of solvent
0.1 to 5.0 percent of emulsifier
0.1 to 5.0 percent of dispersant
0.1 to 5.0 percent of slow-release film-forming agent
0.1 to 5.0 percent of quick-release film-forming agent
0.1-10% of adsorbent
The porous carrier is complemented to 100%
The active component A is slow-acting medicament Bti or pyriproxyfen of Bacillus thuringiensis subspecies Israel; the active component B is quick-acting neurotoxic medicament fenthion, parathion, chlorpyrifos, pirimiphos-methyl, abamectin, ivermectin and emamectin benzoate selected from the following group; the active ingredient A is used for being adsorbed in the porous carrier, and the active ingredient B is wrapped outside the porous carrier;
the slow-release film-forming agent is a hydrophobic high-molecular polymer; the film-forming agent is selected from the following components with good film-forming property, excellent slow-release performance, proper viscosity and strong film-forming firmness: one or more of polyvinyl acetate, polybutyl acrylate, styrene/vinyl acetate copolymer, styrene/vinyl acetate/butyl acrylate copolymer and styrene/acrylamide/butyl acrylate copolymer;
the quick-release film-forming agent is a water-soluble high-molecular polymer; the film-forming agent is selected from the following components with good film-forming property, excellent disintegration property, proper viscosity and strong film-forming firmness: one or more of hydroxyethyl cellulose, pregelatinized starch, sodium carboxymethyl starch, acacia and polyvinyl alcohol.
Preferably, the active ingredient B is fenthion, parathion or ivermectin;
preferably, the slow-release film-forming agent is one or two of polyvinyl acetate, styrene/vinyl acetate/butyl acrylate copolymer or styrene/acrylamide/vinyl acetate copolymer; more preferably, the sustained-release film-forming agent is a composite sustained-release film-forming agent of polyvinyl acetate and styrene/acrylamide/butyl acrylate copolymer in a weight ratio of 1:2-4, and more preferably the weight ratio of the two is 1: 3.
Preferably, the quick-release film-forming agent is one or more of acacia, sodium carboxymethyl starch and polyvinyl alcohol; more preferably, the quick-release film forming agent is a composite quick-release film forming agent of sodium carboxymethyl starch and polyvinyl alcohol in a weight ratio of 1:1-3, and more preferably the weight ratio of the two is 1: 1.5.
The porous carrier is selected from one or more of attapulgite particles, volcanic rock particles, red brick particles, coal gangue particles, medical stone particles, zeolite particles, corncob particles, walnut shell particles and the like with better adsorption performance, and is preferably any one of the attapulgite particles, the volcanic rock particles and the corncob particles.
The solvent is selected from aromatic solvent oil, C6-C30 isoparaffin or dearomatized solvent oil; monoester solvents such as methyl laurate, methyl oleate, isopropyl myristate, isooctyl stearate, benzyl acetate and the like; diester solvents such as dimethyl adipate, diisopropyl adipate, diethyl maleate and dibutyl malonate; tri-ester solvents such as tributyl phosphate, tributyl citrate, acetyl tributyl citrate, and the like; amide solvents such as N, N-dimethyl pelargonamide and N, N-dimethyl caprylamide; one or more ketone solvents such as cyclohexanone, methyl isobutyl ketone, isophorone, etc., preferably monoester, diester or triester solvents with low toxicity, no odor and no irritation.
The emulsifier is selected from one or more of calcium dodecyl benzene sulfonate, diisooctyl sulfosuccinate sodium salt, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, phenethylphenol polyoxyethylene ether and ethylene oxide propylene oxide block copolymer, and is preferably a negative and nonionic compound in the calcium dodecyl benzene sulfonate, the fatty alcohol polyoxyethylene ether, the alkylphenol polyoxyethylene ether and the ethylene oxide propylene oxide block copolymer;
the dispersant is selected from one or more of phenethylphenol polyoxyethylene ether and phosphate ester or salt thereof, polycarboxylate, alkyl naphthalene sulfonate formaldehyde condensate and lignosulfonate, preferably (alkyl) naphthalene sulfonate formaldehyde condensate and lignosulfonate;
the adsorbent is selected from one or more of white carbon black, attapulgite, bentonite, diatomite and the like, and preferably white carbon black or attapulgite.
The sanitary insecticidal granule composition and the preparation method thereof are characterized by comprising the following steps:
a. preparation of an adsorption core: dissolving the active component A in 0.1-10 wt% of solvent according to the formula proportion, adding 0.05-2.5 wt% of emulsifier and 0.05-2.5 wt% of dispersant, stirring, adding the above liquid into porous carrier, adsorbing, adding slow-release film-forming agent, coating in a roller granulator, and drying to obtain slow-release core particles;
b. coating a quick-acting medicament: mixing the active ingredient B with the rest solvent, emulsifier and dispersant, adsorbing with the adsorbent to obtain powder, mixing with the quick-release type film-forming agent, and rolling coating with the above dried delayed-release type core granule in a roller granulator;
c. and drying or airing again to obtain the granules.
Further, the present invention provides the use of the sanitary insecticidal granule for controlling sanitary pests, wherein the sanitary pests are wigglers, fly larvae, preferably wigglers.
Regarding the principle explanation: the applicant finds that two effective components with completely different action mechanisms are compounded in the same preparation, wherein one of the effective components is a specific bacillus thuringiensis subspecies or pyriproxyfen which has slow action speed, high long-term killing rate and extremely low drug resistance risk; the other is an organophosphorus or macrolide medicament with higher action speed and obvious density reduction rate within 24 hours; firstly, the drug resistance risk of organophosphorus or macrolide medicaments is greatly reduced by compounding the two medicaments, and the aim of quickly reducing the density of pests is fulfilled; secondly, the applicant discovers through a large amount of researches that when the specific sustained-release medicament and the specific sustained-release film forming agent are combined to prepare the inner core particle, the compatibility of the two is better, and the better sustained-release effect can be achieved by adopting other film forming agents in the production practice; meanwhile, when the specific quick-release medicament is combined with the specific quick-release film-forming agent, the specific quick-release medicament and the specific quick-release film-forming agent have excellent compatibility, and can achieve better quick-release effect in production practice compared with other film-forming agents.
Compared with the prior art, the invention has the beneficial effects that:
(1) the pesticide active ingredients with different physical and chemical properties are adopted, so that the pesticide active ingredients and the pesticide compound greatly reduce the drug resistance risk of organic phosphorus or macrolide medicaments on the one hand, and on the other hand, the pesticide compound achieves the aim of quickly reducing the density of pests and also has a slow release effect
(2) Compared with a juvenile hormone analogue or a single bacillus thuringiensis preparation, the compound has a faster insecticidal speed, and compared with an organophosphorus or macrolide single preparation, the compound has a longer lasting period;
(3) the porous carrier with better adsorption performance is preferred, the slow release type medicament is better adsorbed and controlled to release, and the lasting period is prolonged.
(4) The invention also prefers a specific hydrophobic slow-release film forming agent to coat the porous granules adsorbing the slow-release medicament, realizes longer-acting controlled release, and simultaneously coats the quick-acting medicament on the outer layer without being adsorbed into the interior by the porous material to influence the effect of quick action.
(5) The quick-acting medicament is coated by preferably selecting the specific hydrophilic quick-release film-forming agent, so that the quick-acting medicament is released more quickly, and the density reduction speed of mosquito and fly larvae is accelerated.
(6) Adds a new compound composition and a new formulation for the field of domestic sanitary insecticide, has obvious drug effect and can be widely popularized and applied.
(7) The special slow-release film-forming agent and the quick-release film-forming agent selected by the invention are particularly further compounded in a special proportion, and the compound slow-release film-forming agent and the compound quick-release film-forming agent have excellent compatibility with corresponding insecticidal active ingredients, and can play a better role in quick release and slow release.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
First, preparation example
Preparation example 1:
dissolving 0.5g of pyriproxyfen in 2.5g of methyl oleate, adding an emulsifier (0.2 g of calcium dodecyl benzene sulfonate and 0.3g of fatty alcohol-polyoxyethylene ether) for stirring uniformly, dispersing with a proper amount of water containing 0.5g of a naphthalenesulfonate formaldehyde condensate as a dispersing agent, carrying out full rolling adsorption on the liquid in a roller granulator for 30min by using a proper amount of attapulgite particles, then adding a diluent containing 1.0g of styrene/acrylamide/butyl acrylate copolymer, carrying out full rolling coating for 30min, and drying to obtain slow-release core particles for later use;
dissolving 4.5g of fenthion in 1.5g of diethyl adipate, adding an emulsifier (0.5 g of calcium dodecyl benzene sulfonate and 1.5g of alkylphenol polyoxyethylene), uniformly stirring, uniformly mixing with 1.0g of polycarboxylate dispersing agent dissolved in a proper amount of water, adsorbing by using 5g of white carbon black, uniformly mixing with a diluent containing 2.0g of polyvinyl alcohol, fully rolling and coating the mixture with the slow-release type core particles in a roller granulator for 30min, and drying to obtain 100g of 5% pyriproxyfen-fenthion granules.
Preparation example 2:
dissolving 80000IU/ml of Bacillus thuringiensis Israeli subspecies suspension agent 0.25ml in a proper amount of water containing 1.0g of lignosulfonate dispersant, fully rolling and adsorbing the liquid in a roller granulator for 30min by using a proper amount of volcanic rock particles, then adding diluent containing styrene/acrylamide/butyl acrylate copolymer 1.5g, fully rolling and coating for 30min, and drying to obtain slow-release core particles for later use;
dissolving 0.1g of ivermectin in 1.0g of dimethyl adipate, adding an emulsifier (0.2 g of fatty alcohol-polyoxyethylene ether and 0.4g of ethylene oxide-propylene oxide segmented copolymer), uniformly stirring, uniformly mixing with 0.5g of naphthalenesulfonate formaldehyde condensate dispersant dissolved in a proper amount of water, adsorbing by 1.0g of white carbon black, uniformly mixing with 0.5g of diluent containing sodium carboxymethyl starch, fully rolling and coating the mixture with the slow-release type core particles in a roller granulator for 30min, and drying to obtain 100g of insecticidal granules containing 200IU/g of bacillus thuringiensis and 0.1% of ivermectin.
Preparation example 3:
dissolving 1.0g of pyriproxyfen in 2.0g of diisopropyl adipate, adding an emulsifier (0.1 g of calcium dodecyl benzene sulfonate and 0.4g of ethylene oxide propylene oxide block copolymer) for stirring uniformly, dispersing with a proper amount of water containing 1.0g of phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt serving as a dispersing agent, carrying out full rolling adsorption on the liquid in a roller granulator for 30min by using a proper amount of corncob particles, then adding a diluent containing 2.0g of styrene/acrylamide/butyl acrylate copolymer, carrying out full rolling coating for 30min, and drying to obtain slow-release type corncob particles for later use;
dissolving 1.0g of parathion in 1.0g of tributyl phosphate, adding an emulsifier (0.2 g of calcium dodecyl benzene sulfonate and 0.8g of castor oil polyoxyethylene ether) for stirring uniformly, uniformly mixing with 0.2g of lignosulfonate dispersant dissolved in a proper amount of water, adsorbing with 2.0g of white carbon black, uniformly mixing with a diluent containing 0.2g of Arabic gum, fully rolling and coating the mixture with the slow-release type core particles in a roller granulator for 30min, and drying to obtain 100g of 2% pyriproxyfen-parathion granules.
Preparation example 4:
dissolving 0.4g of pyriproxyfen in 2.0g of tributyl citrate, adding an emulsifier (0.2 g of calcium dodecyl benzene sulfonate and 0.4g of alkylphenol ethoxylates) for uniformly stirring, dispersing with a proper amount of water containing 0.8g of dispersant lignosulfonate, fully rolling and adsorbing the liquid with a proper amount of attapulgite particles for 30min in a roller granulator, then adding 5.0g of 40% polyvinyl acetate emulsion, fully rolling and coating for 30min, and drying to obtain slow-release core particles for later use;
dissolving ivermectin 0.1g in diethyl adipate 1.5g, adding an emulsifier (calcium dodecyl benzene sulfonate 0.5g and alkylphenol polyoxyethylene ether 1.5 g), stirring uniformly, mixing uniformly with a proper amount of water-soluble polycarboxylate dispersing agent 0.5g, adsorbing with white carbon black 5g, mixing uniformly with a diluent containing polyvinyl alcohol 1.0g, fully rolling and coating with the slow-release type core particles in a roller granulator for 30min, and drying to obtain 100g of 0.5% pyriproxyfen/ivermectin granules.
Preparation example 5: the same procedure as in preparation example 1 was repeated except that the sustained-release active ingredient was of the Israeli subspecies thuringiensis;
preparation example 6: the same preparation example 1 was prepared except that the immediate release type active ingredient was chlorpyrifos;
preparation example 7: the same procedure as in preparation example 1 was repeated except that the immediate release type active ingredient was pirimiphos-methyl;
preparation example 8: the preparation example 1 is the same except that the quick-release active ingredient is abamectin;
preparation example 9: the preparation example 1 is the same except that the quick-release active ingredient is emamectin benzoate;
preparation example 10: the film-forming agent for removing the slow release is 1:2, the preparation example 1 is the same except for the composite slow-release film-forming agent of polyvinyl acetate and styrene/acrylamide/butyl acrylate copolymer;
preparation example 11: the film-forming agent for removing the slow release is 1:4, except for the composite slow-release film-forming agent of polyvinyl acetate and styrene/acrylamide/butyl acrylate copolymer, the preparation example 1 is the same;
preparation example 12: the film-forming agent for removing the slow release is 1:3, the preparation example 1 is the same except for the composite slow-release film-forming agent of polyvinyl acetate and styrene/acrylamide/butyl acrylate copolymer;
preparation example 13: the quick-release film-forming agent is 1:1, except for the composite quick-release film-forming agent of sodium carboxymethyl starch and polyvinyl alcohol, the preparation example 1 is the same;
preparation example 14: the quick-release film-forming agent is 1:3 except for the composite quick-release film-forming agent of sodium carboxymethyl starch and polyvinyl alcohol, the preparation example 1 is the same;
preparation example 15: the preparation example 1 was followed except that the immediate-release film-forming agent was a composite immediate-release film-forming agent of sodium carboxymethyl starch and polyvinyl alcohol at a ratio of 1: 1.5.
Comparative example 1:
dissolving 0.5g of pyriproxyfen in 2.5g of methyl oleate, adding an emulsifier (0.2 g of calcium dodecyl benzene sulfonate and 0.3g of fatty alcohol-polyoxyethylene ether) for stirring uniformly, dispersing with a proper amount of water containing 0.5g of a naphthalenesulfonate formaldehyde condensate as a dispersing agent, carrying out full rolling adsorption on the liquid in a roller granulator for 30min by using a proper amount of attapulgite particles, then adding a diluent containing 2.0g of polyvinyl alcohol, carrying out full rolling coating for 30min, and drying to obtain 0.5% pyriproxyfen granules.
Comparative example 2:
dissolving 4.5g of fenthion in 1.5g of diethyl adipate, adding an emulsifier (0.5 g of calcium dodecyl benzene sulfonate and 1.5g of alkylphenol polyoxyethylene), stirring uniformly, uniformly mixing with 1.0g of polycarboxylate dispersing agent dissolved in a proper amount of water, adsorbing by using 5g of white carbon black, uniformly mixing with a proper amount of diluent containing 2.0g of polyvinyl alcohol, carrying out full rolling adsorption for 30min by using a proper amount of attapulgite particles in a roller granulator, and drying to obtain 4.5% fenthion granules.
Comparative example 3:
80000IU/ml of Bacillus thuringiensis Israeli subspecies suspension agent 0.25ml is dissolved in a proper amount of water containing 1.0g of lignosulfonate dispersant, the liquid is fully rolled and adsorbed for 30min by a proper amount of volcanic rock particles in a roller granulator, then diluent containing 0.5g of sodium carboxymethyl starch is added, and after fully rolling and coating for 30min, the liquid is dried to obtain 200IU/g of Bacillus thuringiensis granules.
Comparative example 4:
dissolving 0.1g of ivermectin in 1.0g of dimethyl adipate, adding an emulsifier (0.2 g of fatty alcohol-polyoxyethylene ether and 0.4g of ethylene oxide-propylene oxide segmented copolymer), stirring uniformly, uniformly mixing with 0.5g of naphthalenesulfonate formaldehyde condensate dispersant dissolved in a proper amount of water, adsorbing with 1.0g of white carbon black, uniformly mixing with a diluent containing 0.5g of sodium carboxymethyl starch, sufficiently rolling and adsorbing with a proper amount of volcanic rock particles in a roller granulator for 30min, and drying to obtain 0.1% of ivermectin granules.
Comparative example 5:
dissolving 0.5g of pyriproxyfen in 2.5g of methyl oleate, adding an emulsifier (0.2 g of calcium dodecyl benzene sulfonate and 0.3g of fatty alcohol-polyoxyethylene ether) for stirring uniformly, dispersing with proper amount of water containing 0.5g of a naphthalenesulfonate formaldehyde condensate as a dispersing agent, adsorbing 2.0g of the liquid white carbon black, then carrying out full rolling adsorption for 30min by using proper amount of common river sand particles in a roller granulator, then adding a diluent containing 1.0g of styrene/vinyl acetate/butyl acrylate copolymer, carrying out full rolling coating for 30min, and drying to obtain slow-release core particles for later use;
dissolving 4.5g of fenthion in 1.5g of diethyl adipate, adding an emulsifier (0.5 g of calcium dodecyl benzene sulfonate and 1.5g of alkylphenol polyoxyethylene), uniformly stirring, uniformly mixing with 1.0g of polycarboxylate dispersing agent dissolved in a proper amount of water, adsorbing by using 5g of white carbon black, uniformly mixing with a diluent containing 2.0g of polyvinyl alcohol, fully rolling and coating the mixture with the slow-release type core particles in a roller granulator for 30min, and drying to obtain 100g of common river sand 5% pyriproxyfen fenthion granules.
Comparative example 6: the preparation example 1 is otherwise the same except that the sustained-release film-forming agent is not added;
comparative example 7: the preparation example 1 was prepared in the same manner except that the immediate release film forming agent was not added;
comparative example 8: the preparation example 1 is otherwise the same except that the slow-release film-forming agent is polyvinylpyrrolidone;
comparative example 9: the preparation example 1 is otherwise the same except that the slow-release film forming agent is polyacrylate;
comparative example 10: the preparation example 1 was followed except that the immediate release film-forming agent was sodium carboxymethylcellulose;
comparative example 11: the same procedure as in preparation example 1 was repeated, except that the immediate release type film-forming agent was polyvinylpyrrolidone.
Application example 1: indoor efficacy test (I) for controlling culex pipiens pallens larvae
The test method comprises the following steps:
adding 3L dechlorinated tap water into white porcelain basin, and mixing at 20g/m3The dosage of the active ingredients is added, the mixture is stirred evenly, 30 healthy 3-instar larvae are added, the mixture is fed according to a normal method, and the mortality rate of 2h, the mortality rate of 24h and the resistance feathering rate of the pyriproxyfen-containing medicament are observed after the test insects are added; the experiment was repeated three times and a blank was set.
During the test, the test water was replenished to the initial water volume scale line at intervals 2 d.
And (3) observing the lasting period: 30 3 rd larvae were added to the test group and the blank control group at 1d, 15d, 30d, 60d, 90d, and 120d, respectively, and the test results were observed according to the above procedure.
The test data are as follows:
TABLE-comparison of the efficacy of 15% pyriproxyfen-fenthion granules with that of a single dose against Culex pipiens pallens larvae
As can be seen from the pharmacodynamic data in Table-1, compared with the single dose of 0.5% pyriproxyfen granules, the 5% pyriproxyfen-fenthion granules have obviously prolonged duration of the resistance to feathering due to the slow-release film forming agent component, and the 90d resistance to feathering of the granules is higher than the resistance to feathering of the granules without the slow-release film forming agent of 0.5% pyriproxyfen for 60 d; compared with the single-dose 4.5% fenthion granules, the 5% pyriproxyfen fenthion granules have the advantages that the release speed is high because the medicament is not adsorbed by a porous carrier, the death rate reaches 100% in 2h on the test day, and the death rate of the single-dose 4.5% fenthion granules in 24h is only 94.4%; compared with the 5% pyriproxyfen fenthion granules prepared by using non-porous normal river sand without adsorption performance outside the invention and the 5% pyriproxyfen fenthion granules prepared by using normal river sand without adsorption performance, the quick-acting medicament has the same effect as the 5% pyriproxyfen fenthion granules prepared by using normal river sand without adsorption performance in the aspect of quick-acting performance, but the lasting effect of inhibiting eclosion rate has obvious advantage especially at 90 days; comparative example 6, in which no sustained-release film forming agent was added, was inferior to the examples of the present invention in terms of sustained release, and comparative example 7, in which no immediate-release film forming agent was added, was inferior to the examples of the present invention in terms of immediate release.
Thus, the compound of the invention has obvious advantages in quick-acting property and persistent effect compared with granules prepared by single agent and non-preparation method of the invention, and certainly, the compound of other juvenile hormone analogues and organophosphorus or macrolide medicaments also has similar effect.
Application example 2: indoor efficacy test for controlling culex pipiens pallens larva
The test method comprises the following steps:
3L dechlorinated tap water was added to a white porcelain basin, and the preparation of example 2 was prepared at 20g/m3The dosage of the feed is added, the mixture is stirred evenly, 30 healthy 3-instar larvae are added, the feed is carried out according to a normal method, and the mortality rate of 24h and the mortality rate of 96h are observed after the test larvae are added; the experiment was repeated three times and a blank was set.
During the test, the test water was replenished to the initial water volume scale line at intervals 2 d.
And (3) observing the lasting period: 30 3 rd larvae were added to the test group and the blank control group at 1d, 15d, 30d, 60d, and 90d, respectively, and the test results were observed according to the above procedure.
The test data are as follows:
TABLE-2 comparison of the efficacy of Bti-ivermectin granules with a single dose against Culex pipiens pallens larvae
As can be seen from the pharmacodynamic data in Table-2, compared with 200IU/g of bacillus thuringiensis and 0.1% of ivermectin in a single dose of the granular insecticide, the granular insecticide has certain advantages in the aspect of lasting effect due to the slow-release film-forming agent component, and the 96-hour killing rate of 30d and 60d to culex pipiens pallens larvae is relatively high; compared with a single dose of 0.1% ivermectin granules, the mortality rate of 24h on the day of the first test can reach 100%, the effect of quickly reducing the population density is achieved, the mortality rate within 15d can reach 100%, and the quick-killing effect of the avermectin is fully exerted; in fact, the Bti and other macrolide medicaments or organophosphorus medicaments have similar effects when being compounded.
And (3) testing physical and chemical properties: release Rate test of the pesticidal granule
Accurately weighing 10g of tested granules, placing the granules into a liquid filter bag, sealing a bag opening, placing the liquid filter bag into a 150m L beaker, adding 100m L of deionized water, completely immersing the liquid filter bag into the deionized water, placing the beaker into a thermostat at 25 ℃, taking out 1m L solution from the central part of a container after 1, 3, 7, 14 and 21 days respectively, taking out the solution after shaking in order to make the solution in the container uniform, supplementing the solution with the same amount of deionized water, and keeping the total volume of the liquid unchanged.
The dissolution rates of pyriproxyfen and fenthion in production examples 1 and 10 to 15 (hereinafter, abbreviated as "systems 1" and "systems 10 to 15") and comparative examples 1 to 2 and 5 to 11 (hereinafter, abbreviated as "systems 1 to 2" and "5 to 11") were measured.
TABLE 3 Release Rate test results for pesticidal granules of the invention
In the release rate test of the insecticidal granules, compared with the conventional pyriproxyfen single-agent pair 1, the pair 5 adopting other porous carriers, the pair 6 without the slow-release agent and even the pair 8-9 with other slow-release agents, the slow-release effect is better in the aspect of slow-release performance; in the dissolution of the pyriproxyfen as the sustained-release insecticide, when a specific composite sustained-release film forming agent is selected, the sustained-release effect is better as in preparation examples 10 to 12, and particularly when the composite sustained-release film forming agents are combined in a specific ratio, the effect is optimal as in preparation example 12. Similarly, compared with the conventional fenthion single-dose pair 2, the pair 5 adopting other porous carriers, the pair 5 without the addition of the quick release agent and even the pair 10-11 with the addition of other quick release agents have better quick release performance in the aspect of quick release effect; in addition, when a specific composite immediate release type film forming agent is selected, the immediate release effect is better as in preparation examples 13-15, and particularly when the composite immediate release type film forming agent is combined in a specific ratio, the effect is optimal as in preparation example 15.
The application examples of the present invention only illustrate the advantages of the composition and the preparation method thereof in terms of quick action and persistence by the comparative effect of the agents, and other combinations, the sustained release film forming agent, the immediate release film forming agent and the porous carrier have similar effects, which are not listed herein.
The invention has been described with reference to specific examples, and it will be understood by those skilled in the art that various changes in the materials, process conditions, and combinations or proportions of the active ingredients and other components may be made without departing from the scope of the invention.
Claims (8)
1. The sanitary insecticidal granules are characterized by being prepared by the following method:
dissolving 0.5g of pyriproxyfen in 2.5g of methyl oleate, adding 0.2g of calcium dodecyl benzene sulfonate and 0.3g of fatty alcohol-polyoxyethylene ether, stirring uniformly, dispersing with 0.5g of water containing a dispersing agent naphthalene sulfonate formaldehyde condensate, carrying out full rolling adsorption on the liquid in a roller granulator for 30min by using attapulgite particles, then adding 1.0g of diluent containing a slow-release film-forming agent styrene/acrylamide/butyl acrylate copolymer, carrying out full rolling coating for 30min, and drying to obtain slow-release core particles for later use;
dissolving 4.5g of fenthion in 1.5g of diethyl adipate, adding 0.5g of calcium dodecyl benzene sulfonate and 1.5g of alkylphenol polyoxyethylene, stirring uniformly, mixing uniformly with 1.0g of polycarboxylate dispersing agent dissolved in water, adsorbing by 5g of white carbon black, mixing uniformly with a diluent containing 2.0g of quick-release film-forming agent polyvinyl alcohol, fully rolling and coating for 30min with the slow-release type core particles in a roller granulator, and drying to obtain 100g of 5% pyriproxyfen fenthion granules.
2. A sanitary insecticide granule as claimed in claim 1, wherein the slow release film forming agent is a composite slow release film forming agent of polyvinyl acetate and styrene/acrylamide/butyl acrylate copolymer in a weight ratio of 1: 2.
3. A sanitary insecticide granule as claimed in claim 1, wherein the slow release film forming agent is a composite slow release film forming agent of polyvinyl acetate and styrene/acrylamide/butyl acrylate copolymer in a weight ratio of 1: 3.
4. A sanitary insecticide granule as claimed in claim 1, wherein the slow release film forming agent is a composite slow release film forming agent of polyvinyl acetate and styrene/acrylamide/butyl acrylate copolymer in a weight ratio of 1: 4.
5. A sanitary insecticidal granule according to claim 1, wherein the immediate release film forming agent is a composite immediate release film forming agent of sodium carboxymethyl starch and polyvinyl alcohol in a weight ratio of 1:1.
6. A sanitary insecticidal granule according to claim 1, wherein the quick release type film forming agent is a composite quick release type film forming agent of sodium carboxymethyl starch and polyvinyl alcohol in a weight ratio of 1: 1.5.
7. A sanitary insecticidal granule according to claim 1, wherein the immediate release film forming agent is a composite immediate release film forming agent of sodium carboxymethyl starch and polyvinyl alcohol in a weight ratio of 1: 3.
8. A granular sanitary insecticide according to any one of claims 1 to 7, wherein said insect pest is Culex pipiens pallens.
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| AU2018292285B2 (en) * | 2017-06-26 | 2023-05-25 | Boehringer Ingelheim Animal Health USA Inc. | Dual active parasiticidal granule compositions, methods and uses thereof |
| CN109221107A (en) * | 2018-09-12 | 2019-01-18 | 绩溪农华生物科技有限公司 | A kind of sustained releasing pesticide granule and preparation method thereof |
| CN109042641A (en) * | 2018-09-14 | 2018-12-21 | 河北威远生物化工有限公司 | A kind of emamectin benzoate B2a/B2b benzoate granule and preparation method thereof |
| CN109258632A (en) * | 2018-09-29 | 2019-01-25 | 绩溪农华生物科技有限公司 | A kind of nano pesticide composition and preparation method thereof |
| CN111296488A (en) * | 2018-12-12 | 2020-06-19 | 江苏功成生物科技有限公司 | Sanitary insecticidal composition containing bacillus sphaericus and application thereof |
| CN111296489A (en) * | 2018-12-12 | 2020-06-19 | 江苏功成生物科技有限公司 | Sanitary insecticidal composition containing bacillus sphaericus and organic phosphorus |
| CN111296491A (en) * | 2018-12-12 | 2020-06-19 | 江苏功成生物科技有限公司 | Sanitary insecticidal composition for preventing and treating mosquito larvae and application thereof |
| CN110326613A (en) * | 2019-08-05 | 2019-10-15 | 安徽金敦福农业科技有限公司 | A kind of released granular pesticide and preparation method thereof |
| CN114600876A (en) * | 2022-03-14 | 2022-06-10 | 中国科学院动物研究所 | Mosquito killing method, poison bait and device |
| CN116210715A (en) * | 2022-12-26 | 2023-06-06 | 武汉地美达环境科技有限公司 | Dithiophosphorus granule and preparation method thereof |
| CN115868497B (en) * | 2023-02-01 | 2023-06-13 | 山东瑞可佳农业科技发展有限公司 | Insecticidal composition containing pyriproxyfen and dinotefuran and application method thereof |
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| CN106035323A (en) * | 2016-05-25 | 2016-10-26 | 广西南宁农事帮农业科技服务有限公司 | Sustained-release pesticide granules and preparation method therefor |
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