WO2017219806A1 - 含吡唑酮类化合物的除草组合物及其应用 - Google Patents

含吡唑酮类化合物的除草组合物及其应用 Download PDF

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Publication number
WO2017219806A1
WO2017219806A1 PCT/CN2017/084919 CN2017084919W WO2017219806A1 WO 2017219806 A1 WO2017219806 A1 WO 2017219806A1 CN 2017084919 W CN2017084919 W CN 2017084919W WO 2017219806 A1 WO2017219806 A1 WO 2017219806A1
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herbicidal composition
group
active ingredient
composition containing
compound according
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PCT/CN2017/084919
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English (en)
French (fr)
Inventor
彭学岗
金涛
张景远
赵德
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青岛清原抗性杂草防治有限公司
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Publication of WO2017219806A1 publication Critical patent/WO2017219806A1/zh

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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
    • A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
    • A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
    • 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
    • A01N25/32—Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
    • 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
    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
    • A01N33/18—Nitro compounds
    • A01N33/20—Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group
    • A01N33/22—Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group having at least one oxygen or sulfur atom and at least one nitro group directly attached to the same aromatic ring system
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
    • A01N37/48—Nitro-carboxylic acids; Derivatives thereof
    • 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
    • A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
    • A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
    • A01N39/04—Aryloxy-acetic acids; Derivatives thereof
    • 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
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
    • 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
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
    • 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
    • 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
    • A01N43/66—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
    • A01N43/68—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
    • A01N43/70—Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, 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
    • A01N47/08—Biocides, 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
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/30—Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl

Definitions

  • the invention belongs to the field of pesticides, and in particular relates to a herbicidal composition containing a pyrazolone compound and application thereof.
  • Chemical weeding is the most economical and effective means of controlling weeds in farmland.
  • long-term continuous high-dose use of single-species or single-acting chemical herbicides is prone to problems such as weed resistance and resistance evolution.
  • Rational compounding or compounding of herbicide compounds has the advantages of expanding weed spectrum, improving control effect, delaying the occurrence and development of weed resistance and drug resistance, and is one of the most effective methods to solve the above problems.
  • HPPD P-hydroxyphenylpyruvate dioxygenase
  • ACCase acetyl-CoA carboxylase
  • ALS acetolactate synthase
  • Protox protoporphyrin oxidase
  • HPPD inhibitors Another class of new herbicides.
  • the action of HPPD inhibitors is characterized by a broad spectrum of herbicidal activity, which can be used before and after emergence, and the weeds die after whitening. Although the symptoms are very similar to those of carotenoid bioinhibitors, their chemical structural features such as polarity and ionization are significantly different from known carotenoid bioinhibitors.
  • the risk of HPPD inhibitor herbicide weed resistance is much lower than that of ACCase inhibitors, and there is no cross-resistance resistance caused by target resistance with other active mechanisms such as ACCase inhibitors and ALS inhibitors.
  • Herbicide Safener also known as Antidote or Protectant, including amides, carbamates, phenoxycarboxylic acids, aryloxyphenoxypropionates, sulfonylureas , sulfonamides, imidazolinones, cyclohexanediones, isoxazole diketones, and triazines, etc., are chemical substances with unique properties. With the wide application of herbicides, the problem of herbicide phytotoxicity continues to emerge, and there is an urgent need for herbicide safeners.
  • the crops protected by herbicide safeners mainly include corn, rice, sugar cane, sorghum, rye, cotton, soybeans and the like.
  • Herbicide safeners selectively protect crops from herbicides without affecting the herbicide activity against target weeds, thereby enhancing crop tolerance to herbicides and increasing herbicide safety for crops. .
  • the present invention provides a herbicidal composition containing a pyrazolone compound and an application thereof, which can effectively solve the weeding and tendon in the weeding and weeding in the sugarcane field.
  • Weed problems such as grass and small canopy have the characteristics of expanding herbicidal spectrum, reducing application rate, safety for crops, and solving resistant weeds.
  • a herbicidal composition containing a pyrazolone compound comprising a herbicidally effective amount of active ingredient A, active ingredient B, And safener compound C, wherein
  • the active ingredient A is one of the following formulas:
  • R 1 is a hydrogen atom, a methyl group, an ethyl group, a cyclopropyl group
  • R 2 is methyl, ethyl, isopropyl
  • R 3 is ethoxy, fluoroethoxy, difluoroethoxy, trifluoroethoxy, pyrazolyl
  • R 4 is a chlorine atom, a methyl group
  • R 5 , R 6 , R 7 are alkyl, alkoxy, halogen-substituted alkyl, halogen-substituted alkoxy;
  • the active ingredient B is selected from one or more of the following compounds:
  • Triazines chlorpyrifos, simazine, cycloazinone, chlorpyrifos;
  • phenoxycarboxylic acid sodium 2-methyltetrachloride, 2,4-butyl butyl ester;
  • Safener Compound C is selected from one or more of the following compounds:
  • R 1 is a hydrogen atom
  • R 2 is a methyl group
  • R 3 is an ethoxy group, a fluoroethoxy group, a difluoroethoxy group, a trifluoroethoxy group, and a pyridyl group.
  • Razolyl is a chlorine atom
  • R 5 , R 6 , R 7 are alkyl, alkoxy, halogen-substituted alkyl, halogen-substituted alkoxy;
  • the active ingredient B is quenching, oxyfluorfen, flufenacetate, clomazone, sodium methoxide, mesalamine, glyphosate, glufosinate, diuron, One or more of saflufenacil;
  • the safener compound C is one or more of dibenzoxazole acid, cyprosulfamide, pyrazolium, furilazole.
  • R 1 is a hydrogen atom
  • R 2 is a methyl group or an ethyl group
  • R 3 is an ethoxy group, a difluoromethoxy group or a trifluoromethoxy group
  • R 4 is a chlorine atom
  • R 5 is a methyl group
  • R 6 is a methyl group
  • R 7 is a hydrogen atom.
  • the weight ratio of A, B and C is 1-100: 1-100: 1-100, preferably 1-50: 1-50: 1-50, more preferably 1-30: 1-30: 1- 30.
  • the synergistic effect of A and the active ingredient B is synergistic, and the safener compound C plays a good safety improvement for the crop.
  • the mass percentage of A, B, and C in the herbicidal composition is from 1 to 95%, preferably from 10 to 80%, based on the total amount.
  • the herbicidal compositions of the present invention comprise from 1 to 95 parts by weight of active ingredient and from 5 to 99 parts by weight of a conventional pesticide adjuvant.
  • auxiliaries of the compositions of the present invention may be carriers, surfactants and the like.
  • carrier refers to an organic or inorganic, natural or synthetic material. They aid in the administration of the active ingredient which is generally inert and must be agriculturally acceptable, especially accepted by the treated plant.
  • the carrier may be solid, such as clay, natural or synthetic silicates, silica, resins, waxes, solid fertilizers, etc.; or liquid, such as water, alcohols, ketones, petroleum fractions, aromatic or waxy hydrocarbons, chlorine Hydrocarbons, liquefied gases, etc.
  • Surfactants may include emulsifiers, dispersants or wetting agents, which may be ionic or nonionic. Examples which may be mentioned are salts of polyacrylic acid, lignosulfonates, salts of phenolsulfonic or naphthalenesulfonic acid, ethylene oxide with aliphatic alcohols or with aliphatic acids or with aliphatic amines and substituted phenols (especially a polymer of an alkylphenol or an arylphenol, a sulfosuccinate, a taurine derivative (especially a taurine alkyl ester), a phosphate ester of an alcohol or a phosphate of a polyhydroxyethylated phenol, Alkyl sulfonates, alkyl aryl sulfonates, alkyl sulfates, lauryl ether sulfates, fatty alcohol sulfates, and sulfated hexadecane, hepta-
  • compositions may also contain various other components such as protective colloids, binders, thickeners, thixotropic agents, penetrants, Stabilizers, chelating agents, dyes, colorants and polymers.
  • compositions of the present invention may be diluted or used directly by the user prior to use.
  • the preparation can be prepared by a usual processing method, that is, after mixing the active material with a liquid solvent or a solid carrier, and then adding one or more of a surfactant such as a dispersing agent, a stabilizer, a wetting agent, a binder, an antifoaming agent, and the like.
  • a surfactant such as a dispersing agent, a stabilizer, a wetting agent, a binder, an antifoaming agent, and the like.
  • Specific formulations of the herbicidal compositions are wettable powders, dispersible oil suspensions, suspensions, suspoemulsions, emulsifiable concentrates, water-dispersible granules (dry suspensions), aqueous emulsions, microemulsions.
  • the original drug, safener, solvent and emulsifier in the above formula are added into the mother liquor to prepare a uniform oil phase, and the deionized water and the antifreezing agent are uniformly mixed into the product preparation kettle, and the mixture is uniformly stirred and mixed.
  • the composition of the invention is a transparent or translucent microemulsion product.
  • compositions of the present invention can be combined with solid and liquid additives conventionally used in prior art formulations.
  • composition of the present invention can be applied to the leaves of the plants to be treated by spraying, i.e., to the weeds, particularly on the surface which is infested or susceptible to weeds which are harmful to the growth of the crop.
  • the present invention provides a group of environmentally friendly herbicides which are easily degraded in the environment.
  • the herbicidal composition of the invention has low cost and convenient use, and has great economic and social benefits for its popularization and application.
  • the herbicidal composition of the present invention can prevent grass weeds such as valerian and goosegrass which are resistant to ALS inhibitors and ACCase inhibitors, and paraquat and glyphosate.
  • grass weeds such as valerian and goosegrass which are resistant to ALS inhibitors and ACCase inhibitors, and paraquat and glyphosate.
  • the broad-leaved weeds, such as the resistant cannabis, are an effective solution for weed resistance management.
  • R 1 is a hydrogen atom
  • R 2 is ethyl
  • R 3 is trifluoromethoxy
  • R 4 is a chlorine atom
  • R 5 is methyl
  • R 6 is methyl
  • R 7 is a hydrogen atom is A 1;
  • R 1 is a hydrogen atom
  • R 2 is methyl
  • R 3 is difluoromethoxy
  • R 4 is a chlorine atom
  • R 5 is methyl
  • R 6 is methyl
  • R 7 is a hydrogen atom is A 2;
  • R 1 is a hydrogen atom
  • R 2 is ethyl
  • R 3 is ethoxy
  • R 4 is a chlorine atom
  • R 5 is methyl
  • R 6 is methyl
  • R 7 is a hydrogen atom when A 3;
  • composition of the formula is: 3% A 1 +50% quenching net + 1% dibenzoxazole acid + 5% dispersing agent phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester +8% emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • composition of the formula is: 3% A 2 + 50% quenching net + 1.5% cyprosulfamide + 5% dispersing agent phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester + 8% emulsified Castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • Formulation composition 6%A 3 +10% oxyfluorfen + 1% dibenzoxazole + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxygen Vinyl ester + 8% emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • the active ingredient B is oxyfluorfen and the safener compound C is cyprosulfamide
  • Formulation composition 6%A 1 +10% oxyfluorfen + 2% cyprosulfamide + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester +8 % emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • the active ingredient B is acesulfame
  • the safener compound C is cyprosulfamide
  • composition of the formula is: 6% A 3 +1% acesulfame + 6% cyprosulfamide + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester +8 % emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • Formulation composition 3%A 1 +30% oxacillin + 1% pyrazole oxalate + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene Ester +8% emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • the active ingredient B is sodium tetramethyl chlorochloride and the safener compound C is dibenzoxazole acid
  • composition of the formula is: 3%A 1 +9% 2 sodium tetrachloride + 2% dibenzoxazole acid + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxygen Vinyl ester + 8% emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • Formulation composition 3%A 1 +15% mesotriamide + 1% furilazole + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester +8% Emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • composition of the formula is: 3% A 2 +15% glyphosate + 3% pyrazole herbicide + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester +8% emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • composition of the formula is: 3%A 1 +20% glufosinate + 1% pyrazolium ester + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester +8% emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • Formulation composition 1.5% A 3 +30% diuron + 0.75% dibenzoxazole + 5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt + 5% emulsifier fatty acid polyoxyethylene ester +8% emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • the active ingredient B is saflufenacil and the safener compound C is cyprosulfamide
  • Formulation composition 6%A 1 +4% saflufenacil +6% cyprosulfamide +5% dispersant phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt +5% emulsifier fatty acid polyoxyethylene ester +8 % emulsifier castor oil polyoxyethylene ether + 2% thickener organic bentonite + methyl oleate to make up.
  • composition of the formula is: 3% A 2 + 50% quenching net + 3% cyprosulfamide + 5% dispersing agent sodium lignosulfonate + 2% wetting agent pulling powder + 0.3% thickener xanthan gum + 5% antifreeze The agent glycerin + balance water to make up.
  • Processing equipment mixing tank, colloid mill, sand mill, shearing machine, etc.
  • the formula consists of: 1.5% A 3 +30% diuron +1.5% pyrazole herbicide + 5% dispersing agent sodium lignosulfonate + 2% wetting agent pulling powder + 0.3% thickener xanthan gum +5% antifreeze glycerol + balance water to make up.
  • Processing equipment mixing tank, colloid mill, sand mill, shearing machine, etc.
  • composition of the formula is: 3%A 1 +50% quenching net + 1% cyprosulfamide + 10% dispersing agent naphthalene sulfonate + 5% wetting agent pulling powder + 1% disintegrant polyvinyl alcohol + filler diatom The soil complements the foot.
  • Processing equipment jet mill, coulter mixer, basket granulator, drying oven, screening machine, etc.
  • composition of the formula is: 12% A 3 + 20% oxyfluorfen + 6% dibenzoxazole + 10% dispersant naphthalene sulfonate + 5% wetting agent pull powder +1% disintegrant Vinyl alcohol + filler diatomaceous earth to make up.
  • Processing equipment jet mill, coulter mixer, basket granulator, drying oven, screening machine, etc.
  • Formulation composition 6%A 3 +30% mesalamine + 2% cyprosulfamide + 10% dispersant naphthalene sulfonate + 5% wetting agent pull powder +1% disintegrant polyvinyl alcohol + filler silicon The algae is made up.
  • Processing equipment jet mill, coulter mixer, basket granulator, drying oven, screening machine, etc.
  • Echinochloa crusgalli and Echinochloa crusgalli were collected from sugarcane fields in Huizhou, Guangdong.
  • Convolvulus arvensis was collected from non-cultivated land in Qingdao, Shandong Province.
  • Conyza canadensis is collected from non-cultivated land in Songzi, Hubei.
  • the above weeds were cultured by pot culture, and placed in an enamel pan with 180 ⁇ 140mm plastic nutrient bowl.
  • the surface soil was collected from the farmland and passed through the air-screened surface (4/5).
  • the initial humidity of the soil was controlled at 20%.
  • the seeds with full and uniform seeds were soaked in warm water at 25 ° C for 6 hours, germinated in a 28 ° C biochemical incubator (dark), and the white weed seeds were evenly placed on the soil surface, and then covered with soil 0.7 cm.
  • the medicine is placed in a controllable solar greenhouse, and a certain amount of water is regularly added to the enamel tray to keep the soil moist.
  • the required active ingredient B is a commercially available original drug, and A is produced by the company, see patent CN201511030154.6.
  • the original drugs were all treated with acetone as a solvent, diluted with 0.1% emulsifier T-80 aqueous solution, and now diluted.
  • each group of A and active ingredient B When determining the distribution ratio or content of each group of A and active ingredient B, it should be measured from the characteristics and virulence of the two agents, and the main purpose of the formulation should be considered. Based on the preliminary pre-test, the study set A, active ingredient B alone and mixed The combined dosages are shown in the table, and a total of 15 groups were designed. Water containing no drug, the same solvent and an emulsifier was used as a blank control.
  • Each treatment was repeated 4 times, and each time 3 pots were treated, 20 seeds of weed seeds were planted per pot, and 60 plants per treatment.
  • the cultured test materials were evenly placed on a platform with an area of 0.5 m 2 , and sprayed with a 3WP-2000 type walking spray tower, and the spray amount was 30 kg/ha.
  • the spray pressure was 0.3 MPa. After all the liquid medicines have been sprayed, close the air valve. After 30 seconds, open the spray tower door and take out the nutrient bowl. Then open the gas valve, spray 50 mL of water, and clean the spray tube.
  • the whole seedlings of the living weeds were cut along the surface of the soil with a blade, and the fresh weight of the weeds was weighed by an analytical balance. For dead weeds, the fresh weight is zero.
  • the investigation was conducted 20 days after the treatment, and a total of 1 investigation was conducted.
  • E measured inhibition rate
  • the E-E0 value is greater than 10% for synergism, less than -10% for antagonism, and between -10% and 10% for additive effect. According to the actual control effect and the characteristics of the herbicide, the balance of the formula and other factors determine the best ratio.
  • X is the fresh weight inhibition rate when A is used as P
  • Y is the fresh weight inhibition rate when the amount of active ingredient B is Q.
  • Table 3A The actual control effect and combined effect of weed on mixed weeds (Gowing method)
  • the herbicide composition prepared in the examples was used to control the weed field test in sugar cane fields.
  • A is mixed with active ingredient B and safener compound C for controlling grass weeds after sugarcane field, and has surprising and unexpected synergistic effects, especially It has a particularly obvious synergistic effect on broadleaf weeds such as weeds, goosegrass, weeds, alfalfa, and twigs, which can reduce the dosage, safely sugarcane, and reduce environmental pollution.
  • Compounding reduces agricultural costs and has a good application prospect.
  • the herbicide composition prepared in the examples was used to control the no-tillage field.
  • A is mixed with active ingredient B, and has surprising and unexpected synergistic effects on glyphosate-resistant canopy, which can reduce the amount of drug used and reduce environmental pollution. And reasonable compounding reduces the cost of agriculture and has a good application prospect.

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Abstract

本发明属于农药领域，具体涉及一种含吡唑酮类化合物的除草组合物及其应用。所述除草组合物包括除草有效量的活性成分A、活性成分B、以及安全剂化合物C，其中，活性成分A为下列通式中的一种：R1是氢原子；R2是甲基；R3是乙氧基；R4是氯原子；R5、R6、R7是烷基等；活性成分B选自以下化合物中的一种或多种：1)三嗪类：莠灭净；2)二苯醚类：乙氧氟草醚等；安全剂化合物C选自以下化合物中的一种或多种：C1：双苯噁唑酸等。该组合物能有效解决灭生性除草、甘蔗田除草中的稗草、牛筋草、小飞蓬等杂草问题，具有扩大杀草谱、减少施用量、对作物安全、能够解决抗性杂草等特点。

Description

含吡唑酮类化合物的除草组合物及其应用 技术领域
本发明属于农药领域，具体涉及一种含吡唑酮类化合物的除草组合物及其应用。
背景技术
化学除草是农田杂草防除中最为经济、有效的手段，但长期连续高剂量地使用单一品种或单一作用方式的化学除草剂，容易造成杂草耐药和抗性演化等问题。除草剂化合物的合理复配或混配具有扩大杂草谱、提高防除效果、延缓杂草耐药性和抗药性的发生与发展等优点，是解决上述问题的最为有效的方法之一。
对羟苯基丙酮酸双氧化酶(HPPD)是继乙酰辅酶A羧化酶(ACCase)抑制剂、乙酰乳酸合成酶(ALS)抑制剂和原卟啉原氧化酶(Protox)抑制剂等之后发现的又一类新型除草剂。HPPD抑制剂的作用特点是具有广谱的除草活性，芽前和芽后均可使用，杂草出现白化后死亡。虽其症状与类胡萝卜素生物抑制剂的作用症状极相似，但其化学结构特点如极性和电离度与已知的类胡萝卜素生物抑制剂有明显的不同。HPPD抑制剂类除草剂杂草抗性风险大大低于ACCase抑制剂，并且与常用的ACCase抑制剂、ALS抑制剂等其他作用机制不存在靶标抗性引起的交互抗性。
除草剂安全剂(Safener)，也称解毒剂(Antidote)或保护剂(Protectant)，包括酰胺类、氨基甲酸酯类、苯氧羧酸类、芳氧苯氧丙酸酯类、磺酰脲类、磺酰胺类、咪唑啉酮类、环已二酮类、异恶唑二酮类、均三氮苯类等，是具有独特性能的化学物质。随着除草剂的广泛应用，除草剂药害问题不断出现，对除草剂安全剂存在迫切需求。除草剂安全剂保护的作物主要有玉米、水稻、甘蔗、高粱、黑麦、棉花、大豆等。除草剂安全剂是在不影响除草剂对靶标杂草活性的前提下，有选择地保护作物免遭除草剂药害，从而增强作物对除草剂的耐受能力，增加除草剂对作物的安全性。
目前，小麦田、水稻田除草剂抗性杂草问题最为严重，其次是灭生性除草剂、玉米田除草剂及其他作物田除草剂的抗性杂草问题，生产上亟需安全性高、杀草谱广、能够解决抗性杂草问题的品种。
发明内容
为解决现有技术中存在的上述问题，本发明提供一种含吡唑酮类化合物的除草组合物及其应用，该组合物能有效解决灭生性除草、甘蔗田除草中的稗草、牛筋草、小飞蓬等杂草问题，具有扩大杀草谱、减少施用量、对作物安全、能够解决抗性杂草等特点。
一种含吡唑酮类化合物的除草组合物，包括除草有效量的活性成分A、活性成分B、以 及安全剂化合物C，其中，
活性成分A为下列通式中的一种：
Figure PCTCN2017084919-appb-000001
R1是氢原子，甲基，乙基，环丙基；
R2是甲基，乙基，异丙基；
R3是乙氧基，氟乙氧基，二氟乙氧基，三氟乙氧基，吡唑基；
R4是氯原子，甲基；
R5、R6、R7是烷基，烷氧基，卤素取代的烷基，卤素取代的烷氧基；
活性成分B选自以下化合物中的一种或多种：
1)三嗪类：莠灭净、西玛津、环嗪酮、扑草净；
2)二苯醚类：乙氧氟草醚、乙羧氟草醚、三氟羧草醚；
3)异噁草松；
4)苯氧羧酸类：2甲4氯钠、2,4-滴丁酯；
5)甲磺草胺；
6)有机磷类：草甘膦、草铵膦；
7)取代脲类：敌草隆、灭草隆、利谷隆、绿麦隆；
8)苯嘧磺草胺；
9)敌草快；
安全剂化合物C选自以下化合物中的一种或多种：
C1：双苯噁唑酸(CAS：163520-33-0)
C2：cyprosulfamide(CAS号：221667-31-8)
C3：吡唑解草酯(CAS号：135590-91-9)
C4：解毒喹(CAS号：99607–70–2)
C5：赤霉酸(CAS号：99607–70–2)
C6：furilazole(CAS号：121776–33–8)
C7：N-(2-2甲氧基苯甲酰基)-4-[(甲基氨基羰基)氨基]苯磺酰胺。
作为优选地，所述活性成分A中R1是氢原子；R2是甲基，乙基；R3是乙氧基，氟乙氧 基，二氟乙氧基，三氟乙氧基，吡唑基；R4是氯原子；R5、R6、R7是烷基，烷氧基，卤素取代的烷基，卤素取代的烷氧基；
所述活性成分B为莠灭净、乙氧氟草醚、乙羧氟草醚、异噁草松、2甲4氯钠、甲磺草胺、草甘膦、草铵膦、敌草隆、苯嘧磺草胺中一种或多种；
所述安全剂化合物C为双苯噁唑酸、cyprosulfamide、吡唑解草酯、furilazole中一种或多种。
更优选地，所述活性成分A中R1是氢原子，R2是甲基或乙基，R3是乙氧基、二氟甲氧基或三氟甲氧基，R4是氯原子，R5是甲基，R6是甲基，R7是氢原子。
其中，A、B、C的重量比为1-100:1-100:1-100，优选为1-50:1-50:1-50，更优选为1-30:1-30:1-30，在所限定的重量比的范围内，A与活性成分B混配取得协同增效的技术效果，安全剂化合物C起到很好的对作物的安全性改善。
所述除草组合物中A、B、C的质量百分含量占总量的1-95％，优选10-80％。通常，本发明的除草组合物包含1-95重量份的活性成分和5-99重量份的农药常规助剂。
本发明组合物的常规助剂可以为载体、表面活性剂等。
本文中的术语“载体”表示一种有机或无机、天然或合成的物质。它们有助于活性成分的施用，该载体一般是惰性的且必须是农业上可接受的，特别是被处理的植物所接受。载体可以是固体的，如陶土、天然或合成的硅酸盐、二氧化硅、树脂、蜡、固体肥料等；或者液体的，如水、醇类、酮类、石油馏分、芳烃或蜡烃、氯代烃、液化气等。
表面活性剂可包括乳化剂、分散剂或润湿剂，它可以是离子型或非离子型的。可提及的实例是聚丙烯酸的盐、木质素磺酸盐、苯酚磺酸或萘磺酸的盐、环氧乙烷与脂肪族醇或与脂族酸或与脂肪族胺与取代苯酚(特别是烷基苯酚或芳基苯酚)的聚合物、磺基琥珀酸盐、牛磺酸衍生物(特别是牛磺酸烷脂)及醇的磷酸酯或多羟乙基化的苯酚的磷酸酯、烷基磺酸盐、烷基芳基磺酸盐、烷基硫酸盐、月桂基醚硫酸盐、脂肪醇硫酸盐，以及硫酸化十六-、十七-和十八烷醇以及硫酸化脂肪醇乙二醇醚，此外还有萘或萘磺酸与苯酚和甲醛的缩合物、聚氧乙烯辛基苯基醚、乙氧基化异辛基酚、辛基酚或壬基酚、烷基苯基聚乙二醇醚、三丁基苯基聚乙二醇醚、三硬脂基苯基聚乙二醇醚、烷基芳基聚醚醇、醇和脂肪醇/氧化乙烯缩合物、乙氧基化蓖麻油、聚氧乙烯烷基醚、乙氧基化聚氧丙烯、月桂醇聚乙二醇醚缩醛、山梨醇酯、木素亚硫酸盐废液，以及蛋白质、变性蛋白、多糖(例如甲基纤维素)、疏水改性淀粉、聚乙烯醇、聚羧酸盐、聚烷氧基化物、聚乙烯胺、聚乙烯吡咯烷酮及其共聚物。至少需要一种表面活性剂存在，以有利于活性成分在水中的分散并有利于使它们能正确地施用于植物。
上述组合物也可含有各种其他的组分，如保护胶体、粘合剂、增稠剂、触变剂、渗透剂、 稳定剂、螯合剂、染料、着色剂和聚合物。
本发明的组合物可以由使用者在使用前经稀释或直接使用。其配制可由通常的加工方法制备，即将活性物质与液体溶剂或固体载体混合后，再加入表面活性剂如分散剂、稳定剂、湿润剂、粘合剂、消泡剂等中的一种或几种。
所述除草组合物的具体制剂为可湿性粉剂、可分散油悬浮剂、悬浮剂、悬乳剂、乳油、水分散粒剂(干悬浮剂)、水乳剂、微乳剂。
将上述配方中原药、安全剂、溶剂、乳化剂加入母液调制釜中，制得均匀油相，将去离子水、抗冻剂等混合均匀注入产品调制釜中，经高速搅拌，混合均匀制成本发明组合物透明或半透明的微乳剂产品。
简而言之，本发明的组合物可以和现有技术的配方中常规使用的固体和液体添加剂混合。
本发明的组合物可通过喷雾的方法被施用于待处理植物叶片上，即施用于杂草，特别是对作物生长有害的杂草侵扰或易侵扰影响的表面上。
当施用本发明的除草组合物时，获得了预料不到的增效效果，并且除草活性比使用单个除草剂的活性预期总和，以及单个除草剂单独活性更为显著。增效效果表现为施用量减少、更宽的杂草控制谱、除草作用更快、更持久，这些特性是杂草控制实践过程中所需要的。就所描述的特性来说，这些新组合物明显地优越于现有的除草剂。
本发明的除草组合物还具有下述优点：
(1)本发明提供了一组环境友好型除草剂，在环境中均易于降解。
(2)本发明除草组合物成本低、使用方便，其推广应用有巨大的经济效益和社会效益。
(3)与现有技术相比，本发明所述除草组合物可防除对ALS抑制剂、ACCase抑制剂产生抗性的稗草、牛筋草等禾本科杂草，对百草枯、草甘膦产生抗性的小飞蓬等阔叶杂草，是杂草抗性管理的有效方案。
具体实施方式
下列实施例并非限制本发明，而只是用来说明本发明是如何实现的。对于某些杂草，这些实施例显示出特别显著的有效性。
当R1是氢原子，R2是乙基，R3是三氟甲氧基，R4是氯原子，R5是甲基，R6是甲基，R7是氢原子时为A1；
当R1是氢原子，R2是甲基，R3是二氟甲氧基，R4是氯原子，R5是甲基，R6是甲基，R7是氢原子时为A2；
当R1是氢原子，R2是乙基，R3是乙氧基，R4是氯原子，R5是甲基，R6是甲基，R7是氢原子时为A3；
A、实施例
1)可分散油悬浮剂
当活性成分B为莠灭净，安全剂化合物C为双苯噁唑酸时
配方组成为：3％A1+50％莠灭净+1％双苯噁唑酸+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
2)可分散油悬浮剂
当活性成分B为莠灭净，安全剂化合物C为cyprosulfamide时
配方组成为：3％A2+50％莠灭净+1.5％cyprosulfamide+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
3)可分散油悬浮剂
当活性成分B为乙氧氟草醚，安全剂化合物C为双苯噁唑酸时
配方组成为：6％A3+10％乙氧氟草醚+1％双苯噁唑酸+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
4)可分散油悬浮剂
当活性成分B为乙氧氟草醚，安全剂化合物C为cyprosulfamide时
配方组成为：6％A1+10％乙氧氟草醚+2％cyprosulfamide+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
5)可分散油悬浮剂
当活性成分B为乙羧氟草醚，安全剂化合物C为cyprosulfamide时
配方组成为：6％A3+1％乙羧氟草醚+6％cyprosulfamide+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
6)可分散油悬浮剂
当活性成分B为异噁草松，安全剂化合物C为吡唑解草酯时
配方组成为：3％A1+30％异噁草松+1％吡唑解草酯+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
7)可分散油悬剂
当活性成分B为2甲4氯钠，安全剂化合物C为双苯噁唑酸时
配方组成为：3％A1+9％2甲4氯钠+2％双苯噁唑酸+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
8)可分散油悬浮剂
当活性成分B为甲磺草胺，安全剂化合物C为furilazole时
配方组成为：3％A1+15％甲磺草胺+1％furilazole+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
9)可分散油悬浮剂
当活性成分B为草甘膦，安全剂化合物C为吡唑解草酯时
配方组成为：3％A2+15％草甘膦+3％吡唑解草酯+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
10)可分散油悬浮剂
当活性成分B为草铵膦，安全剂化合物C为吡唑解草酯时
配方组成为：3％A1+20％草铵膦+1％吡唑解草酯+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
11)可分散油悬剂
当活性成分B为敌草隆，安全剂化合物C为双苯噁唑酸时
配方组成为：1.5％A3+30％敌草隆+0.75％双苯噁唑酸+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
12)可分散油悬浮剂
当活性成分B为苯嘧磺草胺，安全剂化合物C为cyprosulfamide时
配方组成为：6％A1+4％苯嘧磺草胺+6％cyprosulfamide+5％分散剂苯乙基苯酚聚氧乙烯醚磷酸酯三乙醇胺盐+5％乳化剂脂肪酸聚氧乙烯酯+8％乳化剂蓖麻油聚氧乙烯醚+2％增稠剂有机膨润土+油酸甲酯补足。
13)悬浮剂
当活性成分B为莠灭净，安全剂化合物C为cyprosulfamide时
配方组成为：3％A2+50％莠灭净+3％cyprosulfamide+5％分散剂木质素磺酸钠+2％润湿剂拉开粉+0.3％增稠剂黄原胶+5％防冻剂丙三醇+余量水补足。
加工设备：混料釜、胶体磨、砂磨机、剪切机等。
加工过程：将所有物料投入混料釜中，搅拌混合后过胶体磨，之后进入砂磨机三级砂磨，最后在剪切机中剪切均匀即为成品。
14)悬浮剂
当活性成分B为敌草隆，安全剂化合物C为吡唑解草酯时
配方组成为：1.5％A3+30％敌草隆+1.5％吡唑解草酯+5％分散剂木质素磺酸钠+2％润湿剂拉开粉+0.3％增稠剂黄原胶+5％防冻剂丙三醇+余量水补足。
加工设备：混料釜、胶体磨、砂磨机、剪切机等。
加工过程：将所有物料投入混料釜中，搅拌混合后过胶体磨，之后进入砂磨机三级砂磨，最后在剪切机中剪切均匀即为成品。
15)水分散粒剂
当活性成分B为莠灭净，安全剂化合物C为cyprosulfamide时
配方组成为：3％A1+50％莠灭净+1％cyprosulfamide+10％分散剂萘磺酸盐类+5％润湿剂拉开粉+1％崩解剂聚乙烯醇+填料硅藻土补足。
加工设备：气流粉碎机，犁刀式混合机，篮式造粒机，干燥箱，筛分机等。
加工过程：将上述物料混合均匀过气流粉碎，加入捏合，造粒后干燥，最后筛分得到成品。
16)水分散粒剂
当活性成分B为乙氧氟草醚，安全剂化合物C为双苯噁唑酸时
配方组成为：12％A3+20％乙氧氟草醚+6％双苯噁唑酸+10％分散剂萘磺酸盐类+5％润湿剂拉开粉+1％崩解剂聚乙烯醇+填料硅藻土补足。
加工设备：气流粉碎机，犁刀式混合机，篮式造粒机，干燥箱，筛分机等。
加工过程：将上述物料混合均匀过气流粉碎，加入捏合，造粒后干燥，最后筛分得到成品。
17)水分散粒剂
当活性成分B为甲磺草胺，安全剂化合物C为cyprosulfamide时
配方组成为：6％A3+30％甲磺草胺+2％cyprosulfamide+10％分散剂萘磺酸盐类+5％润湿剂拉开粉+1％崩解剂聚乙烯醇+填料硅藻土补足。
加工设备：气流粉碎机，犁刀式混合机，篮式造粒机，干燥箱，筛分机等。
加工过程：将上述物料混合均匀过气流粉碎，加入捏合，造粒后干燥，最后筛分得到成品。
B、药效试验
1)试验条件
1.1)、供试靶标
稗草(Echinochloa crusgalli)、牛筋草(Echinochloa crusgalli)采自广东惠州甘蔗田。田旋花(Convolvulus arvensis)采自山东青岛非耕地。小飞蓬(Conyza canadensis)采自湖北松滋非耕地。
上述杂草采用盆栽法培养，用180х140mm塑料营养钵，摆放于搪瓷盘中，内装从农田采回经风干过筛的表层土壤(4/5处)，土壤湿度初期均控制在20％，挑选籽粒饱满均一的杂草种子，用25℃温水浸泡6小时，在28℃生化培养箱(黑暗)中催芽，将刚刚露白的杂草种子均匀摆放在土壤表面，然后覆土0.7cm。药剂处理后置于可控日光温室内培养，定期在搪瓷盘中加入一定量的水，保持土壤湿润。
1.2)、培养条件
在可控日光温室内进行，温度18～30℃，自然光照，相对湿度57％～72％。
土壤类型为壤土，有机质含量为1.63％，pH＝7.1，碱解氮84.3mg/kg，速效磷38.5mg/kg，速效钾82.1mg/kg。
1.3)、仪器设备
3WP-2000型行走式喷雾塔，农业部南京农业机械研究所。GA110型万分之一电子天平(德国)；ZDR2000智能数据记录仪(杭州泽大仪器有限公司)；SPX型智能生化培养箱(宁波江南仪器厂)。
2)试验设计
2.1)、试剂
2.1.1)、试验药剂
所需活性成分B均为市售原药，A为本公司生产，参见专利CN201511030154.6。
原药均采用丙酮作溶剂，用含量0.1％乳化剂T-80水溶液稀释，现用现稀释。
2.2)、试验处理
2.2.1)、剂量设置
在确定A与活性成分B各组分配比或含量时，应从两种药剂的作用特点及其毒力等衡量，还要考虑该配方的主要使用目的。本研究在前期预试的基础上，设A、活性成分B单用及混 合用量分别见表格，共设计15组。以不含药剂、含相同溶剂及乳化剂的水作为空白对照。
2.2.2)、试验重复
每处理重复4次，每次每处理3盆，每盆播种杂草种子20粒，每处理共60株。
2.3)、处理方式
2.3.1)、处理时间和次数
试验共用药1次。待杂草2叶1心期，间苗，保持每盆内杂草15株，每处理保留45株，稗草、牛筋草继续培养至3叶1心期进行处理，田旋花、小飞蓬培养至4片真叶期进行处理。
2.3.2)、使用器械和用药方法
将培养好的试材均匀摆放在面积0.5m2的平台上，用3WP-2000型行走式喷雾塔茎叶喷雾，喷液量按30公斤/公顷计。喷雾压力0.3MPa。待全部药液喷完后，关闭气阀，30秒后，打开喷雾塔门，取出营养钵。然后打开气阀，喷清水50mL，清洗喷液管。
3)试验方法
采用盆栽法。杂草培养见1.1，参照《农药室内生物测定试验准则除草剂》进行。用药方法见2.3.2，采用茎叶处理法。
4)数据调查与统计分析
4.1)、调查方法
采用绝对数调查法，用刀片沿土壤表面切断存活杂草整株幼苗，用分析天平称量杂草鲜重。对于已经死亡的杂草，按鲜重为零计。
4.2)、调查时间和次数
处理后20天调查，共调查1次。
4.3)、数据统计分析
用Gowing法计算各处理混合组合的理论鲜重抑制率(E0＝X+Y-X*Y/100)，然后与实测抑制率(E)相比较，评价二者混用对杂草的联合作用类型，当E-E0值大于10％为增效作用、小于-10％为拮抗作用、在-10％～10％之间为加成作用。并根据实际防效和除草剂特点、配方的平衡性等因素确定最佳配比。
式中X为A用量为P时的鲜重抑制率；Y为活性成分B用量为Q时的鲜重抑制率。
统计结果见下表。
表1A与莠灭净混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000002
Figure PCTCN2017084919-appb-000003
表2A与乙氧氟草醚混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000004
Figure PCTCN2017084919-appb-000005
表3A与异噁草松混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000006
表4A与2甲4氯钠混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000007
表5A与草甘膦混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000008
Figure PCTCN2017084919-appb-000009
表6A与草铵膦混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000010
表7A与敌草隆混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000011
表8A与苯嘧磺草胺混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000012
Figure PCTCN2017084919-appb-000013
表9A与甲磺草胺混用对杂草的实际防效以及联合作用效应(Gowing法)
Figure PCTCN2017084919-appb-000014
C、大田示范
利用实施例制得的除草剂组合物防除甘蔗田杂草试验。
在广东、广西、福建、海南4个甘蔗区20个试验点进行示范性推广试验。不同示范区甘蔗品种详见表10。
表10不同示范区甘蔗品种情况
示范区 甘蔗品种
广东惠州 粤糖89113
广西柳州 柳糖2号
福建宁德 粤农91-854
海南东方 新台糖22号
施药方法：甘蔗3叶后，杂草3-5叶期，手动喷雾器，兑水量15公斤/667m2，采用茎叶喷雾均匀喷雾，具体试验药剂及剂量见表11，小区面积50平方米，每处理重复4次。施药后45天调查防除效果见表11，甘蔗安全性情况见表12。
Figure PCTCN2017084919-appb-000015
表11大田示范效果情况
Figure PCTCN2017084919-appb-000016
Figure PCTCN2017084919-appb-000017
表12大田示范甘蔗安全性情况
Figure PCTCN2017084919-appb-000018
Figure PCTCN2017084919-appb-000019
注：各示范点内杂草群落类型：惠州：稗草+牛筋草+马唐+藜+反枝苋；柳州：稗草+牛筋草+藜+反枝苋；宁德：稗草+牛筋草+藜；东方：稗草+牛筋草+藜；保定：稗草+牛筋草+马唐+反枝苋+藜。
经过大量试验和探索，本发明意外地发现，A与活性成分B、安全剂化合物C混用，用于甘蔗田苗后防除禾本科杂草，具有令人惊讶的、意想不到的增效作用，尤其是对稗草、牛筋草等禾本科杂草、藜、反枝苋等阔叶类杂草具有尤其明显的增效作用，可降低用药量，并对甘蔗安全，降低对环境的污染，且合理复配降低了农用成本，具有很好的应用前景。
D、大田示范
利用实施例制得的除草剂组合物防除免耕田小飞蓬试验。
在湖北、江苏、安徽3省15个试验点进行示范性推广试验。
施药方法：小飞蓬起身前，手动喷雾器，兑水量15公斤/667m2，采用茎叶喷雾均匀喷雾，具体试验药剂及剂量见表13，小区面积50平方米，每处理重复4次。施药后45天调查防除效果见表13。
Figure PCTCN2017084919-appb-000020
表13大田示范效果情况
Figure PCTCN2017084919-appb-000021
Figure PCTCN2017084919-appb-000022
经过大量试验和探索，本发明意外地发现，A与活性成分B混用，对草甘膦抗性小飞蓬具有令人惊讶的、意想不到的增效作用，可降低用药量，降低对环境的污染，且合理复配降低了农用成本，具有很好的应用前景。

Claims (9)

  1. 一种含吡唑酮类化合物的除草组合物，其特征在于，包括除草有效量的活性成分A、活性成分B、以及安全剂化合物C，其中，
    活性成分A为下列通式中的一种：
    Figure PCTCN2017084919-appb-100001
    R1是氢原子，甲基，乙基，环丙基；
    R2是甲基，乙基，异丙基；
    R3是乙氧基，氟乙氧基，二氟乙氧基，三氟乙氧基，吡唑基；
    R4是氯原子，甲基；
    R5、R6、R7是烷基，烷氧基，卤素取代的烷基，卤素取代的烷氧基；
    活性成分B选自以下化合物中的一种或多种：
    1)三嗪类：莠灭净、西玛津、环嗪酮、扑草净；
    2)二苯醚类：乙氧氟草醚、乙羧氟草醚、三氟羧草醚；
    3)异噁草松；
    4)苯氧羧酸类：2甲4氯钠、2,4-滴丁酯；
    5)甲磺草胺；
    6)有机磷类：草甘膦、草铵膦；
    7)取代脲类：敌草隆、灭草隆、利谷隆、绿麦隆；
    8)苯嘧磺草胺；
    9)敌草快；
    安全剂化合物C选自以下化合物中的一种或多种：
    C1：双苯噁唑酸
    C2：cyprosulfamide
    C3：吡唑解草酯
    C4：解毒喹
    C5：赤霉酸
    C6：furilazole
    C7：N-(2-2甲氧基苯甲酰基)-4-[(甲基氨基羰基)氨基]苯磺酰胺。
  2. 根据权利要求1所述的含吡唑酮类化合物的除草组合物，其特征在于，
    所述活性成分A中R1是氢原子；R2是甲基，乙基；R3是乙氧基，氟乙氧基，二氟乙氧基，三氟乙氧基，吡唑基；R4是氯原子；R5、R6、R7是烷基，烷氧基，卤素取代的烷基，卤素取代的烷氧基；
    所述活性成分B为莠灭净、乙氧氟草醚、乙羧氟草醚、异噁草松、2甲4氯钠、甲磺草胺、草甘膦、草铵膦、敌草隆、苯嘧磺草胺中一种或多种；
    所述安全剂化合物C为双苯噁唑酸、cyprosulfamide、吡唑解草酯、furilazole中一种或多种。
  3. 根据权利要求1所述的含吡唑酮类化合物的除草组合物，其特征在于，所述活性成分A中R1是氢原子，R2是甲基或乙基，R3是乙氧基、二氟甲氧基或三氟甲氧基，R4是氯原子，R5是甲基，R6是甲基，R7是氢原子。
  4. 根据权利要求1-3任意一项所述的含吡唑酮类化合物的除草组合物，其特征在于，A、B、C的重量比为1-100:1-100:1-100，优选为1-50:1-50:1-50，更优选为1-30:1-30:1-30。
  5. 根据权利要求1-3任意一项所述的含吡唑酮类化合物的除草组合物，其特征在于，所述除草组合物中A、B、C的质量百分含量占总量的1-95％，优选10-80％。
  6. 根据权利要求1-3任意一项所述的含吡唑酮类化合物的除草组合物，其特征在于，所述除草组合物中还包含农药常规助剂。
  7. 根据权利要求6所述的含吡唑酮类化合物的除草组合物，其特征在于，所述农药常规助剂包括载体、表面活性剂。
  8. 根据权利要求1-3任意一项所述的含吡唑酮类化合物的除草组合物，其特征在于，所述除草组合物的具体制剂为可湿性粉剂、可分散油悬浮剂、悬浮剂、悬乳剂、乳油、水分散粒剂、水乳剂或微乳剂。
  9. 一种如权利要求1-8任意一项所述含吡唑酮类化合物的除草组合物在防治甘蔗田中杂草中的应用。
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