CN118556700A - Sterilization composition containing difenoconazole and preparation method thereof - Google Patents
Sterilization composition containing difenoconazole and preparation method thereof Download PDFInfo
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- CN118556700A CN118556700A CN202410831899.5A CN202410831899A CN118556700A CN 118556700 A CN118556700 A CN 118556700A CN 202410831899 A CN202410831899 A CN 202410831899A CN 118556700 A CN118556700 A CN 118556700A
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- difenoconazole
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- heptane
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- 239000005760 Difenoconazole Substances 0.000 claims abstract description 75
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000000203 mixture Substances 0.000 claims abstract description 70
- 238000002360 preparation method Methods 0.000 claims abstract description 45
- 230000001954 sterilising effect Effects 0.000 claims abstract description 37
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 37
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 34
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 34
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 34
- 239000004480 active ingredient Substances 0.000 claims abstract description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 36
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- 229920001732 Lignosulfonate Polymers 0.000 claims description 18
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical group [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 claims description 18
- 239000004359 castor oil Substances 0.000 claims description 18
- 235000019438 castor oil Nutrition 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 18
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 18
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 18
- 230000000844 anti-bacterial effect Effects 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 239000004495 emulsifiable concentrate Substances 0.000 claims description 13
- 239000000839 emulsion Substances 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 13
- 239000004563 wettable powder Substances 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000003995 emulsifying agent Substances 0.000 claims description 12
- 239000002562 thickening agent Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical group CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 9
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical group [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 9
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 9
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 9
- 229920000609 methyl cellulose Polymers 0.000 claims description 9
- 239000001923 methylcellulose Substances 0.000 claims description 9
- 235000010981 methylcellulose Nutrition 0.000 claims description 9
- 229920000570 polyether Polymers 0.000 claims description 9
- 238000010008 shearing Methods 0.000 claims description 9
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 9
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 9
- 239000002518 antifoaming agent Substances 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000000080 wetting agent Substances 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 125000003944 tolyl group Chemical group 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims description 3
- 239000007764 o/w emulsion Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 125000003827 glycol group Chemical group 0.000 claims description 2
- 239000000575 pesticide Substances 0.000 abstract description 21
- 239000002689 soil Substances 0.000 abstract description 9
- 239000000447 pesticide residue Substances 0.000 abstract description 2
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 description 9
- 239000005839 Tebuconazole Substances 0.000 description 9
- 241000209140 Triticum Species 0.000 description 5
- 235000021307 Triticum Nutrition 0.000 description 5
- 244000025254 Cannabis sativa Species 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000855 fungicidal effect Effects 0.000 description 2
- 239000000417 fungicide Substances 0.000 description 2
- 239000010665 pine oil Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009885 systemic effect Effects 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000256844 Apis mellifera Species 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000221785 Erysiphales Species 0.000 description 1
- 241000237858 Gastropoda Species 0.000 description 1
- 208000031888 Mycoses Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003124 biologic agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000008029 eradication Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 239000003175 pesticide synergist Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
-
- 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
- A01N25/14—Powders or granules wettable
-
- 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
- A01N27/00—Biocides, pest repellants or attractants, or plant growth regulators containing hydrocarbons
-
- 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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/06—Coniferophyta [gymnosperms], e.g. cypress
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental Sciences (AREA)
- Plant Pathology (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biotechnology (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a sterilization composition containing difenoconazole and a preparation method thereof, and relates to the technical field of pesticides, wherein the sterilization composition contains active ingredients of difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon. The invention not only improves the use efficiency and the safety of pesticides, has important significance for developing environment-friendly pesticides, but also can help to degrade the pesticides, reduce the pesticide residue in soil, has good significance for protecting the surrounding environment, and can effectively solve the problems in the background technology.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to a sterilization composition containing difenoconazole and a preparation method thereof.
Background
Pesticides are chemical substances or biological agents used for controlling crop pests, weeds and regulating plant growth. The bactericidal composition in the pesticide is prepared by mixing two or more bactericides with different action mechanisms, so as to improve the control effect, delay the development of pathogen resistance and prolong the service life of the pesticide. The composition generally has a synergistic effect, can expand the bactericidal spectrum of the medicament, reduce the pesticide dosage, and is more effective for controlling crop diseases.
The sterilization composition commonly used in pesticides at present comprises the combination of difenoconazole and tebuconazole, is mainly used for preventing and treating powdery mildew, is known to be a low-toxicity heterocyclic fungicide pesticide, is mainly used in the field of agriculture, has the characteristics of strong systemic property, broad sterilization spectrum, difficult generation of drug resistance and the like, and the tebuconazole is also an efficient, broad-spectrum and systemic triazole fungicide, and has three functions of protection, treatment and eradication. It is mainly used for preventing and curing various fungal diseases on crops of wheat, rice, peanut, etc. However, it has been found that tebuconazole is degraded slowly in soil and its half-life can be as long as several months to years. This means that tebuconazole will gradually accumulate in the soil, creating a potential risk to the farmland ecosystem. In addition, tebuconazole can enter the water body through precipitation, and the influence on aquatic organisms is generated. Tebuconazole has certain toxicity to fish, snail, bee and other non-target organisms. Irreversible damage to these organisms may occur when tebuconazole enters the body of water or soil. That is, the use of difenoconazole and tebuconazole has a larger influence on the surrounding environment, and is not beneficial to popularization and use.
Disclosure of Invention
Aiming at the defects of the prior art, the sterilization composition containing difenoconazole and the preparation method thereof are provided, so that the use efficiency and the safety of pesticides are improved, the sterilization composition has important significance for developing environment-friendly pesticides, the degradation of the pesticides can be assisted, the pesticide residue in soil is reduced, the sterilization composition has good significance for protecting the surrounding environment, and the problems in the background art can be effectively solved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the bactericidal composition containing difenoconazole contains active ingredients of difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon.
Preferably, the active ingredient is added with a solvent, an emulsifying agent and a solubilizing agent to prepare an emulsifiable concentrate preparation, wherein the solvent is toluene, the emulsifying agent is calcium dodecyl benzene sulfonate and ethoxylated-C16-18, C18-unsaturated alcohol, and the solubilizing agent is castor oil polyoxyethylene ether.
The active ingredient is added with dispersing agent, wetting agent and filler to prepare wettable powder, wherein the dispersing agent is lignin sulfonate, the wetting agent is dodecylbenzene sulfonic acid, and the filler is light calcium carbonate.
The active ingredient is added with a solvent, an emulsifying agent, a solubilizer, an anti-settling agent, an antifreezing agent, a thickening agent and water to prepare a water emulsion preparation, wherein toluene is selected as the solvent, calcium dodecyl benzene sulfonate is selected as the emulsifying agent, castor oil polyoxyethylene ether is selected as the solubilizer, sodium carboxymethyl cellulose is selected as the anti-settling agent, propylene glycol is selected as the antifreezing agent, and hydroxymethyl cellulose is selected as the thickening agent.
The active ingredient is added with dispersing agent, antifreezing agent, thickening agent, defoaming agent and water to prepare a suspension preparation, wherein the dispersing agent is lignin sulfonate, the antifreezing agent is glycol, the thickening agent is methylcellulose, and the defoaming agent is polyether RPE1720.
Preferably, the emulsifiable concentrate preparation comprises 24.7% of difenoconazole, 43.0% of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8% of hydrocarbon, 2.0% of calcium dodecyl benzene sulfonate, 2.0% of ethoxylated-C16-18, C18-unsaturated alcohol, 0.6% of toluene and 5.9% of castor oil polyoxyethylene ether.
The wettable powder comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 3.6 percent of lignosulfonate, 2.7 percent of dodecylbenzene sulfonic acid and the balance of light calcium carbonate.
The water emulsion preparation comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 0.6 percent of toluene, 2.0 percent of calcium dodecyl benzene sulfonate, 2.5 percent of castor oil polyoxyethylene ether, 2.0 percent of sodium carboxymethyl cellulose, 2.0 percent of propylene glycol, 0.8 percent of hydroxymethyl cellulose and the balance of water.
The suspension preparation comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 5.0 percent of lignosulfonate, 1.0 percent of glycol, 0.1 percent of methylcellulose, 0.1 percent of polyether RPE1720 and the balance of water.
The invention also discloses a preparation method of the emulsifiable concentrate preparation of the sterilization composition containing difenoconazole, which comprises the following steps: s1, weighing toluene according to a proportion, adding the toluene into a stirring tank, and sequentially adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon into the stirring tank, and fully stirring to enable the active ingredients to be completely dissolved in a toluene solvent.
S2, adding calcium dodecyl benzene sulfonate, ethoxylated-C16-18, C18-unsaturated alcohol and castor oil polyoxyethylene ether into a stirring tank, continuously stirring, uniformly stirring to form transparent oily liquid, and filling to obtain the emulsifiable concentrate preparation of the sterilization composition containing difenoconazole.
The invention also discloses a preparation method of wettable powder of the sterilization composition containing difenoconazole, which comprises the following steps: h1, weighing difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, hydrocarbon, lignosulfonate, dodecylbenzene sulfonic acid and light calcium carbonate according to the proportion, putting the mixture into a stirring kettle, mixing and stirring uniformly.
And H2, taking out the mixture in the stirring kettle, putting the mixture into the stirring kettle after being crushed by an airflow crusher, and uniformly mixing the mixture to obtain wettable powder of the sterilization composition containing difenoconazole.
The invention also discloses a preparation method of the water emulsion preparation of the sterilization composition containing difenoconazole, which comprises the following steps: q1, adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, hydrocarbon, toluene, calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether into a stirring tank according to the ration, and uniformly mixing to form an oil phase A.
And Q2, taking part of water, uniformly mixing with sodium carboxymethyl cellulose, propylene glycol and hydroxymethyl cellulose to form a water phase B.
Q3, adding the water phase B into a reaction kettle, slowly adding the oil phase A into the reaction kettle while stirring at a high speed until the phase inversion point is reached, starting high-speed shearing, adding the rest of water, and shearing for 30 minutes to form an oil-in-water emulsion, thus obtaining the water emulsion preparation of the sterilization composition containing difenoconazole.
The invention also discloses a preparation method of the suspension preparation of the sterilization composition containing difenoconazole, which comprises the following steps: k1, adding water, lignosulfonate, ethylene glycol, methyl cellulose and polyether RPE1720 into a reaction kettle, and uniformly mixing by high-speed shearing to obtain a mixture A.
K2, adding the mixture A into a ball mill, adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon into the ball mill, and ball milling for 2 hours to ensure that the particle size is below 5 microns, thus obtaining the suspension preparation of the sterilization composition containing the difenoconazole.
Compared with the prior art, the invention provides the sterilization composition containing difenoconazole and the preparation method thereof, and the sterilization composition has the following beneficial effects: the invention combines difenoconazole with 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon, the CAS number of the 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane is 8002-09-03, also called pine oil, and the pine oil not only can be used as an effective pesticide and bactericide, but also can be used as a pesticide synergist, improves the use efficiency and safety of pesticides, and simultaneously has important significance for developing environment-friendly pesticides as a natural source compound.
The added hydrocarbon can also be used for developing grass damage resistant crops, enhancing the resistance of crops to grass damage, reducing the dependence on herbicides, helping to reduce the use of chemical pesticides and promoting the development of sustainable agriculture, and the hydrocarbon is favorable for degrading pesticides and reducing the influence of pesticides on the environment.
Detailed Description
In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be described in further detail with reference to specific embodiments.
Example 1
The invention provides a sterilization composition containing difenoconazole, which contains active ingredients of difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon.
The active ingredients can be prepared into an emulsifiable concentrate preparation after being added with a solvent, an emulsifying agent and a solubilizing agent, wherein the solvent is toluene, the emulsifying agent is calcium dodecyl benzene sulfonate and ethoxylated-C16-18, C18-unsaturated alcohol, and the solubilizing agent is castor oil polyoxyethylene ether.
Specifically, the emulsifiable concentrate preparation comprises 24.7% of difenoconazole, 43.0% of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8% of hydrocarbon, 2.0% of calcium dodecyl benzene sulfonate, 2.0% of ethoxylated-C16-18, C18-unsaturated alcohol, 0.6% of toluene and 5.9% of castor oil polyoxyethylene ether.
The method for preparing the emulsifiable concentrate preparation of the sterilization composition containing difenoconazole is shown as follows, and comprises the following steps: s1, weighing toluene according to a proportion, adding the toluene into a stirring tank, and sequentially adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon into the stirring tank, and fully stirring to enable the active ingredients to be completely dissolved in a toluene solvent.
S2, adding calcium dodecyl benzene sulfonate, ethoxylated-C16-18, C18-unsaturated alcohol and castor oil polyoxyethylene ether into a stirring tank, continuously stirring, uniformly stirring to form transparent oily liquid, and filling to obtain the emulsifiable concentrate preparation of the sterilization composition containing difenoconazole.
Example two
The invention provides a sterilization composition containing difenoconazole, which contains active ingredients of difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon.
The active ingredients are added with dispersing agents, wetting agents and fillers to prepare wettable powder, wherein the dispersing agents are lignosulfonate, the wetting agents are dodecylbenzene sulfonic acid, and the fillers are light calcium carbonate.
Specifically, the wettable powder comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 3.6 percent of lignosulfonate, 2.7 percent of dodecylbenzene sulfonic acid and the balance of light calcium carbonate.
The method for preparing the wettable powder of the sterilization composition containing difenoconazole comprises the following steps: h1, weighing difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, hydrocarbon, lignosulfonate, dodecylbenzene sulfonic acid and light calcium carbonate according to the proportion, putting the mixture into a stirring kettle, mixing and stirring uniformly.
And H2, taking out the mixture in the stirring kettle, putting the mixture into the stirring kettle after being crushed by an airflow crusher, and uniformly mixing the mixture to obtain wettable powder of the sterilization composition containing difenoconazole.
Example III
The invention provides a sterilization composition containing difenoconazole, which contains active ingredients of difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon.
The active ingredients are added with a solvent, an emulsifying agent, a solubilizer, an anti-settling agent, an antifreezing agent, a thickening agent and water to prepare a water emulsion preparation, wherein toluene is selected as the solvent, calcium dodecyl benzene sulfonate is selected as the emulsifying agent, castor oil polyoxyethylene ether is selected as the solubilizer, sodium carboxymethyl cellulose is selected as the anti-settling agent, propylene glycol is selected as the antifreezing agent, and hydroxymethyl cellulose is selected as the thickening agent.
Specifically, the water emulsion comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 0.6 percent of toluene, 2.0 percent of calcium dodecyl benzene sulfonate, 2.5 percent of castor oil polyoxyethylene ether, 2.0 percent of sodium carboxymethyl cellulose, 2.0 percent of propylene glycol, 0.8 percent of hydroxymethyl cellulose and the balance of water.
A method for preparing an aqueous emulsion formulation of a bactericidal composition containing difenoconazole comprising the steps of: q1, adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, hydrocarbon, toluene, calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether into a stirring tank according to the ration, and uniformly mixing to form an oil phase A.
And Q2, taking part of water, uniformly mixing with sodium carboxymethyl cellulose, propylene glycol and hydroxymethyl cellulose to form a water phase B.
Q3, adding the water phase B into a reaction kettle, slowly adding the oil phase A into the reaction kettle while stirring at a high speed until the phase inversion point is reached, starting high-speed shearing, adding the rest of water, and shearing for 30 minutes to form an oil-in-water emulsion, thus obtaining the water emulsion preparation of the sterilization composition containing difenoconazole.
Example IV
The invention provides a sterilization composition containing difenoconazole, which contains active ingredients of difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon.
The active ingredients are added with dispersing agents, antifreezing agents, thickening agents, defoaming agents and water to prepare a suspension preparation, wherein the dispersing agents are lignin sulfonate, the antifreezing agents are ethylene glycol, the thickening agents are methylcellulose, and the defoaming agents are polyether RPE1720.
Specifically, the suspension preparation comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 5.0 percent of lignosulfonate, 1.0 percent of glycol, 0.1 percent of methylcellulose, 1720.1 percent of polyether RPE and the balance of water.
A method of preparing a suspension formulation of a bactericidal composition containing difenoconazole comprising the steps of: k1, adding water, lignosulfonate, ethylene glycol, methyl cellulose and polyether RPE1720 into a reaction kettle, and uniformly mixing by high-speed shearing to obtain a mixture A.
K2, adding the mixture A into a ball mill, adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon into the ball mill, and ball milling for 2 hours to ensure that the particle size is below 5 microns, thus obtaining the suspension preparation of the sterilization composition containing the difenoconazole.
And 5 adjacent wheat fields with the same specification and the same soil quality are adopted for testing, and the emulsifiable concentrate preparation, the wettable powder preparation, the water emulsion preparation and the suspension preparation of the sterilization composition containing the difenoconazole prepared in the examples are diluted according to the specified dosage, and are uniformly sprayed on 4 wheat fields by using a sprayer, wherein the application dosage is that the leaf surfaces are fully wetted and the liquid medicine does not flow down from the leaf surfaces. The pesticide containing the sterilization composition of difenoconazole and tebuconazole on the market is taken as a control example and sprayed on another wheat field according to the method.
After 30 days, 5 pieces of soil having the same weight (1 kg) as each sample were extracted from 5 pieces of wheat fields, and 5 pieces of soil were each detected by gas chromatography, and the detection results are shown in the following table.
As can be directly seen from the table, the bactericidal composition prepared by the invention has less residue in soil, less influence on environment and much lower residue than the specification in GB 2763.1-2022, which proves that the bactericidal composition prepared by the invention is safer to use and has higher popularization value.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.
Claims (9)
1. The sterilization composition containing difenoconazole is characterized in that: comprises active components of difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon.
2. The difenoconazole-containing bactericidal composition according to claim 1, wherein: the active ingredient is added with a solvent, an emulsifying agent and a solubilizing agent to prepare an emulsifiable concentrate preparation, wherein the solvent is toluene, the emulsifying agent is calcium dodecyl benzene sulfonate and ethoxylated-C16-18, C18-unsaturated alcohol, and the solubilizing agent is castor oil polyoxyethylene ether; the emulsifiable concentrate preparation comprises 24.7% of difenoconazole, 43.0% of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8% of hydrocarbon, 2.0% of calcium dodecyl benzene sulfonate, 2.0% of ethoxylated-C16-18, C18-unsaturated alcohol, 0.6% of toluene and 5.9% of castor oil polyoxyethylene ether.
3. The difenoconazole-containing bactericidal composition according to claim 1, wherein: the active ingredient is added with a dispersing agent, a wetting agent and a filler to prepare wettable powder, wherein the dispersing agent is lignin sulfonate, the wetting agent is dodecylbenzene sulfonic acid, and the filler is light calcium carbonate; the wettable powder comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 3.6 percent of lignosulfonate, 2.7 percent of dodecylbenzene sulfonic acid and the balance of light calcium carbonate.
4. The difenoconazole-containing bactericidal composition according to claim 1, wherein: the active ingredient is added with a solvent, an emulsifying agent, a solubilizer, an anti-settling agent, an antifreezing agent, a thickening agent and water to prepare a water emulsion preparation, wherein the solvent is toluene, the emulsifying agent is calcium dodecyl benzene sulfonate, the solubilizer is castor oil polyoxyethylene ether, the anti-settling agent is sodium carboxymethyl cellulose, the antifreezing agent is propylene glycol, and the thickening agent is hydroxymethyl cellulose; the water emulsion preparation comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 0.6 percent of toluene, 2.0 percent of calcium dodecyl benzene sulfonate, 2.5 percent of castor oil polyoxyethylene ether, 2.0 percent of sodium carboxymethyl cellulose, 2.0 percent of propylene glycol, 0.8 percent of hydroxymethyl cellulose and the balance of water.
5. The difenoconazole-containing bactericidal composition according to claim 1, wherein: the active ingredient is added with a dispersing agent, an antifreezing agent, a thickening agent, a defoaming agent and water to prepare a suspension preparation, wherein the dispersing agent is lignin sulfonate, the antifreezing agent is glycol, the thickening agent is methylcellulose, and the defoaming agent is polyether RPE1720; the suspension preparation comprises 24.7 percent of difenoconazole, 43.0 percent of 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, 21.8 percent of hydrocarbon, 5.0 percent of lignosulfonate, 1.0 percent of glycol, 0.1 percent of methylcellulose, 0.1 percent of polyether RPE1720 and the balance of water.
6. The method for preparing the emulsifiable concentrate formulation of the sterilization composition containing difenoconazole as claimed in claim 2, which is characterized by comprising the following steps:
S1, weighing toluene according to a proportion, adding the toluene into a stirring tank, and sequentially adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon into the stirring tank, and fully stirring to enable active ingredients to be completely dissolved in a toluene solvent;
S2, adding calcium dodecyl benzene sulfonate, ethoxylated-C16-18, C18-unsaturated alcohol and castor oil polyoxyethylene ether into a stirring tank, continuously stirring, uniformly stirring to form transparent oily liquid, and filling to obtain the emulsifiable concentrate preparation of the sterilization composition containing difenoconazole.
7. The method for preparing wettable powder of the difenoconazole-containing bactericidal composition according to claim 3, which is characterized by comprising the following steps:
H1, weighing difenoconazole, 1-hydroperoxy radical-2, 7-3 methyl bicyclo [3.1.1] heptane, hydrocarbon, lignosulfonate, dodecylbenzene sulfonic acid and light calcium carbonate according to the proportion, putting into a stirring kettle, mixing, and uniformly stirring;
And H2, taking out the mixture in the stirring kettle, putting the mixture into the stirring kettle after being crushed by an airflow crusher, and uniformly mixing the mixture to obtain wettable powder of the sterilization composition containing difenoconazole.
8. The method for preparing the aqueous emulsion preparation of the difenoconazole-containing bactericidal composition according to claim 4, wherein said method comprises the following steps:
Q1, adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane, hydrocarbon, toluene, calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether into a stirring tank according to the ration, and uniformly mixing to form an oil phase A;
Q2, taking part of water, uniformly mixing with sodium carboxymethyl cellulose, propylene glycol and hydroxymethyl cellulose to form a water phase B;
Q3, adding the water phase B into a reaction kettle, slowly adding the oil phase A into the reaction kettle while stirring at a high speed until the phase inversion point is reached, starting high-speed shearing, adding the rest of water, and shearing for 30 minutes to form an oil-in-water emulsion, thus obtaining the water emulsion preparation of the sterilization composition containing difenoconazole.
9. The method for preparing the suspension preparation of the difenoconazole-containing bactericidal composition according to claim 5, comprising the steps of:
K1, adding water, lignosulfonate, ethylene glycol, methyl cellulose and polyether RPE1720 into a reaction kettle, and uniformly mixing by high-speed shearing to obtain a mixture A;
k2, adding the mixture A into a ball mill, adding difenoconazole, 1-hydroperoxy radical-2, 7-3-methyl bicyclo [3.1.1] heptane and hydrocarbon into the ball mill, and ball milling for 2 hours to ensure that the particle size is below 5 microns, thus obtaining the suspension preparation of the sterilization composition containing the difenoconazole.
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