Herbicide composition and application thereof
By combining the three herbicides, 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid, difluorosulforon and fluzosulforon, a herbicide composition with a wide herbicide spectrum and significant weed control effect was formed, which solved the problem of degradation of prevention and weed resistance caused by long-term, large-scale and single use of herbicides, and achieved efficient and economical weed prevention effect.
Patent Information
- Application Number
- CN202411859687.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-17
- Publication Date
- 2025-04-08
AI Technical Summary
Long-term, large-scale, single use of herbicides leads to a significant decrease in the prevention effect and leads to the occurrence of weed resistance.
Three herbicides, 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid, difluorosulforamide and fluzosulforon, were combined to form a herbicide composition with a wide herbicide spectrum and significant effect on weed control.
Through compound use, the prevention effect of annual grass family and broadleaf weeds has been significantly improved, delayed the occurrence of weed resistance, and reduced the dosage of pesticides, reducing farmers' medication costs and environmental impact.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of herbicides, and in particular to a herbicide composition and application thereof. Background Art
[0002] Herbicides can be used to control weeds in farmland or kill weeds or shrubs in non-agricultural land. 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid, florasulam, flucarbazone-sodium, etc. are all herbicides known in the art.
[0003] Among them, the structural formula of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid is as follows: .
[0004] 4-Amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives are new hormone herbicides of the aryl picolinate class, which simulate the effects of large-scale secretion of plant growth hormones, causing overstimulation of specific auxin regulatory genes, interfering with multiple growth processes of sensitive plants. It is absorbed by plant stems, leaves and roots, binds to hormone receptors in the plant body, stimulates excessive division of plant cells and blocks the conduction tissue, and finally causes the plant to die due to nutrient depletion.
[0005] Florasulam, CAS registration number: 145701-23-1, molecular formula: C 12 H 8 F 3 N 5 O 3 S, its structural formula is as follows: .
[0006] Bispyribac is a triazole pyrimidine sulfonamide herbicide, an acetolactate synthase (ALS) inhibitor, highly selective for wheat crops and lawns, and can be applied to winter wheat, winter wheat, spring wheat, spring barley, lawns, onions, grasslands, pastures, etc. In actual application, it is mainly used for post-emergence control of broad-leaved weeds in winter wheat fields such as cleavers, chickweed, Polygonum weeds, and Asteraceae weeds.
[0007] Flucarbazone-sodium, CAS registration number 181274-17-9, molecular formula: C 12 H 10 F 3 N 4 NaO 6S. Its structural formula is shown below: .
[0008] Fluzosulfuron-methyl is a sulfonylurea systemic, highly effective wheat field herbicide that has significant preventive effects on grass weeds such as wild oats, brome, and alopecuroides, as well as a variety of dicotyledonous weeds.
[0009] Due to the long-term, large-scale, single and unreasonable use of herbicides, the control effect of herbicides has been significantly reduced, and weed resistance has occurred. Reasonable compounding or mixing of herbicide compounds may effectively delay the occurrence of weed resistance, expand the weed control spectrum, and improve the weed control effect, which is one of the directions for optimizing the weed control effect. At present, no solution has been found to compound 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid (or its agricultural salts, esters and amide derivatives), bispyribac and fluazifop-butyl.
[0010] In view of this, the present invention is proposed. Summary of the invention
[0011] In order to solve the above technical problems, the present invention provides a herbicide composition with a broad weed control spectrum and significant weed control effect and its application. The active ingredients of the herbicide composition include bispyribac and fluazifop-butyl, and also include 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives. It shows excellent synergistic effect, can reduce the dosage of pesticides, and thus reduce the cost of pesticides for farmers and the degree of impact on the environment.
[0012] Specifically, the technical solution of the present invention is as follows: In a first aspect, the present invention provides a herbicide composition comprising effective active ingredients and adjuvants, wherein the effective active ingredients include bispyribac and fluazifop-butyl, and also include 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives.
[0013] The present invention unexpectedly discovered during the research process that the compound use of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid (or its agricultural salts, esters and amide derivatives), bispyribac and fluazifop-butyl herbicides having different structural types and action mechanisms has an obvious synergistic effect, can improve the control effect of these three components on annual grass and broad-leaved weeds to a greater extent, and can expand the weed control spectrum, and has a significant weed control effect.
[0014] Preferably, based on 1 part by weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, the amount of florasulam is 0.1-30 parts by weight, and the amount of fluazifop-butyl is 0.1-60 parts by weight.
[0015] Preferably, based on 1 part by weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, the amount of florasulam is 0.1-20 parts by weight, and the amount of fluazifop-butyl is 0.2-50 parts by weight.
[0016] Preferably, based on 1 part by weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, the amount of florasulam is 0.2-20 parts by weight, and the amount of fluazifop-butyl is 0.5-40 parts by weight.
[0017] Preferably, based on 1 part by weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, the amount of florasulam is 0.2-10 parts by weight, and the amount of fluazifop-butyl is 0.5-40 parts by weight.
[0018] Preferably, the mass percentage content of the active ingredient of the present invention in the herbicide composition is 1-99%, preferably 5-80%, more preferably 5-60%.
[0019] Preferably, the adjuvants of the present invention include pesticide-acceptable surfactants, carriers and safeners.
[0020] Preferably, the herbicide composition of the present invention is in the form of emulsifiable concentrate, water emulsion, water suspension, oil suspension, suspoemulsion, dispersible oil suspension, microcapsule suspension, wettable powder, soluble powder, water dispersible granules or soluble granules.
[0021] In a second aspect, the present invention provides use of the herbicide composition in controlling annual grass and / or broadleaf weeds.
[0022] Preferably, the application comprises: using the herbicide composition for controlling annual grass and / or broadleaf weeds in wheat fields.
[0023] Further preferably, the weeds are one or more of wild oats, brome, barnyard grass, aesculus tauschii, hard grass, alopecuroides, sophora japonica, shepherd's purse, cleaver, magnolia bark, rhubarb, chickweed and veronica.
[0024] More preferably, the weeds are shepherd's purse, descurainia, wild oats and brome.
[0025] Beneficial effects: The present invention provides a herbicide composition and its application. The active ingredients of the herbicide composition include bispyribac and fluazifop-butyl, and also include 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salt, ester and amide derivatives. The present invention compounds three active ingredients, namely 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid (or its agricultural salt, ester and amide derivative), bispyribac and fluazifop-butyl. According to indoor combined toxicity test, the compounding of the three can effectively expand the weed control spectrum of the product and have obvious synergistic effect; according to field efficacy test, the compounding has excellent control effect on annual grass weeds and broad-leaved weeds in wheat fields, is safe for wheat, and is suitable for agricultural promotion and use. DETAILED DESCRIPTION
[0026] The invention provides a herbicide composition, wherein the effective active ingredients of the herbicide composition contain 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid (or its agricultural salt, ester and amide derivatives), bispyribac and fluazifop-butyl.
[0027] Although in the present invention, the active ingredients can show significant synergistic effect as long as they include 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid (or its agricultural salts, esters and amide derivatives), florasulam and fluazifop-methyl, from the perspective of further improving the synergistic effect: the weight ratio of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, florasulam and fluazifop-methyl is 1:0.1-30:0.1-60; preferably, 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid (or its agricultural salts, esters and amide derivatives), ... Preferably, the weight ratio of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, florasulam and fluzosulfuron is 1:0.1-20:0.2-50; preferably, the weight ratio of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, florasulam and fluzosulfuron is 1:0.2-20:0.5-40; preferably, the weight ratio of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, florasulam and fluzosulfuron is 1:0.2-10:0.5-40.
[0028] In the herbicide composition provided by the present invention, the content of the active ingredient in the herbicide composition can vary in a wide range. Specifically, the content of the active ingredient in the composition is 1-99% by weight, preferably 5-80% by weight, and more preferably 5-60% by weight. Specific examples of the content of the active ingredient in the composition include: 1 weight%, 2 weight%, 3 weight%, 4 weight%, 5 weight%, 6 weight%, 7 weight%, 8 weight%, 9 weight%, 10 weight%, 11 weight%, 12 weight%, 13 weight%, 14 weight%, 15 weight%, 16 weight%, 17 weight%, 18 weight%, 19 weight%, 20 weight%, 21 weight%, 22 weight%, 23 weight%, 24 weight%, 25 weight%, 26 weight%, 27 weight%, 28 weight%, 29 weight%, 30 weight%, 31 weight%, 32 weight%, 33 weight%, 34 weight%, 35 weight%, 36 weight%, 37 weight%, 38 weight%, 39 weight%, 40 weight%, 41 weight%, 42 weight%, 43 weight%, 44 weight%, 45 weight%, 46 weight%, 47 weight%, 48 weight%, 49 weight%, 50 weight %, 51 weight %, 52 weight %, 53 weight %, 54 weight %, 55 weight %, 56 weight %, 57 weight %, 58 weight %, 59 weight %, 60 weight %, 61 weight %, 62 weight %, 63 weight %, 64 weight %, 65 weight %, 66 weight %, 67 weight %, 68 weight %, 69 weight %, 70 weight %, 71 weight %, 72 weight %, 73 weight %, 74 weight %, 75 weight %, 76 weight %, 77 weight %, 78 weight %, 79 weight %, 80 weight %, 81 weight %, 82 weight %, 83 weight %, 84 weight %, 85 weight %, 86 weight %, 87 weight %, 88 weight %, 89 weight %, 90 weight %, 91 weight %, 92 weight %, 93 weight %, 94 weight %, 95 weight %, 96 weight %, 97 weight %, 98 weight %, 99 weight %, etc., and the numerical range formed by any two of them.
[0029] The herbicide composition of the present invention generally contains, in addition to the active ingredient, a surfactant, a carrier and a safener which are acceptable in pesticides.
[0030] The above-mentioned surfactant can be any surfactant known in the field of pesticide formulations. In the present invention, it is preferably one or more of an emulsifier, a dispersant and a wetting agent.
[0031] The above-mentioned emulsifier can be various emulsifiers well known in the field of pesticide formulations. Specifically, the emulsifier can be one or more of calcium dodecylbenzene sulfonate, triphenyl phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, alkylphenol polyoxyethylene polyoxypropylene ether, fatty amine, ethylene oxide adduct of fatty amide, fatty acid polyoxyethylene ester, rosin acid ethylene oxide adduct, polyol fatty acid ester and ethylene oxide adduct thereof, styrylphenyl polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, terminal hydroxyl polyoxyethylene polyoxypropylene ether, styrylphenol formaldehyde resin, polyoxyethylene polyoxypropylene ether and castor oil polyoxyethylene ether.
[0032] The above-mentioned dispersant can be various dispersants known in the field of pesticide formulations. Specifically, the dispersant can be one or more of acrylic acid homopolymer sodium salt, maleic acid disodium salt, naphthalenesulfonic acid formaldehyde condensate sodium salt, rosin block polyoxyethylene ether polyoxypropylene ether sulfonate, terminal hydroxyl polyoxyethylene polyoxypropylene ether block copolymer, triphenyl phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether phosphate, p-hydroxyphenyl lignin sulfonate sodium salt and calcium lignin sulfonate.
[0033] The wetting agent can be any wetting agent known in the field of pesticide formulations. Specifically, the wetting agent can be one or more of sodium dodecyl sulfate, sodium secondary alkyl sulfate, sodium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether, alkyl naphthalene sulfonate, and alkylphenol resin polyoxyethylene ether sulfate.
[0034] The other carriers except the above-mentioned surfactants can be various carriers known in the field of pesticide formulations, including various silicates, carbonates, sulfates, oxides, phosphates, plant carriers, and synthetic carriers. Specifically, for example, the carrier can be one or more of white carbon black, kaolin, diatomaceous earth, clay, talc, organic bentonite, pumice, titanium dioxide, dextrin, cellulose powder, light calcium carbonate, soluble starch, corn starch, sawdust powder, urea, amine fertilizer, a mixture of urea and amine fertilizer, glucose, maltose, sucrose, anhydrous potassium carbonate, anhydrous sodium carbonate, anhydrous potassium bicarbonate, anhydrous sodium bicarbonate, attapulgite, a mixture of anhydrous potassium carbonate and anhydrous potassium bicarbonate, and a mixture of anhydrous sodium carbonate and anhydrous sodium bicarbonate.
[0035] The herbicide composition of the present invention may further contain various formulation adjuvants commonly used in the field of pesticide formulations. Specifically, the formulation adjuvant may be one or more of a solvent, a cosolvent, a thickener, an antifreeze agent, a protective agent, a defoaming agent, a disintegrant, a stabilizer, a safener, a preservative and a binder.
[0036] The above-mentioned solvent may be any solvent known in the field of pesticide formulations. Specifically, the solvent may be one or more of an organic solvent, vegetable oil, mineral oil, solvent oil and water.
[0037] The organic solvent includes one or more of N-methylpyrrolidone, tetrahydrofuran, dimethyl sulfoxide, N,N-dimethyldecylamide, N,N-dimethylformamide, trimethylbenzene, tetramethylbenzene, xylene, toluene, octane, heptane, methanol, isopropanol, n-butanol, tetrahydrofurfuryl alcohol, tributyl phosphate, 1,4-dioxane and cyclohexanone.
[0038] The vegetable oil includes one or more of methylated vegetable oil, rosin-based vegetable oil, turpentine oil, epoxidized soybean oil, soybean oil, peanut oil, rapeseed oil, castor oil, corn oil and pine nut oil.
[0039] The mineral oil includes one or more of liquid wax, motor oil, kerosene and lubricating oil.
[0040] At the same time, the above solvents can also be used as co-solvents.
[0041] The antifreeze agent may be any antifreeze agent known in the field of pesticide formulations. In the present invention, the antifreeze agent is preferably one or more of ethylene glycol, propylene glycol, glycerol and urea.
[0042] The thickener may be any thickener known in the field of pesticide formulations. Specifically, the thickener may be one or more of xanthan gum, polyvinyl alcohol, polypropylene alcohol, polyethylene glycol, white carbon black, diatomaceous earth, kaolin, clay, sodium alginate, magnesium aluminum silicate, sodium aluminum silicate, carboxymethyl cellulose, sodium hydroxypropyl cellulose and organic bentonite.
[0043] The defoaming agent can be any defoaming agent known in the field of pesticide formulations. In the present invention, it is preferably one or more of organosiloxane, tributyl phosphate and silicone.
[0044] The stabilizer is selected from one or more of triphenyl phosphite, epichlorohydrin and acetic anhydride.
[0045] The preservative is selected from one or more of benzoic acid, sodium benzoate, 1,2-benzisothiazolin-3-one (BIT for short), kasone and potassium sorbate.
[0046] The safener is selected from one or more of clofonetoxane or ester, dichloropropane, fenpyroxetine, and pyraclostrobin.
[0047] According to the present invention, the formulation of the herbicide composition can be various formulations commonly used in the art, for example, the formulation of the herbicide composition can be emulsifiable concentrate, aqueous emulsion, aqueous suspension, oil suspension, suspoemulsion, dispersible oil suspension, microcapsule suspension, wettable powder, soluble powder, water dispersible granules or soluble granules. The above formulations can be prepared by conventional methods in the art, and the present invention has no special requirements.
[0048] Preferably, the emulsifiable concentrate preparation is composed of 1-95% active ingredient, 0-10% safener, 0-20% cosolvent, 1-30% emulsifier, and the solvent is supplemented to 100% by weight.
[0049] The preparation method of the above emulsifiable concentrate preparation may include, for example, mixing and stirring the active components, safener, solvent, co-solvent and emulsifier to form a uniform and transparent oil phase, thereby obtaining the emulsifiable concentrate preparation.
[0050] Preferably, the aqueous emulsion or microemulsion is composed of 1-95% active ingredient, 0-10% safener, 1-30% emulsifier, 0-30% cosolvent, 1-30% solvent, 0-10% antifreeze agent, 0-10% thickener, and water to 100% by weight.
[0051] Preferably, the method for preparing the aqueous emulsion may include, for example, mixing the active ingredient, safener, emulsifier, cosolvent and solvent to form a uniform oil phase; mixing water, thickener, antifreeze agent, etc. to form a uniform water phase. Under high-speed shearing, the water phase is added to the oil phase or the oil phase is added to the water phase to form an aqueous emulsion with good dispersibility.
[0052] Preferably, the aqueous suspension concentrate is composed of 1-95% active ingredient, 0-10% safener, 1-30% surfactant, 1-10% antifreeze agent, 0.1-5% thickener, and water to 100% by weight.
[0053] Preparation method of water suspension: using water as medium, add active ingredients, safener, surfactant and auxiliary agent into sand mill, grind to a certain particle size, filter. Then add measured thickener into the ground mother liquor, shear and disperse evenly to make water suspension.
[0054] Preferably, the suspoemulsion is composed of 1-95% active ingredient, 0-10% safener, 1-30% solvent, 1-30% emulsifier, 1-30% surfactant, 1-10% antifreeze, 0.1-5% thickener, and water to 100% by weight.
[0055] Preparation method of suspoemulsion: using water as medium, add two active components, safener, surfactant and auxiliary agent into sand mill, grind to a certain particle size, filter, complete the preparation of suspension component, and set aside; prepare the emulsion component according to the above-mentioned water emulsion preparation method for the other active component; mix the suspension component and emulsion component evenly according to the proportion to prepare suspoemulsion. Then add the measured thickener into the ground mother liquor, disperse evenly, and prepare suspoemulsion.
[0056] Preferably, the dispersible oil suspension comprises, by weight percentage, 1-95% active ingredient, 0-10% safener, 1-30% surfactant, 1-10% antifreeze agent, 0.1-5% thickener, and oil to make up to 100%.
[0057] Preparation method of dispersible oil suspension: using oil as medium, add active components, safener, surfactant and auxiliary agent into sand mill, grind to a certain particle size, filter. Then add measured thickener into the ground mother liquor, shear and disperse evenly, and make dispersible oil suspension.
[0058] Preferably, the microcapsule suspension is composed of 1-95% active ingredient, 0-10% safener, 1-30% emulsifier, 0-30% cosolvent, 1-30% solvent, 0-30% capsule material, 0-10% antifreeze agent, 0-10% thickener, and water to 100%.
[0059] Preferably, the preparation method of the microcapsule suspension may include, for example, mixing the active ingredient, safener, emulsifier, cosolvent and solvent to form a uniform oil phase; mixing water, thickener, antifreeze agent, etc. to form a uniform water phase. Under high-speed shearing, the water phase is added to the oil phase or the oil phase is added to the water phase to form an emulsion with good dispersibility, and then the microcapsule suspension is formed through an encapsulation reaction.
[0060] Preferably, the water dispersible granules or wettable powders are composed of 1-95% active ingredient, 0-10% safener, 1-30% surfactant, and other carriers to make up to 100% by weight.
[0061] The preparation method of water-dispersible granules is as follows: the active components, safener, dispersant, wetting agent and carrier are mixed evenly, and then crushed to a certain particle size by air flow, and then water is added for kneading, and finally added to a granulator for granulation, and water-dispersible granules or soluble granules can be obtained after drying.
[0062] The preparation method of wettable powder is: fully mix the active components, safeners, various adjuvants and other carriers and other fillers, and grind them with an ultrafine grinder.
[0063] The herbicide composition provided by the present invention exhibits an obvious synergistic effect. The mixed composition significantly improves the control effect compared with its single agent, reduces the dosage of pesticides, and thus reduces the cost of pesticides for farmers and the degree of impact on the environment.
[0064] The herbicide composition provided by the present invention has a wide weed control spectrum. The herbicide composition provided by the present invention can control multiple weeds at the same time, is easy to use and highly effective, and has good control effects on annual grass and broad-leaved weeds in wheat fields.
[0065] The herbicide composition provided by the present invention is a composite combination of herbicides with different action mechanisms, so that the herbicidal properties of each component herbicide are well complemented, and the occurrence and development of weed resistance can be effectively delayed. Furthermore, the present invention provides a preparation prepared by the herbicide composition of the present invention.
[0066] Furthermore, the present invention also provides the use of the above-mentioned herbicide composition in controlling annual grass and broad-leaved weeds in wheat fields.
[0067] The above-mentioned weeds can be one or more of wild oats, brome, aestivum, bluegrass, foxtail millet, sowthistle, shepherd's purse, cleaver, marigold, sedge, sedge, chickweed and veronica.
[0068] In particular, the inventors of the present invention unexpectedly discovered that the herbicide composition provided by the present invention has extremely significant control effects on shepherd's purse, sophora japonica, chickweed, alopecuroides, wild oats, and brome, and is also highly safe for crops (such as wheat).
[0069] The herbicide composition of the present invention can be provided in the form of a finished preparation, that is, the various substances in the composition have been mixed; it can also be provided in the form of a separate preparation, which can be mixed in a bucket or tank before use and selectively mixed with water for dilution according to the required concentration of the active substance.
[0070] The composition of the present invention may also be used in admixture with other compounds having fungicidal, insecticidal or herbicidal properties, or with nematicides, protectants, growth regulators, plant nutrients or soil conditioners.
[0071] According to the present invention, the specific application method of the herbicide composition is generally to treat the whole wheat field with the herbicide composition of the present invention during the wheat 3-leaf to jointing stage. The application method is stem and leaf spraying, and the application method is simple.
[0072] The usage amount of the herbicide composition provided by the present invention can mitigate the influence of climate by preparing it into a suitable dosage form.
[0073] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0074] The endpoints and any values of the ranges disclosed in this specification are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of each range, the endpoint values of each range and the individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.
[0075] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "specific implementations", or "some specific implementations" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the embodiment of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, without contradiction.
[0076] In the examples provided in this specification, if no specific techniques or conditions are specified, the techniques or conditions described in the literature in this field or the product instructions are used. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased through regular channels.
[0077] The following examples and comparative examples were prepared using the following technical drugs: 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester technical drug, purity of 93%, produced by Corteva Agricultural Science and Technology Co., Ltd.; bispyribac technical drug, purity of 98%, produced by Corteva Agricultural Science and Technology Co., Ltd.; fluazifop-sodium technical drug, purity of 98%, produced by Shandong Binnong Technology Co., Ltd. In the following examples, the amount of the herbicidal composition used is the actual amount, that is, the amount after deducting impurities.
[0078] Example 1 This example provides a herbicidal composition (16 wt % 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester·bifenazol·fluazifop-methyl emulsifiable concentrate).
[0079] The formula is: 25g of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, 10g of bispyribac, 125g of fluazifop-butyl, 20g of pyraclostrobin, 400g of dimethyl sulfoxide, 40g of calcium dodecylbenzenesulfonate (emulsifier), 60g of tristyrylphenol polyoxyethylene ether (emulsifier), and make up to 1kg of solvent oil (solvent).
[0080] The preparation method is as follows: the above-mentioned weight amounts of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam, fluazifop-butyl, pyraclostrobin, solvent oil, calcium dodecylbenzenesulfonate, castor oil polyoxyethylene ether, and dimethyl sulfoxide are mixed into a uniform oil phase to obtain an emulsifiable concentrate containing 16 weight % of the active ingredient.
[0081] Example 2 This example provides a herbicidal composition (23 wt % 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester·bifenazol·fluazifop-ethyl emulsion in water).
[0082] The formula is: 10g of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, 20g of bispyribac, 200g of fluazifop-methyl, 300g of dimethyl sulfoxide, 10g of chlorpyrifos, 40g of castor oil polyoxyethylene ether, 40g of fatty alcohol polyoxyethylene ether, 50g of 1,2-propylene glycol, 10g of xanthan gum, and make up to 1kg with water.
[0083] The preparation method comprises the following steps: mixing the above-mentioned 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam, fluazifop-sodium, dimethyl sulfoxide, fenthiocarb, castor oil polyoxyethylene ether and fatty alcohol polyoxyethylene ether into a uniform oil phase; mixing ethylene glycol, xanthan gum and water into a uniform water phase; and adding the oil phase into the water phase under high-speed stirring or shearing to form a water emulsion with good dispersibility containing 23% by weight of the active ingredient.
[0084] Example 3 This example provides a herbicidal composition (18.5 wt % 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester·bifenazol·fluazifop-methyl dispersible oil suspension concentrate).
[0085] The formula is: 5g of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, 35g of bispyribac, 145g of fluazifop-methyl, 20g of clofonate-methyl, 60g of polyoxyethylene fatty acid ester, 40g of sorbitan polyoxyethylene ether, 40g of organic bentonite, and methyl oleate is made up to 1kg.
[0086] The preparation method is as follows: using methyl oleate as a medium, adding the above-mentioned 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam, fluazifop-butyl, clofonate-methyl, polyoxyethylene fatty acid ester, sorbitol polyoxyethylene ether, and organic bentonite into a sand mill and grinding them into fine powder, thereby obtaining an oil suspension containing 18.5% by weight of the active ingredient.
[0087] Example 4 This example provides a herbicidal composition (30 wt % 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester·bifenazol·fluazifop-methyl suspension).
[0088] The formula is: 40g of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, 50g of bispyribac, 210g of fluazifop-methyl, 40g of dichloropropyleneamine, 60g of naphthalenesulfonate (dispersant), 40g of alkyl polyoxyethylene ether (wetting agent), 150g of glycerol (antifreeze), 60g of sodium alginate (thickener), 5g of silicone defoamer, and water is added to 1000g.
[0089] The preparation method is as follows: using water as a medium, adding the above-mentioned weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam, fluazifop-sodium, dichloropropyleneamine, naphthalenesulfonate, alkyl polyoxyethylene ether, glycerol, sodium alginate, silicone defoamer and water into a shearing kettle, shearing evenly and then grinding into a sand mill kettle to obtain a suspension containing 30 weight % of the active ingredient.
[0090] Example 5 This example provides a herbicidal composition (19.5 wt % 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester·bifenazol·fluazifop-methyl suspoemulsion).
[0091] The formula is: 15g of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, 30g of bispyribac, 150g of fluazifop-butyl, 300g of solvent oil, 15g of pyraclostrobin, 80g of calcium dodecylbenzenesulfonate, 80g of fatty alcohol polyoxyethylene ether, 30g of xanthan gum, 60g of propylene glycol, and make up to 1kg with water.
[0092] The preparation method comprises the following steps: using water as a medium, adding the above-mentioned fluazifop-sodium, calcium dodecylbenzenesulfonate, fatty alcohol polyoxyethylene ether, xanthan gum and propylene glycol into a sand mill and grinding them into fine powder, so as to obtain a fluazifop-sodium aqueous suspension; fully mixing 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam, pyraclostrobin, solvent oil, calcium dodecylbenzenesulfonate and fatty alcohol polyoxyethylene ether to form an oil phase; and adding the oil phase into the fluazifop-sodium aqueous suspension to obtain a suspoemulsion containing 19.5% by weight of the active ingredient.
[0093] Example 6 This example provides a herbicidal composition (66 wt % of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester·bifenazol·fluazifop-methyl water dispersible granules).
[0094] The formula is: 80g of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, 80g of bispyribac, 500g of fluazifop-methyl, 80g of clofonetic acid, 50g of sodium dodecyl sulfate, 100g of sodium salt of acrylic acid homopolymer, 50g of starch, and diatomaceous earth is added to make up to 1kg.
[0095] The preparation method is as follows: the above-mentioned 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam, fluazifop-methyl, quinoline, sodium dodecyl sulfate, sodium salt of acrylic acid homopolymer, starch and diatomaceous earth are mixed and crushed, and then extruded and granulated to prepare water-dispersible granules containing 66% by weight of the active ingredient.
[0096] Example 7 This example provides a herbicidal composition (58% by weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester·bifenazol·fluazifop-methyl wettable powder).
[0097] The formula is: 100g of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, 80g of bispyribac, 400g of fluazifop-methyl, 100g of quinoline, 50g of sodium dodecyl sulfate (wetting agent), 100g of naphthalenesulfonate (dispersant), and 1000g of light calcium carbonate (filler); The preparation method is as follows: the above-mentioned weight amounts of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam, fluazifop-sodium, sodium dodecyl sulfate, naphthalenesulfonate and light calcium carbonate are mixed and crushed to prepare a wettable powder containing 58 weight % of active ingredients.
[0098] Comparative Example 1 Water dispersible granules of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester with an active ingredient content of 10%.
[0099] Comparative Example 2 A suspension concentrate of florasulam with an active ingredient content of 50g / L.
[0100] Comparative Example 3 Fluazuron-methyl water dispersible granules with an active ingredient content of 70%.
[0101] Test Example 1 This test example is an indoor combined action determination test.
[0102] Test targets: Artemisia selengensis and wild oats.
[0103] Preparation of the agent: 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester in Comparative Example 1 is dissolved in an appropriate amount of N,N-dimethylformamide, and the bispyribac technical drug in Comparative Example 2 and the fluazifop-butyl technical drug in Comparative Example 3 are dissolved in an appropriate amount of dimethyl sulfoxide, and a 0.1% Tween 80 aqueous solution is used to prepare the required concentration for use.
[0104] Test method: Use the greenhouse pot method to sow weed seeds in small pots filled with 3 / 5 seedling substrate (field soil: nutrient soil: vermiculite = 3:1:1), sow 20 seeds in each pot, and cover with 1~2mm of soil after sowing. Water by bottom penetration method. After the water completely soaks the seedling substrate, pour out the excess water in the tray and transfer it to the artificial climate room for cultivation. When the weeds grow to the 2~4 leaf stage, use ASS-5 walking spray tower to spray the stems and leaves, and set up clear water treatment as a blank control. Continue to cultivate and observe, and investigate the fresh weight of the aboveground parts of each treatment after 21 days. Except for 1~2 days before and after spraying, water should be watered regularly to maintain soil moisture.
[0105] The fresh weight rate of weeds was calculated according to the following formula.
[0106] Data statistical analysis methods: The herbicidal activity of the mixture was tested by the Colby method, namely, E 0 =ABC / 10000; wherein A is the fresh weight rate of weeds per dose in comparative example 1 (4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester), B is the fresh weight rate of weeds per dose in comparative example 2 (bifenazolidinone), C is the fresh weight rate of weeds per dose in comparative example 3 (fluzosulfuron), E is the fresh weight rate of weeds per dose in comparative example 2 (fluzosulfuron), 0is the theoretical fresh weight rate of weeds when mixed with herbicides, and E is the measured fresh weight rate of weeds when mixed with herbicides. According to the Colby method, when E 0 -E>10%, indicating that the mixed herbicide produces a synergistic effect; when E 0 When -E<-10%, it indicates that the mixed herbicide produces antagonism; when E 0 When the -E value is between ±10%, it indicates that the mixed herbicides have an additive effect.
[0107] The combined effect of the combination of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam and fluazifop-methyl on grass and broadleaf weeds was tested, and the proportions and results are shown in Table 1.
[0108] Table 1 Results of indoor combined action test of herbicide combinations on grass and broadleaf weeds The results in Table 1 show that the combination of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam and fluazifop-methyl, the dosage of which was used, showed a significant synergistic effect on the grass weeds wild oats and the broad-leaved weeds Artemisia denudata. Moreover, when the weight ratio of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam and fluazifop-methyl was 1-5:2-8:20-30, the synergistic effect was significant.
[0109] Test Example 2 This test example further verifies the efficacy of the herbicidal formulations of the embodiments and comparative examples against weeds.
[0110] The test was carried out in Zhaoquanying Town, Shunyi District, Beijing, and the field efficacy test on annual weeds in wheat fields was carried out using the embodiments and comparative examples.
[0111] Table 2 Results of the field efficacy of herbicide formulations on annual weeds in wheat fields 30 days after application and wheat yield at harvest From the results in Table 2, it can be seen that the herbicide preparations of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid methyl ester, florasulam and fluazifop-methyl all showed excellent control effects on brome grass and broad-leaved weeds such as Artemisia argyi and Shepherd's purse; they were highly safe for wheat, and the wheat yield was significantly higher than the wheat yield when a single agent was used at the same or even high dosage, and there was no significant difference in yield from manual weeding.
[0112] In summary, the herbicidal composition and herbicidal preparation provided by the present invention are used to control annual weeds in wheat fields, which can not only improve the weed control effect, but also significantly reduce the amount of the agent used and is safe for wheat.
[0113] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. A herbicide composition comprising an effective active ingredient and an adjuvant, characterized in that: The effective active ingredients include florasulam and fluazifop-butyl, and also include 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives.
2. The herbicide composition according to claim 1, characterized in that: Based on 1 part by weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, the amount of florasulam used is 0.1-30 parts by weight, and the amount of fluazifop-butyl used is 0.1-60 parts by weight.
3. The herbicide composition according to claim 2, characterized in that: Based on 1 part by weight of 4-amino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylic acid or its agricultural salts, esters and amide derivatives, the amount of florasulam is 0.2-10 parts by weight, and the amount of fluazifop-butyl is 0.5-40 parts by weight.
4. The herbicide composition according to any one of claims 1 to 3, characterized in that: The mass percentage content of the active ingredient in the herbicide composition is 1-99%, preferably 5-80%, more preferably 5-60%.
5. The herbicide composition according to any one of claims 1 to 4, characterized in that: The auxiliary materials include surfactants, carriers and safeners that are acceptable in pesticides.
6. The herbicide composition according to any one of claims 1 to 5, characterized in that: The dosage form is emulsifiable concentrate, water emulsion, water suspension, oil suspension, suspoemulsion, dispersible oil suspension, microcapsule suspension, wettable powder, soluble powder, water dispersible granules or soluble granules.
7. Use of the herbicide composition according to any one of claims 1 to 6 for controlling annual grass and / or broadleaf weeds.
8. The use according to claim 7, characterized in that: The herbicide composition is used for preventing and controlling annual grass and / or broadleaf weeds in wheat fields.
9. The use according to claim 7 or 8, characterized in that: The weeds are one or more of wild oats, brome, barnyard grass, aesculus tauschii, hard grass, foxtail millet, sowthistle, shepherd's purse, cleaver, magnolia officinalis, sedge, lacryma-volucrata, chickweed and veronica.
10. The use according to claim 9, characterized in that: The weeds are shepherd's purse, sophora japonica, wild oats and brome.