WO2024008051A1 - 一种除草组合物及其应用 - Google Patents
一种除草组合物及其应用 Download PDFInfo
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- WO2024008051A1 WO2024008051A1 PCT/CN2023/105587 CN2023105587W WO2024008051A1 WO 2024008051 A1 WO2024008051 A1 WO 2024008051A1 CN 2023105587 W CN2023105587 W CN 2023105587W WO 2024008051 A1 WO2024008051 A1 WO 2024008051A1
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- Prior art keywords
- alkyl
- compound
- composition
- alkoxy
- glufosinate
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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
- 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
- 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
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P13/00—Herbicides; Algicides
Definitions
- the present invention relates to the technical field of pesticides, and in particular to herbicidal compositions and their applications.
- Glufosinate is an organophosphorus non-conductive herbicide and an inhibitor of plant glutamine synthetase. It can cause nitrogen metabolism disorders in plants, excessive accumulation of ammonium, and disintegration of chloroplasts, thereby inhibiting photosynthesis and eventually Causes plant death.
- Glufosinate has the characteristics of low toxicity, high herbicidal activity, broad herbicidal spectrum, and resistance to drift. It exerts its active effect slower than paraquat but faster than glyphosate.
- Glufosinate is a mixture of racemates with one chiral carbon atom, and its configuration is divided into "L-type" and "D-type".
- the one with real herbicidal activity is "L-type glufosinate-ammonium", while “D-type-glufosinate-ammonium” has no biological activity and its structure is relatively stable.
- Precise glufosinate-ammonium is the purification of "L-type glufosinate-ammonium”. Its herbicidal activity is twice that of ordinary glufosinate-ammonium. The application amount per mu is only 50% of that of glufosinate-ammonium. The application cost of the two is basically the same.
- Glyphosate, glufosinate-ammonium, diquat and paraquat are also known as the "Four King Kong” among biocidal herbicides. They are widely used in weeding in non-cultivated land, no-till land, crop fields, etc., and have great control over weeds. important role. In recent years, due to the long-term and large-scale use of a single dose of the above-mentioned herbicide, weed resistance has become increasingly serious, and the dosage has increased, resulting in serious environmental pollution. The rational combination of herbicides has the advantages of increasing weed control effectiveness, reducing dosage, expanding herbicidal spectrum, and delaying weed resistance.
- herbicidal activity means that the herbicide controls harmful plants and achieves the desired herbicidal effect
- safety means that the herbicide is safe or phytotoxic to useful plants, animals, people, ecological environment, etc., and reaches an acceptable range.
- the present invention provides a herbicidal composition, which has the effect of reducing the amount of active ingredients and increasing the effectiveness when applied to harmful plants, and can be used to eliminate crop stubble and provide the next crop. Crops can grow quickly, have an outstanding effect on crops withering, and can also be used to improve crop quality and increase yield.
- a herbicidal composition comprising Compound A and Compound B; wherein,
- the compound A is a compound represented by general formula (I), its stereoisomers, racemates, tautomers, isotope markers, nitrogen oxides, pharmaceutically acceptable salts or esters, and solvates. solvates of compounds or pharmaceutically acceptable salts,
- R 1 , R 2 , R 3 and R 4 are the same or different, and are independently selected from hydrogen, halogen, C 1 -C 6 alkyl or halogenated C 1 -C 6 alkyl;
- R 5 , R 6 , R 7 , and R 8 are the same or different, and are independently selected from hydrogen, halogen, C 1 -C 6 alkyl, halogenated C 1 -C 6 alkyl, and C 1 -C 6 alkoxy. or halogenated C 1 -C 6 alkoxy;
- R 9 and R 10 are the same or different, and are independently selected from hydrogen, cyano, C 1 -C 6 alkyl or halo C 1 -C 6 alkyl;
- R 11 and R 12 are the same or different, and are independently selected from hydrogen, cyano, C 1 -C 6 alkyl, halo C 1 -C 6 alkyl, COOR 13 or CONR 14 R 15 ;
- R 13 is selected from hydrogen, C 1 -C 6 alkyl, halo C 1 -C 6 alkyl, C 1 -C 3 alkoxy C 1 -C 6 alkyl, C 3 -C 6 alkenyl, C 3 -C 6 alkynyl, unsubstituted or C 6 -C 10 aryl C 1 -C 6 alkyl substituted by 1-4 Ra, 5-10 membered heteroaryl C 1 -C 6 alkyl or 3-10 One-membered heterocyclyl C 1 -C 6 alkyl; each Ra is the same or different, independently selected from halogen, cyano, nitro, C 1 -C 6 alkyl, halogenated C 1 -C 6 alkyl, C 1 -C 6 alkoxy or halogenated C 1 -C 6 alkoxy;
- R 14 and R 15 are the same or different, and are independently selected from hydrogen, C 1 -C 6 alkyl or C 1 -C 4 alkoxy C 1 -C 6 alkyl;
- the compound B is: B1) glufosinate-ammonium or its salt, or B2) refined glufosinate-ammonium or its salt.
- the salt includes any salt acceptable in agriculture, forestry or horticulture, specifically: sodium salt, potassium salt, ammonium salt, especially isopropyl ammonium salt, etc.
- Compound A of the present invention is a compound disclosed in patent application CN202011497249.X (publication number CN114644622A), the full text of which is incorporated into the present invention.
- R 1 , R 2 , R 3 and R 4 are the same or different, and are independently selected from hydrogen, halogen, C 1 -C 4 alkyl or halogenated C 1 -C 4 alkyl;
- R 5 , R 6 , R 7 , and R 8 are the same or different, and are independently selected from hydrogen, halogen, C 1 -C 4 alkyl, halogenated C 1 -C 4 alkyl, and C 1 -C 4 alkoxy. or halogenated C 1 -C 4 alkoxy;
- R 9 and R 10 are the same or different, and are independently selected from hydrogen, C 1 -C 4 alkyl or halo C 1 -C 4 alkyl;
- R 11 and R 12 are the same or different, and are independently selected from hydrogen, cyano, C 1 -C 6 alkyl, halo C 1 -C 6 alkyl, COOR 13 or CONR 14 R 15 ;
- R 13 is selected from hydrogen, C 1 -C 6 alkyl, halo C 1 -C 6 alkyl, C 1 -C 3 alkoxy C 1 -C 3 alkyl, C 3 -C 6 alkenyl, C 3 -C 6 alkynyl, not C 6 -C 8 aryl C 1 -C 4 alkyl substituted or substituted by 1 to 4 Ra, 5-8 membered heteroaryl C 1 -C 4 alkyl or 3-6 membered heterocyclyl C 1 - C 4 alkyl; each Ra is the same or different, independently selected from halogen, cyano, nitro, C 1 -C 4 alkyl, halogenated C 1 -C 4 alkyl, C 1 -C 4 alkoxy base or halogenated C 1 -C 4 alkoxy group;
- R 14 and R 15 are the same or different, and are independently selected from hydrogen, C 1 -C 4 alkyl or C 1 -C 4 alkoxy C 1 -C 6 alkyl.
- R 1 , R 2 , R 3 and R 4 are the same or different, and are independently selected from hydrogen, fluorine, chlorine, bromine, methyl, ethyl, tris Fluoromethyl or trifluoroethyl;
- R 5 , R 6 , R 7 , R 8 are the same or different, and are independently selected from hydrogen, fluorine, chlorine, bromine, methyl, ethyl, trifluoromethyl, trifluoroethyl, methoxy, ethoxy base, trifluoromethoxy or trifluoroethoxy;
- R 9 and R 10 are the same or different, and are independently selected from hydrogen, C 1 -C 4 alkyl or halo C 1 -C 4 alkyl;
- R 11 and R 12 are the same or different, and are independently selected from hydrogen, cyano, C 1 -C 4 alkyl, halo C 1 -C 4 alkyl, COOR 13 or CONR 14 R 15 ;
- R 13 is selected from hydrogen, C 1 -C 6 alkyl, halo C 1 -C 6 alkyl, C 1 -C 3 alkoxy C 1 -C 3 alkyl, C 3 -C 6 alkenyl, C 3 -C 6 alkynyl, unsubstituted or benzyl substituted by 1 to 4 Ra, furylmethyl, tetrahydrofurylmethyl or 1,3-dioxolaneethyl; each Ra is the same or different from each other Independently selected from fluorine, chlorine, cyano, nitro, methyl, ethyl, trifluoromethyl, trifluoroethyl, methoxy, ethoxy, trifluoromethoxy or trifluoroethoxy;
- R 14 and R 15 are the same or different, and are independently selected from hydrogen, C 1 -C 4 alkyl or C 1 -C 3 alkoxy C 1 -C 3 alkyl.
- R 1 , R 2 , R 3 and R 4 are the same or different, and are independently selected from hydrogen, fluorine, chlorine, methyl, ethyl, trifluoromethyl base or trifluoroethyl;
- R 5 , R 6 , R 7 , R 8 are the same or different, and are independently selected from hydrogen, fluorine, chlorine, methyl, ethyl, trifluoromethyl, trifluoroethyl, methoxy, ethoxy, Trifluoromethoxy or trifluoroethoxy;
- R 9 and R 10 are the same or different, and are independently selected from hydrogen, methyl, ethyl, propyl, butyl, trifluoromethyl or trifluoroethyl;
- R 11 and R 12 are the same or different, and are independently selected from hydrogen, cyano, C 1 -C 4 alkyl, halo C 1 -C 4 alkyl, COOR 13 or CONR 14 R 15 ;
- R 13 is selected from hydrogen, C 1 -C 6 alkyl, halo C 1 -C 6 alkyl, C 1 -C 3 alkoxy C 1 -C 3 alkyl, allyl, propargyl, unsubstituted Or benzyl, furylmethyl, tetrahydrofurylmethyl or 1,3-dioxolaneethyl substituted by 1-4 Ra; each Ra is the same or different, independently selected from fluorine, chlorine, cyano, nitro, methyl, ethyl, trifluoromethyl, trifluoroethyl, methoxy, ethoxy, trifluoromethoxy or trifluoroethoxy;
- R 14 and R 15 are the same or different, and are independently selected from hydrogen, C 1 -C 4 alkyl or C 1 -C 3 alkoxy C 1 -C 3 alkyl.
- R 1 , R 2 , R 3 and R 4 are the same or different, and are independently selected from hydrogen, fluorine, chlorine, methyl or trifluoromethyl;
- R 5 , R 6 , R 7 , and R 8 are the same or different, and are independently selected from hydrogen, fluorine, chlorine, methyl, trifluoromethyl, methoxy or trifluoromethoxy;
- R 9 and R 10 are the same or different, and are independently selected from hydrogen, methyl, ethyl, propyl or butyl;
- R 11 and R 12 are the same or different, and are independently selected from hydrogen, methyl, ethyl or COOR 13 ;
- R 13 is selected from hydrogen, C 1 -C 4 alkyl, halo C 1 -C 4 alkyl, C 1 -C 3 alkoxy C 1 -C 3 alkyl, allyl, propargyl, benzyl , furylmethyl, tetrahydrofurylmethyl or 1,3-dioxolaneethyl.
- R 1 , R 2 , R 3 and R 4 are the same or different, and are independently selected from hydrogen, fluorine, chlorine or trifluoromethyl;
- R 5 , R 6 , R 7 , R 8 are the same or different, and are independently selected from hydrogen, fluorine, chlorine, methyl or trifluoromethyl;
- R 9 and R 10 are the same or different, and are independently selected from hydrogen or methyl;
- R 11 and R 12 are the same or different, and are independently selected from methyl, ethyl or COOR 13 ;
- R 13 is selected from hydrogen, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, trifluoromethyl, trifluoroethyl, methoxyethyl, ethoxyethyl base, allyl, propargyl, benzyl, furylmethyl, tetrahydrofurylmethyl or 1,3-dioxolaneethyl.
- the compound represented by general formula (I) is a compound represented by the following general formula (IA):
- R 13 is selected from C 1 -C 6 alkyl, halogenated C 1 -C 6 alkyl, C 1 -C 3 alkoxy C 1 -C 6 alkyl, unsubstituted or substituted by 1-4 Ra C 6 -C 10 aryl C 1 -C 6 alkyl, 5-10 membered heteroaryl C 1 -C 6 alkyl or 3-10 membered heterocyclyl C 1 -C 6 alkyl; each Ra is the same or different, independently selected from halogen, cyano, nitro, C 1 -C 6 alkyl, haloC 1 -C 6 alkyl, C 1 -C 6 alkoxy or haloC 1 -C 6 Alkoxy.
- R 13 is selected from methyl, ethyl, benzyl, methoxyethyl or tetrahydrofurylmethyl.
- the specific structure is as follows:
- the weight ratio of Compound A and Compound B is 1: (0.1-200); in this In some embodiments of the invention, the weight ratio of Compound A and Compound B in the composition is 1: (1-150), or 1: (1.4-100), for example: 7:10; 7:20; 7 :30;7:40;7:50;1:2;1:4;1:6;1:8;1:10;1:20;1:30;1:40;1:50;1:60 ;1:80 etc.
- the sum of the masses of Compound A and Compound B accounts for 1-90% of the total mass; preferably, in the composition, the mass of Compound A and Compound B The sum of the masses accounts for 5-90% of the total, such as 1%, 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80% or 90%.
- compound A and compound B exist independently.
- compound A and compound B are mixed, for example, tank-mixed.
- Compound A and Compound B are first made into solutions respectively, and then the Compound A solution and Compound B solution are poured into a bucket and mixed.
- the composition is in the form of a formulation.
- the preparation is a liquid preparation or a solid preparation.
- the preparation is, for example, an emulsifiable concentrate, a water suspension, an oil suspension, a wettable powder, a granule, a water-dispersible granule or an aqueous formulation that is acceptable for pesticides, agriculture, forestry or horticulture.
- the composition further includes pesticides, agricultural, forestry or horticulturally acceptable auxiliaries, such as wetting agents, emulsifiers, dispersants, thickeners, antifreeze agents, etc.
- pesticides such as wetting agents, emulsifiers, dispersants, thickeners, antifreeze agents, etc.
- auxiliaries such as wetting agents, emulsifiers, dispersants, thickeners, antifreeze agents, etc.
- agents, disintegrants, binders, defoaming agents, stabilizers, fillers and carriers include pesticides, agricultural, forestry or horticulturally acceptable auxiliaries, such as wetting agents, emulsifiers, dispersants, thickeners, antifreeze agents, etc.
- agents disintegrants, binders, defoaming agents, stabilizers, fillers and carriers.
- the content of the auxiliary agent in the composition in terms of weight percentage, can be 2-60%, such as 8-50%, exemplarily 2%, 6%, 8% , 10%, 18.7%, 19%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%.
- the wetting agent may be selected from: trisiloxane polyoxyethylene ether, sodium lauroyl glutamate, sodium lauryl sulfate, castor oil polyoxyethylene ether, triphenyl One or more of ethylphenol polyoxyethylene ether, sodium dodecylbenzene sulfonate, sodium alkylnaphthalene sulfonate, sodium isooctyl succinate sulfonate and fatty alcohol polyoxyethylene ether.
- the emulsifier can be selected from: sodium lignosulfonate, agricultural milk, phenylphenol polyoxyethyl ether phosphate, naphthalene sulfonate formaldehyde condensate, benzyl dimethylphenol polyoxyethyl ether, dehydration Sorbitol fatty acid ester polyoxyethylene ether, fatty alcohol polyoxyethylene ether, sorbitan oleate (Span 80), fatty alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, nonylphenol polyoxyethylene One or more of ether phosphate and castor oil polyoxyethylene ether phosphate.
- the dispersant can be selected from: sodium lignin sulfonate, fatty alcohol polyoxyethylene ether sulfate, naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate formaldehyde condensate sodium salt, phosphate ester, polyoxyethylene sorbitan fat acid ester, polyvinyl alcohol, ammonium sulfate, sodium methylene bisnaphthalene sulfonate, sodium methylnaphthalene sulfonate formaldehyde condensate, calcium dodecylbenzene sulfonate, naphthalene sulfonic acid condensate sodium salt, alkylphenol poly One or more of oxyethylene ether and phenethylphenol polyoxyethylene ether.
- the thickener may be selected from one or more of magnesium aluminum silicate, polyvinyl acetate, xanthan gum, gelatin, arabic gum, polyvinyl alcohol, etc.
- the antifreeze may be selected from one or more of propylene glycol, ethylene glycol, glycerin, and the like.
- the disintegrant may be selected from one or more of sodium bicarbonate, ammonium sulfate, sodium sulfate, calcium sulfate and magnesium chloride.
- the binder can be selected from: xanthan gum, starch, urea-formaldehyde resin, gelatin, gum arabic, carboxymethyl cellulose and carboxyethyl One or more of cellulose, etc.
- the defoaming agent may be selected from one or more of silicone oil, n-octanol, silicone, butyl phosphate, isobutyl phosphate, etc.
- the stabilizer may be selected from one or more of triethanolamine, epichlorohydrin, butyl glycidyl ether, triphenyl phosphite, and the like.
- the filler includes solid filler or liquid filler, wherein the solid filler can be selected from one or more of kaolin, attapulgite, diatomite, white carbon black, bentonite, montmorillonite, talc, calcium carbonate, etc. kind; the liquid filler can be selected from one or more of water, soybean oil, castor oil and mineral oil.
- the solvents that can be used in the composition are toluene, xylene, trimethylbenzene, dimethyl sulfoxide, N,N-dimethylformamide, butanone, cyclohexanone, methanol, isopropyl
- the present invention also provides the application of the composition, which is used to control harmful plants, improve the quality and yield of crops, or destroy crops or eliminate stubble.
- the harmful plants are, for example, grass weeds, broadleaf weeds, sedge weeds or other unwanted crop plants.
- the present invention also provides a method for controlling harmful plants, especially a method for controlling harmful plants in crops, which method is to apply the composition to the harmful plants and/or the places where the harmful plants grow.
- the application rate is a herbicidal active amount.
- the present invention also provides a method for improving the quality and yield of crops, which method is to apply the composition to crops, crop seeds or tubers or other propagable parts, and crop growing ground.
- the present invention also provides a method for destroying crops or eliminating stubble, which method is to apply the composition to crops, seeds or tubers of crops or other reproductive parts, and crop growing ground.
- the composition is directionally applied on non-cultivated land, to promote withering or stubble elimination after crop harvest, before crop sowing, after crop sowing and before emergence, before crop transplantation, and between crop rows.
- the composition can be used for stem and leaf spraying: including: non-arable land weeding; farmland crop inter-row directional spray weeding, fruit tree inter-row directional spray weeding, seedling inter-row directional spray weeding; crop (such as cotton, rice, rapeseed, sugar beet, potatoes, peanuts, etc.) after harvest withering or stubble elimination.
- the composition can be used for soil spraying: before sowing farmland crops, before emergence after sowing farmland crops, before transplanting fruit trees, before transplanting seedlings, before sowing lawns, before sowing flowers, etc. .
- the composition has a soil sealing effect.
- the composition When used for soil spraying and stem and leaf spraying, it also has a certain soil sealing effect on pre-emergent weeds (inhibiting the growth of weeds). emergence).
- the non-cultivated land includes but is not limited to forest trees (fields), roads, forest fire roads, railways, etc.; the farmland crops include but is not limited to corn, sorghum, wheat, barley, and rye.
- triticale and durum wheat rice, sugar cane, soybeans, legumes (such as peas, beans and lentils), peanuts, sunflowers, sugar beets, potatoes, cotton, brassicas (such as broccoli, cabbage, Cabbage, etc.);
- the fruit trees include but are not limited to apples, pears, peaches, apricots, walnuts, pecans, olives, cherries, plums, citrus, coffee trees, etc.;
- the seedlings include but are not limited to pine, fir, oak, maple, willow Trees, hawthorns, crabapples, etc.;
- the lawns include but are not limited to bermudagrass, multiflora ryegrass, tall fescue, etc.;
- the flowers include but are not limited to roses, petunias, marigolds, snapdragons, etc.
- the herbicidal composition of the present invention is a compound herbicidal composition containing the above-mentioned compound A, glufosinate-ammonium or refined glufosinate-ammonium; under the action of the compound herbicidal composition, the harmful plants will show symptoms faster Faster, and under the interaction of the two active ingredients, the control effect of the herbicide is improved, the weeds are killed more thoroughly, and the time for weeds to turn green is extended.
- the herbicidal composition of the present invention has a synergistic effect compared with a single agent, with lower dosage and better effect.
- the herbicidal composition of the present invention has a wide range of applications, and the applicable directions include: non-arable land, stubble control after crop harvest, before crop sowing, after crop sowing and before emergence, and directional application between crop rows; the herbicidal composition It has a fast passivation speed with the soil and can be quickly decomposed by soil microorganisms after entering the soil. It is safe for crops planted 1-4 days after application and has no hidden damage to crops.
- the herbicidal composition of the present invention has a broad herbicidal spectrum and can control gramineous, broad-leaf and sedge weeds; it is especially targeted at current malignant weeds, such as Canadian silvergrass, small flying canopy, and hollow lotus seeds. Excellent control effect on grass, nightshade, field bindweed and other weeds.
- the two active ingredients Compound A and Compound B in the herbicidal composition of the present invention have different mechanisms of action. Compounds with different mechanisms of action interact with each other to prolong the resistance of weeds while reducing the dosage of pesticides.
- the herbicidal composition of the present invention can also improve crop quality and increase yield.
- Compound A used in the examples has the following structure:
- Test materials Commelina bengalensis Linn. (a spontaneous weed in wasteland, transplanted indoors); Cyperus rotundus L. (a spontaneous weed in wasteland, transplanted indoors).
- test materials Indoor potting method, select rice bag grass and cyperus rotundus plants of uniform size in the 3-leaf stage that grow spontaneously in the wasteland, transplant them with soil into a seedling pot with a diameter of 9cm, and fill the pot with soil in a ratio of 1:1
- the mixed soil of substrate and sandy loam is watered by absorbing water from the bottom of the pot, and placed in a plant culture room for cultivation.
- E - The actual control effect after compound A and compound B are mixed in the above proportion.
- EE 0 >10% is synergistic effect;
- EE 0 ⁇ -10% is antagonism;
- EE 0 value between ⁇ 10% is additive effect.
- compound IA-17%, glufosinate-ammonium 30%, alkylphenol polyoxyethylene ether 4%, phenethylphenol polyoxyethylene ether 15% and the remaining three Toluene is supplemented to 100%, and an emulsifiable concentrate with a mass percentage of 37% is prepared according to conventional preparation methods.
- compound IA-17%, glufosinate-ammonium 40%, NNO (sodium methylene bisnaphthalene sulfonate) 9%, sodium lignosulfonate 7%, white carbon black 9% and the remaining amount of kaolin are supplemented to 100%, and a wettable powder with a mass percentage of 47% is prepared according to conventional preparation methods.
- compound IA-15% Based on the weight percentage of each component in the composition, compound IA-15%, glufosinate ammonium 30%, sodium menaphthalene sulfonate formaldehyde condensate 6%, fatty alcohol polyoxyethylene ether 3%, magnesium aluminum silicate 0.5%, ethylene glycol 7%, tributyl phosphate 2%, silicone oil 0.2% and the remaining water to make up to 100%, and prepare a suspension with a mass percentage of 35% according to the conventional preparation method.
- compound IA-27%, glufosinate-ammonium 30%, alkylphenol polyoxyethylene ether 4%, phenethylphenol polyoxyethylene ether 15% and the balance triphosphate Toluene is supplemented to 100%, and an emulsifiable concentrate with a mass percentage of 37% is prepared according to conventional preparation methods.
- compound IA-27%, glufosinate-ammonium 40%, NNO (sodium methylene bisnaphthalene sulfonate) 9%, sodium lignosulfonate 7%, white carbon black 9% and the remaining amount of kaolin are supplemented to 100%, and a wettable powder with a mass percentage of 47% is prepared according to conventional preparation methods.
- compound IA-25% Based on the weight percentage of each component in the composition, compound IA-25%, glufosinate ammonium 30%, sodium menaphthalene sulfonate formaldehyde condensate 6%, fatty alcohol polyoxyethylene ether 3%, magnesium aluminum silicate 0.5%, ethylene glycol 7%, tributyl phosphate 2%, silicone oil 0.2% and the remaining water to make up to 100%, and prepare a suspension with a mass percentage of 35% according to the conventional preparation method.
- compound IA-37%, glufosinate-ammonium 30%, alkylphenol polyoxyethylene ether 4%, phenethylphenol polyoxyethylene ether 15% and the balance triphosphate Toluene is supplemented to 100%, and an emulsifiable concentrate with a mass percentage of 37% is prepared according to conventional preparation methods.
- compound IA-37%, glufosinate-ammonium 40%, NNO (sodium methylene bisnaphthalene sulfonate) 9%, sodium lignosulfonate 7%, white carbon black 9% and the remaining amount of kaolin are supplemented to 100%, and a wettable powder with a mass percentage of 47% is prepared according to conventional preparation methods.
- compound IA-35% Based on the weight percentage of each component in the composition, compound IA-35%, glufosinate ammonium 30%, sodium menaphthalene sulfonate formaldehyde condensate 6%, fatty alcohol polyoxyethylene ether 3%, magnesium aluminum silicate 0.5%, ethylene glycol 7%, tributyl phosphate 2%, silicone oil 0.2% and the remaining water to make up to 100%, and prepare a suspension with a mass percentage of 35% according to the conventional preparation method.
- compound IA-47% Based on the weight percentage of each component in the composition, compound IA-47%, glufosinate-ammonium 30%, alkylphenol polyoxyethylene ether 4%, phenethylphenol polyoxyethylene ether 15% and the balance triphosphate Toluene is supplemented to 100%, and an emulsifiable concentrate with a mass percentage of 37% is prepared according to conventional preparation methods.
- compound IA-47%, glufosinate-ammonium 40%, NNO (sodium methylene bisnaphthalene sulfonate) 9%, sodium lignosulfonate 7%, white carbon black 9% and the remaining amount of kaolin are supplemented to 100%, and a wettable powder with a mass percentage of 47% is prepared according to conventional preparation methods.
- compound IA-45% Based on the weight percentage of each component in the composition, compound IA-45%, glufosinate ammonium 30%, sodium menaphthalene sulfonate formaldehyde condensate 6%, fatty alcohol polyoxyethylene ether 3%, magnesium aluminum silicate 0.5%, ethylene glycol 7%, tributyl phosphate 2%, silicone oil 0.2% and the balance make up the water to 100%, and prepare a suspension with a mass percentage of 35% according to conventional preparation methods.
- Target weeds barnyard grass, amaranth, Introducetta, nightshade, and field bindweed;
- test agents and dosages are shown in Table 5; control agents: 18% glufosinate-ammonium SL (commercially available), 10% refined glufosinate-ammonium SL (commercially available).
- Tank mix 10% IA-1EC + 18% glufosinate SL (that is, 10% IA-1 emulsifiable concentrate and 18% glufosinate ammonium soluble agent are tank mixed), 10% IA-2EC + 18% glufosinate ammonium SL, 10% IA-3EC+18% glufosinate-ammonium SL, 10% IA-4EC+18% glufosinate-ammonium SL (Note: EC appearing in the text is the abbreviation of the dosage form "emulsifiable concentrate"; SL appearing in the text is the dosage form "soluble agent” abbreviation).
- Determination method Indoor potting method, sow a certain amount of nightshade seeds in seedling pots with a diameter of 9cm, and sow an appropriate amount in each pot; transplant large-leaf barnyard grass, amaranth, small flying canopy, and field bindweed outdoors to a diameter of In a 9cm seedling pot, cultivate it in the plant culture room.
- the nightshade is at the four-leaf stage
- the barnyard grass is at the 6-leaf stage
- the small flying canopy is at the 6-leaf stage
- the field bindweed is at the 6-leaf stage
- the amaranth is at the flowering stage
- the target weeds are placed in the plant culture room for cultivation.
- the control effect of each treatment on weeds is regularly observed.
- the fresh weight of the above-ground parts or the fresh weight of the plant is measured.
- the control effect of the pesticide on the target weeds is evaluated by the fresh weight control effect (%). Toxicity effects (see Table 5).
- Example 18 Field efficacy test of the herbicidal composition of the present invention on wasteland weeds
- Target weeds Graminous weeds (barnyard grass, crabgrass, wheatgrass) and broadleaf weeds (quinoa, milkweed, Canada goldenrod).
- test chemicals and doses are shown in Table 6 to Table 8; test method: accurately weigh various chemicals according to the area of the test plot, dilute them with water, and use a backpack sprayer to spray evenly.
- the nozzle is specially designed for herbicides. fan-shaped nozzle. When spraying, pay attention to spraying the liquid medicine evenly into the test plot to ensure that there is no leakage or over-spraying.
- weed death was observed 3 days, 7 days, and 30 days after treatment.
- Weed control effects were visually inspected 3 days and 7 days after treatment.
- Weed control effects were measured 30 days after treatment and the weed control effects were compared.
- Herbicidal activity (the dosage is the dosage of active ingredients per acre of land).
- the herbicidal composition of the present invention causes symptoms of harmful plants quickly, and has significant control effect on both gramineous weeds and broadleaf weeds, with significant synergy and long lasting effect. .
- Example 19 Indoor soil sealing test of compound A and glufosinate-ammonium composition
- Compound A + glufosinate has a good soil sealing effect on barnyardgrass, with plant control effect values above 80%.
- the compound A+glufosinate-ammonium has certain soil sealing activity on multiflora ryegrass. The results are shown in Table 9-Table 12.
- Target crops Xianyu 335 corn; target weeds: barnyard grass (3.5 leaves), cowgrass (3.5 leaves).
- the herbicidal composition of the present invention shows symptoms quickly on the tested weeds, has excellent control effect and has a long lasting effect. 0 days after the treatment, the treated weed leaves showed symptoms of dehydration, wilting and dryness. ; 3 days after treatment, all treated weeds were completely dead; 30 days after treatment, the weed control effect still reached more than 80%.
- the herbicidal composition of the present invention is safe for the test crops.
- the interval between treatments is short.
- the seeds were sown 0 days after the treatment.
- a small number of dead spots appeared on the young leaves of the corn, but then the The corn grows and the symptoms can gradually recover; 3 days and 3 days after taking the medicine Seven days after sowing, there were no obvious symptoms of phytotoxicity on the corn leaves of all treatments.
- Example 21 Directional spray test of the herbicidal composition of the present invention in corn fields
- Test method The test location is Gengzhuang Village, Sangzidian Town, Tianqiao District, Jinan City, Shandong province, and the target crop is corn (Zhengdan 958).
- the previous crop was wheat, and the wheat stubble was not treated.
- volunteer wheat had grown, and the corn field was directional sprayed using a tank mix method.
- the dosage of the compound A + glufosinate ammonium composition was 3.5 + 20 g a.i./mu. At this time, The weather was clear and windless.
- the grass phases are: crabgrass, tigertail grass, teff, green amaranth, amaranth, amaranth, sage, spiny amaranth, wild watermelon seedlings, reeds, amaranth, gray-green
- pigweeds and vetches most of the weeds at this time have 2-5 leaves, so directional spraying should be carried out across the field.
- Example 22 The herbicidal composition of the present invention is used as a cotton defoliant
- Test method The test location is Gengzhuang Village, Sangzidian Town, Tianqiao District, Jinan City, Shandong province, and the target crop is cotton.
- the application method of compound A + glufosinate ammonium composition is whole-field stem and leaf spraying, and the dose is 1.5+20g a.i./mu.
- the effect of the agent in promoting cotton boll flocculation is finally investigated, and the absolute value survey method is used to investigate the cotton defoliation rate.
- the test reference is NY/ T1464.26-2007 Pesticide Field Efficacy Test Guidelines Part 26: Cotton Withering Agent Test.
Abstract
提供了一种除草组合物及其应用，所述除草组合物包括化合物A和化合物B；所述化合物A具有式(I)所示的结构，所述化合物B为：B1)草铵膦或其盐、或者B2)精草铵膦或其盐。该组合物不仅可以优势互补，扩大杀草谱，降低了返青率，而且取得了明显的协同增效作用，极大的延长了返青时间，提高了杀草效果。
Description
本申请要求2022年7月4日向中国国家知识产权局提交的专利申请号为202210788277X，发明名称为“一种除草组合物及其应用”的在先申请的优先权。该在先申请的全文通过引用的方式结合于本申请中。
本发明涉及农药技术领域，具体涉及除草组合物及其应用。
草铵膦属于有机磷类非传导性灭生除草剂，是植物谷氨酰胺合成酶抑制剂，可致植物体内的氮代谢紊乱，铵的积累过量，叶绿体解体，从而使光合作用受到抑制，最终导致植物死亡。草铵膦具有毒性低、除草活性高、杀草谱广、不易漂移等特点，发挥活性作用的速度比百草枯慢，但快于草甘膦。草铵膦是外消旋体的混合物，有一个手性碳原子，构型分为“L型”和“D型”。真正具有除草活性的是“L型-草铵膦”，而“D型-草铵膦”没有生物活性，结构相对稳定。精草铵膦就是“L型-草铵膦”的提纯，其除草活性为普通草铵膦的两倍，亩施用量仅为草铵膦的50％，施用成本二者基本相当。
草甘膦、草铵膦、敌草快和百草枯又被称为灭生性除草剂中的“四大金刚”，广泛应用于非耕地、免耕地、农作物田等除草，对杂草的防除具有重要作用。近年来，由于长期大量的使用上述一种除草剂单剂，导致杂草抗性日趋严重，且剂量升高，导致对环境污染严重。除草剂之间的合理复配具有增加杂草防效，减少用药量，扩大杀草谱的优点，且可以延缓杂草的抗药性。
对除草剂的评价，理论上主要有两条标准，一是除草活性，二是安全性。除草活性指除草剂防除有害植物达到所希望的除草效果；安全性指施用除草剂对有用植物、动物、人、生态环境等安全或植物毒性达到所接受的范围。
然而在实践中，可以满足上述标准的单一活性物质的除草剂越来越少，单一活性成分药剂不能应用或只能以极低的剂量使用，从而不能保证达到所希望的除草效果。因此，需要在不影响除草活性的前提下，减少施用量来满足上述的标准。
发明内容
为了克服现有技术中的问题，本发明提供了一种除草组合物，所述除草组合物在应用于有害植物时具有活性成分减量增效的作用，且可应用于作物灭茬，为下茬作物快速腾茬，对作物有突出的催枯作用，还可以应用于作物提质增产。
本发明的技术方案包括：
一种除草组合物，包括化合物A和化合物B；其中，
所述化合物A为通式(I)所示的化合物、其立体异构体、消旋体、互变异构体、同位素标记物、氮氧化物、药学上可接受的盐或酯、溶剂合物或者药学上可接受的盐的溶剂合物，
其中，R1、R2、R3、R4相同或不同，彼此独立地选自氢、卤素、C1-C6烷基或卤代C1-C6烷基；
R5、R6、R7、R8相同或不同，彼此独立地选自氢、卤素、C1-C6烷基、卤代C1-C6烷基、C1-C6烷氧基或卤代C1-C6烷氧基；
R9、R10相同或不同，彼此独立地选自氢、氰基、C1-C6烷基或卤代C1-C6烷基；
R11、R12相同或不同，彼此独立地选自氢、氰基、C1-C6烷基、卤代C1-C6烷基、COOR13或CONR14R15；
R13选自氢、C1-C6烷基、卤代C1-C6烷基、C1-C3烷氧基C1-C6烷基、C3-C6烯基、C3-C6炔基、未取代或被1-4个Ra取代的C6-C10芳基C1-C6烷基、5-10元杂芳基C1-C6烷基或3-10元杂环基C1-C6烷基；每个Ra相同或不同，彼此独立地选自卤素、氰基、硝基、C1-C6烷基、卤代C1-C6烷基、C1-C6烷氧基或卤代C1-C6烷氧基；
R14、R15相同或不同，彼此独立地选自氢、C1-C6烷基或C1-C4烷氧基C1-C6烷基；
所述化合物B为：B1)草铵膦或其盐、或者B2)精草铵膦或其盐。
本发明中，所述盐包括其农业、林业或园艺学上可接受的任意盐，具体可以为：钠盐、钾盐、铵盐、特别是异丙铵盐等。
本发明所述化合物A为专利申请CN202011497249.X(公开号CN114644622A)中所公开的化合物，该申请全文引入到本发明中。
在本发明一些实施方式中，通式(I)中，R1、R2、R3、R4相同或不同，彼此独立地选自氢、卤素、C1-C4烷基或卤代C1-C4烷基；
R5、R6、R7、R8相同或不同，彼此独立地选自氢、卤素、C1-C4烷基、卤代C1-C4烷基、C1-C4烷氧基或卤代C1-C4烷氧基；
R9、R10相同或不同，彼此独立地选自氢、C1-C4烷基或卤代C1-C4烷基；
R11、R12相同或不同，彼此独立地选自氢、氰基、C1-C6烷基、卤代C1-C6烷基、COOR13或CONR14R15；
R13选自氢、C1-C6烷基、卤代C1-C6烷基、C1-C3烷氧基C1-C3烷基、C3-C6烯基、C3-C6炔基、未
取代或被1-4个Ra取代的C6-C8芳基C1-C4烷基、5-8元杂芳基C1-C4烷基或3-6元杂环基C1-C4烷基；每个Ra相同或不同，彼此独立地选自卤素、氰基、硝基、C1-C4烷基、卤代C1-C4烷基、C1-C4烷氧基或卤代C1-C4烷氧基；
R14、R15相同或不同，彼此独立地选自氢、C1-C4烷基或C1-C4烷氧基C1-C6烷基。
在本发明一些实施方式中，通式(I)中，R1、R2、R3、R4相同或不同，彼此独立地选自氢、氟、氯、溴、甲基、乙基、三氟甲基或三氟乙基；
R5、R6、R7、R8相同或不同，彼此独立地选自氢、氟、氯、溴、甲基、乙基、三氟甲基、三氟乙基、甲氧基、乙氧基、三氟甲氧基或三氟乙氧基；
R9、R10相同或不同，彼此独立地选自氢、C1-C4烷基或卤代C1-C4烷基；
R11、R12相同或不同，彼此独立地选自氢、氰基、C1-C4烷基、卤代C1-C4烷基、COOR13或CONR14R15；
R13选自氢、C1-C6烷基、卤代C1-C6烷基、C1-C3烷氧基C1-C3烷基、C3-C6烯基、C3-C6炔基、未取代或被1-4个Ra取代的苄基、呋喃基甲基、四氢呋喃基甲基或1,3-二氧环戊烷乙基；每个Ra相同或不同，彼此独立地选自氟、氯、氰基、硝基、甲基、乙基、三氟甲基、三氟乙基、甲氧基、乙氧基、三氟甲氧基或三氟乙氧基；
R14、R15相同或不同，彼此独立地选自氢、C1-C4烷基或C1-C3烷氧基C1-C3烷基。
在本发明一些实施方式中，通式(I)中，R1、R2、R3、R4相同或不同，彼此独立地选自氢、氟、氯、甲基、乙基、三氟甲基或三氟乙基；
R5、R6、R7、R8相同或不同，彼此独立地选自氢、氟、氯、甲基、乙基、三氟甲基、三氟乙基、甲氧基、乙氧基、三氟甲氧基或三氟乙氧基；
R9、R10相同或不同，彼此独立地选自氢、甲基、乙基、丙基、丁基、三氟甲基或三氟乙基；
R11、R12相同或不同，彼此独立地选自氢、氰基、C1-C4烷基、卤代C1-C4烷基、COOR13或CONR14R15；
R13选自氢、C1-C6烷基、卤代C1-C6烷基、C1-C3烷氧基C1-C3烷基、烯丙基、炔丙基、未取代或被1-4个Ra取代的苄基、呋喃基甲基、四氢呋喃基甲基或1,3-二氧环戊烷乙基；每个Ra相同或不同，彼此独立地选自氟、氯、氰基、硝基、甲基、乙基、三氟甲基、三氟乙基、甲氧基、乙氧基、三氟甲氧基或三氟乙氧基；
R14、R15相同或不同，彼此独立地选自氢、C1-C4烷基或C1-C3烷氧基C1-C3烷基。
在本发明一些实施方式中，通式(I)中，R1、R2、R3、R4相同或不同，彼此独立地选自氢、氟、氯、甲基或三氟甲基；
R5、R6、R7、R8相同或不同，彼此独立地选自氢、氟、氯、甲基、三氟甲基、甲氧基或三氟甲氧基；
R9、R10相同或不同，彼此独立地选自氢、甲基、乙基、丙基或丁基；
R11、R12相同或不同，彼此独立地选自氢、甲基、乙基或COOR13；
R13选自氢、C1-C4烷基、卤代C1-C4烷基、C1-C3烷氧基C1-C3烷基、烯丙基、炔丙基、苄基、呋喃基甲基、四氢呋喃基甲基或1,3-二氧环戊烷乙基。
在本发明一些实施方式中，通式(I)中，R1、R2、R3、R4相同或不同，彼此独立地选自氢、氟、氯或三氟甲基；
R5、R6、R7、R8相同或不同，彼此独立地选自氢、氟、氯、甲基或三氟甲基；
R9、R10相同或不同，彼此独立地选自氢或甲基；
R11、R12相同或不同，彼此独立地选自甲基、乙基或COOR13；
R13选自氢、甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、三氟甲基、三氟乙基、甲氧基乙基、乙氧基乙基、烯丙基、炔丙基、苄基、呋喃基甲基、四氢呋喃基甲基或1,3-二氧环戊烷乙基。
在本发明一些实施方式中，通式(I)所示的化合物为如下通式(IA)所示的化合物：
其中，R13选自C1-C6烷基、卤代C1-C6烷基、C1-C3烷氧基C1-C6烷基、未取代或被1-4个Ra取代的C6-C10芳基C1-C6烷基、5-10元杂芳基C1-C6烷基或3-10元杂环基C1-C6烷基；每个Ra相同或不同，彼此独立地选自卤素、氰基、硝基、C1-C6烷基、卤代C1-C6烷基、C1-C6烷氧基或卤代C1-C6烷氧基。
在本发明一些实施方式中，通式(IA)中，R13选自甲基、乙基、苄基、甲氧基乙基或四氢呋喃基甲基。具体结构如下：
根据本发明的实施方案，所述组合物中，化合物A和化合物B的重量比为1：(0.1-200)；在本
发明的一些实施方式中，所述组合物中，化合物A和化合物B的重量比为1：(1-150)，或1：(1.4-100)，例如：7:10；7:20；7:30；7:40；7:50；1:2；1:4；1:6；1:8；1:10；1:20；1:30；1:40；1:50；1:60；1:80等。
根据本发明的实施方案，所述组合物中，化合物A和化合物B的质量之和占总量的百分含量为1-90％；优选的，所述组合物中，化合物A和化合物B的质量之和占总量的百分含量为5-90％，如1％、5％、10％、20％、30％、40％、50％、60％、70％、80％或90％。
在本发明一些实施方式中，所述组合物中，所述化合物A和化合物B是独立存在的。使用时再将化合物A和化合物B进行混配，例如进行桶混。在一个实施方式中，先将化合物A和化合物B分别制成溶液，再将化合物A溶液和化合物B溶液倒入桶中混合。
在本发明一些实施方式中，所述组合物为制剂形式。所述制剂为液体制剂或固体制剂。所述制剂例如为乳油、水悬浮剂、油悬浮剂、可湿性粉剂、颗粒剂、水分散粒剂或水剂等农药、农业、林业或园艺学上可接受的剂型。
在本发明一些实施方式中，所述组合物还包括农药、农业、林业或园艺学上可接受的助剂，所述助剂例如为润湿剂、乳化剂、分散剂、增稠剂、防冻剂、崩解剂、粘结剂、消泡剂、稳定剂、填料和载体中的一种或多种。
根据本发明的实施方式，所述助剂在所述组合物中的含量，以重量百分数计，可以为2-60％，例如为8-50％，示例性为2％、6％、8％、10％、18.7％、19％、20％、25％、30％、35％、40％、45％、50％、55％、60％。
根据本发明的实施方式，所述润湿剂可以选自：三硅氧烷聚氧乙烯醚、N-月桂酰基谷氨酸钠、十二烷基硫酸钠、蓖麻油聚氧乙烯醚、三苯乙基苯酚聚氧乙烯醚、十二烷基苯磺酸钠、烷基萘磺酸钠、异辛醇琥珀酸酯磺酸钠和脂肪醇聚氧乙烯醚等中的一种或多种。
所述乳化剂可以选自：木质素磺酸钠、农乳、苯基酚聚氧乙基醚磷酸酯、萘磺酸盐甲醛缩合物、苄基二甲基酚聚氧乙基醚、失水山梨醇脂肪酸酯聚氧乙烯醚、脂肪醇聚氧乙烯醚、山梨醇酐油酸酯(斯盘80)、脂肪醇聚氧乙烯醚、壬基酚聚氧乙烯醚、壬基酚聚氧乙烯醚磷酸酯和蓖麻油聚氧乙烯醚磷酸酯等中的一种或多种。
所述分散剂可以选自：木质素磺酸钠、脂肪醇聚氧乙烯醚硫酸盐、萘磺酸盐甲醛缩合物、萘磺酸甲醛缩合物钠盐、磷酸酯、聚氧乙烯山梨聚糖脂肪酸酯、聚乙烯醇、硫酸铵、亚甲基双萘磺酸钠、甲基萘磺酸钠甲醛缩合物、十二烷基苯磺酸钙、萘磺酸缩合物钠盐、烷基酚聚氧乙烯醚和苯乙基酚聚氧乙烯醚等中的一种或多种。
所述增稠剂可以选自：硅酸镁铝、聚乙酸乙烯酯、黄原胶、明胶、阿拉伯胶和聚乙烯醇等中的一种或多种。
所述防冻剂可以选自：丙二醇、乙二醇和丙三醇等中的一种或多种。
所述崩解剂可以选自：碳酸氢钠、硫酸铵、硫酸钠、硫酸钙和氯化镁中的一种或多种。
所述粘结剂可以选自：黄原胶、淀粉、脲醛树脂、明胶、阿拉伯胶、羧甲基纤维素和羧乙基
纤维素等中的一种或多种。
所述消泡剂可以选自：硅油、正-辛醇、硅酮、磷酸丁酯、磷酸异丁酯等中的一种或多种。
所述稳定剂可以选自：三乙醇胺、环氧氯丙烷、丁基缩水甘油醚和亚磷酸三苯酯等中的一种或多种。
所述填料包括固体填料或液体填料，其中，固体填料可以选自：高岭土、凹凸棒土、硅藻土、白炭黑、膨润土、蒙脱石、滑石粉和碳酸钙等中的一种或多种；液体填料可以选自水、大豆油、蓖麻油和矿物油等中的一种或多种。
根据本发明的实施方式，所述组合物中可使用的溶剂为甲苯、二甲苯、三甲苯、二甲亚砜、N,N-二甲基甲酰胺、丁酮、环已酮、甲醇、异丙醇、丁醇、乙二醇、四氢呋喃、磷酸三丁酯、机油、植物油、提炼油、硅油、玉米油和水等中的一种或多种。
本发明还提供了所述组合物的应用，其用于防治有害植物、用于作物的提质增产或者用于作物的摧枯或灭茬。
根据本发明的实施方案，所述有害植物例如为禾本科杂草、阔叶类杂草、莎草科杂草或者其他不想要的作物植物。
本发明还提供一种防治有害植物的方法，特别是防治作物中的有害植物的方法，所述方法是将所述组合物施用于有害植物和/或有害植物生长地。优选地，施用量为除草活性量。
本发明还提供一种用于作物的提质增产的方法，所述方法是将所述组合物施用于作物、作物的种子或块茎或其他可繁殖部位、作物生长地上。
本发明还提供一种用于作物的摧枯或灭茬的方法，所述方法是将所述组合物施用于作物、作物的种子或块茎或其他可繁殖部位、作物生长地上。
根据本发明的实施方案，将所述组合物在非耕地、作物收获后的催枯或灭茬、作物播种前、作物播种后出苗前、作物移栽前、作物行间定向施用。
在本发明的一个实施方案中，所述组合物可用于茎叶喷雾：包括：非耕地除草；农田作物行间定向喷雾除草、果树行间定向喷雾除草、苗木行间定向喷雾除草；对作物(如棉花、水稻、油菜、甜菜、薯类、花生等)收获后的催枯或灭茬。
在本发明的一个实施方案中，所述组合物可用于土壤喷雾：包括：农田作物播种前、农田作物播种后出苗前、果树移栽前、苗木移栽前、草坪播种前、花卉播种前等。
根据本发明的实施方案，所述组合物具有土壤封闭的效果，所述组合物对用于土壤喷雾以及茎叶喷雾时，对未出苗的杂草也有一定的土壤封闭的效果(抑制杂草的出苗)。
在本发明的一个实施方案中，所述非耕地包括但不限于林木(场)、公路、森林防火道、铁路等地；所述农田作物包括但不限于玉米、高梁、小麦、大麦、黑麦、黑小麦和硬粒小麦、稻、甘蔗、大豆、豆类蔬菜(如豌豆、菜豆和扁豆)、花生、向日葵、糖用甜菜、土豆、棉花、芸苔属作物(如西蓝花、卷心菜、甘蓝等)；所述果树包括但不限于苹果、梨、桃、杏、胡桃、山核桃、橄榄、樱桃、李子、柑橘、咖啡树等；所述苗木包括但不限于松属、冷杉、橡树、枫树、柳
树、山楂、海棠等；所述草坪包括但不限于狗牙根、多花黑麦草、高羊茅等；所述花卉包括但不限于玫瑰、矮牵牛、万寿菊和金鱼草等。
本发明所述组合物的有益效果是：
(1)本发明所述的除草组合物是包含上述化合物A、草铵膦或精草铵膦的复配除草组合物；有害植物在复配除草组合物的作用下，有害植物的显症速度更快，且在两种有效成分的相互作用下，提高除草剂的防效，死草更彻底，并延长杂草返青时长。
(2)本发明所述的除草组合物与单剂相比具有增效作用，用量更低，效果更好。
(3)本发明所述的除草组合物应用范围广泛，可应用方向包括：非耕地、作物收获后的灭茬、作物播种前、作物播种后出苗前、作物行间定向施用；所述除草组合物与土壤的钝化速度快，进入土壤后可迅速被土壤微生物分解，对施用1-4天后种植的作物安全，且对作物无隐性药害。
(4)本发明所述的除草组合物杀草谱广泛，可防治禾本科、阔叶及莎草科杂草；特别针对于目前的恶性杂草，如：加拿大一枝花、小飞蓬、空心莲子草、龙葵、田旋花等杂草防效优异。
(5)本发明所述的除草组合物中两活性成分化合物A和化合物B的作用机理不同，不同作用机理的化合物相互作用，在减少用药量的同时，延长杂草的抗药性。
(6)本发明所述的除草组合物还可以提升作物的质量和增加产量。
下文将结合具体实施例对本发明的技术方案做更进一步的详细说明。应当理解，下列实施例仅为示例性地说明和解释本发明，而不应被解释为对本发明保护范围的限制。凡基于本发明上述内容所实现的技术均涵盖在本发明旨在保护的范围内。
除非另有说明，以下实施例中使用的原料和试剂均为市售商品，或者可以通过已知方法制备。
实施例中所使用的化合物A具有如下所示结构：
一、化合物A和化合物B单剂和组合物室内除草活性测试。
试验材料：饭包草(Commelina bengalensis Linn.)(荒地自生杂草，室内移栽)；香附子(Cyperus rotundusL.)(荒地自生杂草，室内移栽)。
试验材料准备：室内盆栽法，选取荒地自生的大小均匀的3叶期的饭包草、香附子植株，带土移栽于口径为9cm的育苗盆中，盆内填充土为比例1：1的基质与沙壤土的混合土，采取盆底吸水的方式浇水，放置植物培养室中培养。
试验方法：
待饭包草、香附子分别生长至7叶期、5叶期合适叶龄，在3WP～2000型行走式喷雾塔上进行喷雾处理。分别称取一定质量的纯度均为98.8％的化合物IA-1～IA-4，纯度为95％草铵膦原药，加入丙酮充分溶解后用0.1％的吐温80水溶液稀释，分别配制成单剂母液，根据混配目的设置系列配比(重量比)，各单剂及每组配比混剂设置5个浓度梯度，进行茎叶喷雾处理。处理后的试验材料置于植物培养室培养，定期观察各处理对杂草的防除效果，15天后称地上部分鲜重，以鲜重防效E(％)评价药剂对靶标杂草的毒力作用。
计算方法：
以化合物A和化合物B两药剂混用为例，按上述比例混用后的实际防效(鲜重防效)E按公式(1)计算，理论防效E0(％)按公式(2)计算：
式中：
X一化合物A用量为P时的杂草防效；
Y一化合物B用量为Q时的杂草防效；
E0一化合物A用量为P时的理论防效+化合物B用量为Q时的理论防效；
E一化合物A与化合物B按上述比例混用后的实际防效。E-E0>10％为增效作用；E-E0<-10％为拮抗作用；E-E0值介于±10％之间为加成作用。
测定结果表明(见表1-表4)，化合物IA-1～IA-4与草铵膦在混配比例范围内(化合物IA-1～IA-4：草铵膦＝1：1.43～100)全部具有明显的增效作用。其中，在剂量为20+2.5、20+3.5、25+1.5、25+2.5、25+3.5g a.i/mu(有效成分克/亩)可完全杀死两种供试杂草。
表1化合物IA-1+草铵膦对杂草的联合作用测定试验结果
表2化合物IA-2与草铵膦对杂草的联合作用测定试验结果
表3化合物IA-3与草铵膦对杂草的联合作用测定试验结果
表4化合物IA-4与草铵膦对杂草的联合作用测定试验结果
二、制剂的配制及其药效试验
实施例1
以组合物中各组分的重量百分数计，将化合物IA-17％、草铵膦30％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例2
以组合物中各组分的重量百分数计，将化合物IA-17％、精草铵膦15％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例3
以组合物中各组分的重量百分数计，将化合物IA-17％、草铵膦40％、NNO(亚甲基双萘磺酸钠)9％、木质素磺酸钠7％、白炭黑9％和余量的高岭土补足至100％，按照常规的制剂方法配制成质量百分含量为47％的可湿性粉剂。
实施例4
以组合物中各组分的重量百分数计，将化合物IA-15％、草铵膦30％、甲基萘磺酸钠甲醛缩合物6％、脂肪醇聚氧乙烯醚3％、硅酸镁铝0.5％、乙二醇7％、磷酸三丁酯2％、硅油0.2％和余量的水补足至100％，按照常规的制剂方法配制成质量百分含量为35％的悬浮剂。
实施例5
以组合物中各组分的重量百分数计，将化合物IA-27％、草铵膦30％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例6
以组合物中各组分的重量百分数计，将化合物IA-27％、精草铵膦15％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例7
以组合物中各组分的重量百分数计，将化合物IA-27％、草铵膦40％、NNO(亚甲基双萘磺酸钠)9％、木质素磺酸钠7％、白炭黑9％和余量的高岭土补足至100％，按照常规的制剂方法配制成质量百分含量为47％的可湿性粉剂。
实施例8
以组合物中各组分的重量百分数计，将化合物IA-25％、草铵膦30％、甲基萘磺酸钠甲醛缩合物6％、脂肪醇聚氧乙烯醚3％、硅酸镁铝0.5％、乙二醇7％、磷酸三丁酯2％、硅油0.2％和余量的水补足至100％，按照常规的制剂方法配制成质量百分含量为35％的悬浮剂。
实施例9
以组合物中各组分的重量百分数计，将化合物IA-37％、草铵膦30％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例10
以组合物中各组分的重量百分数计，将化合物IA-37％、精草铵膦15％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例11
以组合物中各组分的重量百分数计，将化合物IA-37％、草铵膦40％、NNO(亚甲基双萘磺酸钠)9％、木质素磺酸钠7％、白炭黑9％和余量的高岭土补足至100％，按照常规的制剂方法配制成质量百分含量为47％的可湿性粉剂。
实施例12
以组合物中各组分的重量百分数计，将化合物IA-35％、草铵膦30％、甲基萘磺酸钠甲醛缩合物6％、脂肪醇聚氧乙烯醚3％、硅酸镁铝0.5％、乙二醇7％、磷酸三丁酯2％、硅油0.2％和余量的水补足至100％，按照常规的制剂方法配制成质量百分含量为35％的悬浮剂。
实施例13
以组合物中各组分的重量百分数计，将化合物IA-47％、草铵膦30％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例14
以组合物中各组分的重量百分数计，将化合物IA-47％、精草铵膦15％、烷基酚聚氧乙烯醚4％、苯乙基酚聚氧乙烯醚15％和余量的三甲苯补足至100％，按照常规的制剂方法配制成质量百分含量为37％的乳油。
实施例15
以组合物中各组分的重量百分数计，将化合物IA-47％、草铵膦40％、NNO(亚甲基双萘磺酸钠)9％、木质素磺酸钠7％、白炭黑9％和余量的高岭土补足至100％，按照常规的制剂方法配制成质量百分含量为47％的可湿性粉剂。
实施例16
以组合物中各组分的重量百分数计，将化合物IA-45％、草铵膦30％、甲基萘磺酸钠甲醛缩合物6％、脂肪醇聚氧乙烯醚3％、硅酸镁铝0.5％、乙二醇7％、磷酸三丁酯2％、硅油0.2％和余量的
水补足至100％，按照常规的制剂方法配制成质量百分含量为35％的悬浮剂。
实施例17本发明除草组合物的制剂药效比对试验
靶标杂草：稗草、铁苋菜、小飞蓬、龙葵、田旋花；
试验药剂及剂量见表5所示；对照药剂：18％草铵膦SL(市售)、10％精草铵膦SL(市售)。桶混：10％IA-1EC+18％草铵膦SL(即将10％IA-1的乳油与18％草铵膦的可溶液剂进行桶混)，10％IA-2EC+18％草铵膦SL，10％IA-3EC+18％草铵膦SL，10％IA-4EC+18％草铵膦SL(注：文中出现EC为剂型“乳油”缩写；文中出现SL为剂型“可溶液剂”缩写)。
测定方法：室内盆栽法，将定量的龙葵种子播种于口径为9cm的育苗盆中，每盆播种适量；于室外移栽大叶龄稗草、铁苋菜、小飞蓬、田旋花到口径为9cm的育苗盆中，在植物培养室中培养，待龙葵四叶期、稗草6叶期、小飞蓬6叶期、田旋花6叶期、铁苋菜开花期时，在3WP～2000型行走式喷雾塔上进行喷雾处理。处理后靶标杂草置于植物培养室培养，定期观察各处理对杂草的防除效果，15天后称地上部分鲜重或株鲜重，以鲜重防效(％)评价药剂对靶标杂草的毒力作用(见表5)。
计算方法：
试验结果：
表5本发明除草组合物的制剂药效比对试验结果(15天后)
药后1天，实施例1-16的经处理的供试杂草叶片均表现出不同程度的脱水、枯斑症状，化合物A与草铵膦或精草胺膦复配与单剂相比可提高杂草的显症速度，由表5结果可知，药后15天，化合物IA-1～IA-4与草铵膦或精草胺膦复配，对稗草、铁苋菜、龙葵完全杀死，明显提高小飞蓬、田旋花的鲜重防效。化合物IA-1～IA-4与草铵膦或精草胺膦复配可提高对杂草的除草活性，且在保证药效情况下，降低药剂的用药量。
实施例18本发明除草组合物的荒地杂草田间药效试验
靶标杂草：禾本科杂草(稗草、马唐、大穗看麦娘)和阔叶杂草(藜、乳苣、加拿大一枝黄花)。
试验药剂及剂量见表6-表8所示；试验方法：按照试验小区的面积，准确称量好各种药剂，并兑水稀释后，利用背负式喷雾器，进行均匀喷雾，喷头选用除草剂专用的扇形喷头。喷雾时，要注意将药液均匀喷施到试验小区中，做到没有漏喷、多喷的现象。
试验后分别在药后3天、7天、30天观察杂草死亡情况，药后3天、7天目测调查杂草防效，药后30天数测调查杂草株防效并比较各种药剂的除草活性(用量均为每亩地有效成分的用量)。
试验结果：
表6施药后3天目测防效结果
表7施药后7天目测防效结果
表8施药后30天株防效结果
由上表6-表8可知，本发明除草组合物对有害植物的显症速度快，并且对禾本科杂草和阔叶杂草都具有显著的防效，增效性显著，持效期长。
实施例19化合物A和草铵膦组合物室内土壤封闭试验
在大田试验过程中，发现化合物A还具有一定的土壤封闭活性，对化合物A和草铵膦组合物进行如下室内试验：
在玻璃温室中，选择稗草、多花黑麦草、马齿苋、苘麻进行化合物A和草铵膦组合物室内除草活性比对试验(土壤喷雾)，采用桶混的方法进行试验，其中，10％化合物AEC的剂量为10g a.i/mu，18％草铵膦SL的剂量为20g a.i/mu，进行土壤喷雾。结果为：化合物A+草铵膦对苘麻、马齿苋土壤封闭效果优异，防治效果值均在95％以上，对稗草具有较好的土壤封闭效果，株防治效果值在80％以上，化合物A+草铵膦对多花黑麦草具有一定的土壤封闭活性，结果详见表9-表12。
表9化合物IA-1和草铵膦组合物室内除草活性(土壤封闭)
表10化合物IA-2和草铵膦组合物室内除草活性(土壤封闭)
表11化合物IA-3和草铵膦组合物室内除草活性(土壤封闭)
表12化合物IA-4和草铵膦组合物室内除草活性(土壤封闭)
实施例20本发明除草组合物的田间安全性及药效试验
靶标作物：先玉335玉米；靶标杂草：稗草(3.5叶)、牛筋草(3.5叶)。
于6月初玉米播种前3天，用实施例4、8、12、16(有效成分含量：23.5g a.i/mu)分别对杂草茎叶喷雾处理。试验药剂处理后，分别于药后0天、3天、5天播种玉米。
试验结果：
表13除草活性田间试验结果
表14后茬玉米安全性田间试验结果
从表13结果可看出，本发明的除草组合物对供试杂草显症速度快、防效优异且持效期长，药后0天，处理杂草叶片即出现脱水、萎蔫、干枯症状；药后3天，所有处理杂草完全死亡；药后30天，对杂草防效仍达到80％以上。
从表14结果可看出，本发明的除草组合物对供试作物安全，药后间隔时间短，药后0天播种，于药后7天调查，玉米幼嫩叶片出现少量枯斑，但随玉米生长，症状可逐渐恢复；药后3天以及药
后7天播种，所有处理玉米叶片无明显药害症状。
实施例21本发明除草组合物在玉米田定向喷雾试验
试验方法：试验地点为山东省济南市天桥区桑梓店镇耿庄村，靶标作物为玉米(郑单958)。前茬作物为小麦，麦茬未处理，此时已有自生小麦长出，采用桶混的方式进行玉米田的定向喷雾处理，化合物A+草铵膦组合物剂量为3.5+20g a.i./mu，此时天气晴朗无风。在玉米7-8叶期时草相为：马唐、虎尾草、画眉草、青葙、繁穗苋、凹头苋、猪毛菜、刺苋、野西瓜苗、芦苇、铁苋菜、灰绿藜、野豌豆，此时杂草叶龄多为2-5叶，进行全田定向喷雾处理。
小麦灭茬处理20天调查结果表明：自生小麦已死亡，玉米生长正常。
化合物A+草铵膦组合物在玉米田间定向喷雾使用后，1、3、7、10、14天调查结果发现：1天后杂草叶片脱水干枯，3天后玉米田中的大部分杂草已干枯死亡，7天后玉米田中的杂草已全部干枯死亡。玉米生长正常。玉米成熟后，经实地测产发现，施用化合物A+草铵膦组合物后，增产率在20％以上，明显增产，结果详见表15-表19。
表15化合物IA-1+草铵膦组合物玉米田间定向喷雾目测防效
表16化合物IA-2+草铵膦组合物玉米田间定向喷雾目测防效
表17化合物IA-3+草铵膦组合物玉米田间定向喷雾目测防效
表18化合物IA-4+草铵膦组合物玉米田间定向喷雾目测防效
表19化合物A+草铵膦组合物玉米田间定向喷雾测产结果
实施例22本发明除草组合物作为棉花落叶剂使用
试验方法：试验地点为山东省济南市天桥区桑梓店镇耿庄村，靶标作物为棉花。化合物A+草铵膦组合物的施用方式为全田茎叶喷雾，剂量为1.5+20g a.i./mu，最终调查药剂促进棉铃吐絮效果，并选用绝对值调查法调查棉花脱叶率，试验参考NY/T1464.26-2007农药田间药效试验准则第26部分：棉花催枯剂试验。
棉田喷施化合物A+草铵膦组合物(剂量为1.5+20g a.i/mu)后，与对照区相比较，叶片提早脱落，药后5天发现，叶片相较于对照处理区有褶皱、脱水、干枯的现象，到15天时，叶片脱落率显著高于对照处理区；药后20天，叶片基本全部脱落，结果详见表20。
棉田喷施化合物A+草铵膦组合物(剂量为1.5+20g a.i/mu)后，对棉铃的吐絮也有一定的效果，药后20天，处理区的霜前花率明显高于对照区，从总体来看处理区的霜前花率明显高于对照区，有利于提高棉花的产量和质量，结果详见表21。
表20化合物A+草铵膦组合物(剂量为1.5+20g a.i/mu)棉花的脱叶率(％)
表21化合物A+草铵膦组合物(剂量为1.5+20g a.i/mu)棉花的霜前花率(％)
以上，对本发明的实施方式进行了说明。但是，本发明不限定于上述实施方式。凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
- 一种除草组合物，包括化合物A和化合物B；其中，所述化合物A为通式(I)所示的化合物、其立体异构体、消旋体、互变异构体、同位素标记物、氮氧化物、药学上可接受的盐或酯、溶剂合物或者药学上可接受的盐的溶剂合物，
其中，R1、R2、R3、R4相同或不同，彼此独立地选自氢、卤素、C1-C6烷基或卤代C1-C6烷基；R5、R6、R7、R8相同或不同，彼此独立地选自氢、卤素、C1-C6烷基、卤代C1-C6烷基、C1-C6烷氧基或卤代C1-C6烷氧基；R9、R10相同或不同，彼此独立地选自氢、氰基、C1-C6烷基或卤代C1-C6烷基；R11、R12相同或不同，彼此独立地选自氢、氰基、C1-C6烷基、卤代C1-C6烷基、COOR13或CONR14R15；R13选自氢、C1-C6烷基、卤代C1-C6烷基、C1-C3烷氧基C1-C6烷基、C3-C6烯基、C3-C6炔基、未取代或被1-4个Ra取代的C6-C10芳基C1-C6烷基、5-10元杂芳基C1-C6烷基或3-10元杂环基C1-C6烷基；每个Ra相同或不同，彼此独立地选自卤素、氰基、硝基、C1-C6烷基、卤代C1-C6烷基、C1-C6烷氧基或卤代C1-C6烷氧基；R14、R15相同或不同，彼此独立地选自氢、C1-C6烷基或C1-C4烷氧基C1-C6烷基；所述化合物B为：B1)草铵膦或其盐、或者B2)精草铵膦或其盐。 - 如权利要求1所述的组合物，其中，通式(I)所示的化合物为如下通式(IA)所示的化合物：
其中，R13选自C1-C6烷基、卤代C1-C6烷基、C1-C3烷氧基C1-C6烷基、未取代或被1-4个Ra取代的C6-C10芳基C1-C6烷基、5-10元杂芳基C1-C6烷基或3-10元杂环基C1-C6烷基；每个Ra相同或不同，彼此独立地选自卤素、氰基、硝基、C1-C6烷基、卤代C1-C6烷基、C1-C6烷氧基或卤代C1-C6烷氧基。 - 如权利要求1所述的组合物，其中，通式(I)化合物为如下化合物：
- 如权利要求1所述的组合物，其中，所述组合物中，化合物A和化合物B的重量比为1：(0.1-200)。
- 如权利要求1所述的组合物，其中，所述组合物中，化合物A和化合物B的质量之和占总量的百分含量为1-90％；优选的，所述组合物中，化合物A和化合物B的质量之和占总量的百分含量为5-90％。
- 如权利要求1所述的组合物，其中，所述组合物中，所述化合物A和化合物B是独立存在的，使用时再将化合物A和化合物B进行混配；优选的，所述组合物为制剂形式；所述制剂为液体制剂或固体制剂；所述制剂例如为乳油、水悬浮剂、油悬浮剂、可湿性粉剂、颗粒剂、水分散粒剂或水剂等农药、农业、林业或园艺学上可接受的剂型；优选的，所述组合物还包括农药、农业、林业或园艺学上可接受的助剂，所述助剂例如为润湿剂、乳化剂、分散剂、增稠剂、防冻剂、崩解剂、粘结剂、消泡剂、稳定剂、填料和载体中的一种或多种。
- 权利要求1-6任一项所述的组合物的应用，其用于防治有害植物、用于作物的提质增产或者用于作物的摧枯或灭茬。
- 一种防治有害植物的方法，所述方法是将权利要求1-6中任一项所述的组合物施用于有害植物和/或有害植物生长地；优选地，所述组合物可用于茎叶喷雾或土壤喷雾。
- 一种用于作物的提质增产的方法，所述方法是将权利要求1-6中任一项所述的组合物施用于作物、作物的种子或块茎或其他可繁殖部位、作物生长地上；优选地，所述组合物可用于茎叶喷雾或土壤喷雾。
- 一种用于作物的摧枯或灭茬的方法，所述方法是将权利要求1-6中任一项所述的组合物施用于作物、作物的种子或块茎或其他可繁殖部位、作物生长地上；优选地，所述组合物可用于茎叶喷雾或土壤喷雾。
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