WO2017206825A1 - Weeding composition having synergistic effects - Google Patents

Weeding composition having synergistic effects Download PDF

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Publication number
WO2017206825A1
WO2017206825A1 PCT/CN2017/086260 CN2017086260W WO2017206825A1 WO 2017206825 A1 WO2017206825 A1 WO 2017206825A1 CN 2017086260 W CN2017086260 W CN 2017086260W WO 2017206825 A1 WO2017206825 A1 WO 2017206825A1
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composition
active ingredient
herbicidal composition
composition according
herbicidal
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PCT/CN2017/086260
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French (fr)
Chinese (zh)
Inventor
吴进龙
仲汉根
季红进
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江苏辉丰农化股份有限公司
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Publication of WO2017206825A1 publication Critical patent/WO2017206825A1/en

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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/541,3-Diazines; Hydrogenated 1,3-diazines

Definitions

  • the invention belongs to the field of agricultural plant protection, and in particular relates to a herbicidal composition with improved properties.
  • the active ingredient diflufenican is a carotenoid biosynthesis inhibitor. Causes chlorophyll destruction and cell rupture, and plant death.
  • Isoflufena is an amide herbicide that can form an anti-leaching medicinal soil layer on the soil surface before and after germination of the weeds to maintain activity throughout the growing period of the crop.
  • the flirazone can inhibit the carotenoid biosynthesis, and the carotenoid content in the weed plants of the absorption agent decreases, causing the chlorophyll to be destroyed and the cell membrane to rupture.
  • Weeds are characterized by decolorization or whitening of the young shoots, and finally the entire plant is wilted and dead.
  • Pyribenzoxim is a broad-spectrum herbicide for rice fields, a novel oxime ester compound, and a broad-spectrum selective post-emergence herbicide.
  • the mechanism of action is similar to sulfonylureas and imidazolium herbicides, all of which are acetolactate synthase (ALS) inhibitors. It has selective super-efficient post-emergence herbicidal activity against rice, common wheat and Zoysiagrass, and has no pre-emergence herbicidal activity. It is used to control various grasses and broadleaf weeds such as valerian, big stalk, maiden and spicy sorghum. The effect of the plan is outstanding, and it is safe for rice and common wheat.
  • ALS acetolactate synthase
  • the herbicide weeding rate is slower and can inhibit weed growth after application, but it must die after 2 weeks.
  • the drug is moderately broad and effective for the 1.5 to 6.5 leaf stage of Valerian. In the 2.5-3.5 leaf stage, 100% control can be achieved at a dose of 10g/h; a dose of 20g/h can be achieved in the 3.5-4.5 leaf stage to achieve 100% control.
  • the purpose of the invention is to screen the herbicide containing two different weeding principles for the resistance of the herbicide in practical application and the problem of soil residue, so as to improve the control effect of the herbicide, delay the generation of the resistance, and reduce the application amount. Reduce the cost of prevention.
  • Another object of the present invention is to provide an application of the above composition for controlling weeds in the agricultural field.
  • the object of the invention can be achieved by the following measures:
  • the present invention provides a synergistic herbicidal composition
  • a synergistic herbicidal composition comprising the active ingredients A and B, wherein the active ingredient A is diflufenic acid and the active ingredient B is pyrimidinyl ether.
  • the active ingredient of the composition of the present invention may contain only A and B, and may further contain other active ingredients without affecting the overall performance of the composition.
  • the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 50:50 to 1.
  • the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 30:30 to 1.
  • the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 20:20 to 1.
  • the weight ratio between the two components of A and B can be arbitrarily adjusted within the range of the following ratios: 50:1, 45:1, 40:1, 35:1, 30: 1, 29:1, 28:1, 27:1, 26:1, 25:1, 24:1, 23:1, 22:1, 21:1, 20:1, 19:1, 18:1 17:1, 16:1, 15:1, 14:1, 13:1, 12:1, 11:1, 10:1, 9:1, 8:1, 7:1, 6:1, 5: 1, 4:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, 1:20, 1:21, 1: 22, 1:23, 1:24, 1:25, 1:26, 1:27, 1:28, 1:29, 1:30, 1:35:, 1:40, 1:45, 1:50 It is also possible to select within the range consisting of any two of the above ratios.
  • composition provided by the present invention can be formulated into a pesticide-acceptable dosage form together with an active ingredient and an agrochemical adjuvant.
  • the active ingredient pyridoxal and pyrimethoxam has a mass content of 5 to 85%, preferably 5 to 75%.
  • compositions of the present invention may also comprise carriers, adjuvants and/or surfactants. Common auxiliaries can be mixed during the application.
  • Suitable auxiliaries may be solid or liquid, they are usually materials commonly used in the processing of dosage forms, such as natural or regenerated minerals, solvents, dispersants, wetting agents, adhesives, thickeners, binders or fertilizers. .
  • the method of application of the compositions of the invention comprises the use of the compositions of the invention for aerial parts of plants, in particular leaves or foliage.
  • the frequency of administration and the amount administered will depend on the biological and climatic conditions of the pathogen.
  • Can produce plants Long sites, such as rice fields, are wetted with a liquid formulation of the composition, or the composition is applied to the soil in solid form, such as in the form of granules (soil application), the composition can be introduced from the soil into the plant through the roots of the plant (inhalation) effect).
  • compositions may be applied only by the active ingredient (also referred to as the active ingredient) or may be used in combination with the additives, so that the composition of the present invention can be prepared into various dosage forms such as a suspending agent, a dispersible oil suspension, and an aqueous emulsion. , emulsifiable concentrate, water-dispersible granules, etc.
  • the compositions may be applied by spraying, misting, dusting, spreading or pouring, and the like.
  • composition of the present invention can be prepared into various dosage forms by a known method, for example, the active ingredient and an auxiliary agent such as a solvent, a solid carrier, and if necessary, can be uniformly mixed with a surfactant and ground to prepare a desired form.
  • an auxiliary agent such as a solvent, a solid carrier, and if necessary, can be uniformly mixed with a surfactant and ground to prepare a desired form.
  • the above solvent may be selected from aromatic hydrocarbons, preferably containing from 8 to 12 carbon atoms, such as a mixture of xylenes or substituted benzenes, phthalates such as dibutyl phthalate or dicaprylic acid, aliphatic hydrocarbons such as rings.
  • aromatic hydrocarbons preferably containing from 8 to 12 carbon atoms, such as a mixture of xylenes or substituted benzenes, phthalates such as dibutyl phthalate or dicaprylic acid, aliphatic hydrocarbons such as rings.
  • Alkenes or paraffins, alcohols and glycols and their ethers and esters such as ethanol, ethylene glycol, ethylene glycol monomethyl
  • ketones such as cyclohexanone
  • highly polar solvents such as N-methyl-2 Pyrrolidone, dimethyl sulfoxide or dimethylformamide
  • vegetable or vegetable oils such as soybean oil.
  • the above solid carriers are typically natural mineral fillers such as talc, kaolin, montmorillonite or activated clay.
  • a highly dispersible silicic acid or a highly dispersible adsorbent polymer carrier such as a particulate adsorbent carrier or a non-adsorbing carrier, and a suitable particulate adsorbent carrier is porous, such as pumice, bentonite or Bentonite; a suitable non-adsorbing carrier such as calcite or sand.
  • a large amount of pre-granulated materials of inorganic or organic nature can be used as a carrier, in particular dolomite.
  • Suitable surfactants are lignosulfonic acid, naphthalenesulfonic acid, phenolsulfonic acid, alkaline earth metal or amine salts, alkylarylsulfonates, alkyl groups Sulfates, alkyl sulfonates, fatty alcohol sulphates, fatty acids and sulfated fatty alcohol glycol ethers, as well as condensates of sulfonated naphthalene and naphthalene derivatives with formaldehyde, naphthalene or naphthalene sulfonic acid with phenol and formaldehyde Condensate, polyoxyethylene octyl phenyl ether, ethoxylated isooctyl phenol, octyl phenol, nonyl phenol, alkyl aryl polyglycol ether, tributyl benzene poly
  • the two active ingredients in the compositions of the present invention exhibit synergistic effects, the activity of which is more pronounced than the expected sum of activity using a single compound, and the individual activity of a single compound.
  • the synergistic effect is manifested by allowing for a reduced application rate, a broader herbicidal control profile, quicker effect, longer lasting control effect, better control of weeds by only one or a few applications, and widening of possible application intervals . These characteristics are particularly needed to control weed control practices.
  • the herbicidal composition of the invention can be applied to the control of crop weeds in the agricultural field, in particular to control weeds and calves Or weeds such as flat stalks.
  • the other characteristics exhibited by the herbicidal composition of the present invention are mainly as follows: 1. Since the chemical composition of the two single agents of the present composition is very different, the mechanism of action is completely different, and there is no cross-resistance, and two single agents can be delayed. The resulting resistance problem is used alone; 2. The composition of the present invention is safe and effective against crops. It has been proved by experiments that the herbicide composition of the invention has stable chemical properties, remarkable synergistic effect, and exhibits obvious synergistic effect and complementary effect on the control object.
  • the active ingredient flufenic acid and pyrimethoxam, auxiliary agent and filler are uniformly mixed according to the formula, pulverized into a wettable powder by air flow, and then added with a certain amount of water to be mixed and granulated, and after being sieved by drying. A water dispersible granule product is obtained.
  • Example 1 72% flufenacetate pyrimidine ether water dispersible granules
  • Example 2 72% flufenacetate pyrimidine ether water dispersible granules
  • the active ingredient pyripramine and pyrimethoxam, dispersant, wetting agent, thickener and water are mixed uniformly according to the formula, and after sanding and/or high-speed shearing, semi-finished products are obtained. After the analysis, the water is added and uniformly filtered to obtain the finished product.
  • the surfactant is mixed with the oil base and mixed in proportion, and the active ingredient piracetamide and pyrimidin are added under shearing and stirring, and ground in a sand mill and ground until a certain range of particle diameter is can.
  • Example 6 25% flufenacetate ⁇ pyrimidine ether dispersible oil suspension agent
  • the active ingredient flufenacetamide is mixed with pyrimidine oxalate, solvent and auxiliary agent under mechanical agitation, then added to the emulsifier and stabilizer to be evenly stirred. Finally, water is added and stirred at a speed of 100-12000 rpm. 10-30 minutes to make it a homogeneous milky product.
  • Example 8 42% flufenacetate pyrimidine ether water emulsion
  • the disease index and control effect were calculated.
  • the control effect is converted into the probability value (y)
  • the concentration of the drug solution ( ⁇ g/ml) is converted into the logarithm value (x)
  • the virulence equation is calculated by the least squares method and the concentration EC50 is suppressed
  • the virulence index of the drug is calculated according to the method of Sun Yunpei. Grade Co-toxicity coefficient (CTC).
  • CTC Grade Co-toxicity coefficient
  • Measured virulence index (ATI) (standard drug EC50 / test drug EC50) * 100
  • Theoretical virulence index (TTI) A virulence index * Percentage of A in the mixture + B virulence index * Percentage of B in the mixture
  • CTC Co-toxicity coefficient [mixture measured virulence index (ATI) / mixed theory virulence index (TTI)] * 100
  • CTC ⁇ 80 the composition showed antagonism, 80 ⁇ CTC ⁇ 120, the composition showed an additive effect, CTC ⁇ 120, and the composition showed synergistic effect.

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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

Disclosed in the present invention is a weeding composition having synergistic effects, and in particular a herbicide composition for effectively preventing and removing weeds. The composition comprises a component A and a component B, where component A is diflufenican and component B is pyribenzoxim. Pharmacodynamic tests show that the composition has positive characteristics of strong complementarity, obvious synergistic effect, increased weed control spectrum, reduced application amount, prolonged appropriate application time, high crop safety, reduced environmental pollution, good environmental compatibility, and the like.

Description

具有增效作用的除草组合物Synergistic herbicidal composition 技术领域Technical field
本发明属于农业植物保护领域,特别是涉及一种具有改进性能的除草组合物。The invention belongs to the field of agricultural plant protection, and in particular relates to a herbicidal composition with improved properties.
背景技术Background technique
活性组分吡氟酰草胺(diflufenican)该药属于类胡萝卜素生物合成抑制剂。导致叶绿素破坏及细胞破裂,植物死亡。吡氟草胺是一种酰胺类除草剂,在杂草发芽前后施用可在土表形成抗淋溶的药土层,在作物整个生长期保持活性。当杂草萌发通过药土层幼芽或根系均能吸收药剂,吡氟草胺具有抑制类胡萝卜素生物合成作用,吸收药剂的杂草植株中类胡萝卜素含量下降,导致叶绿素被破坏,细胞膜破裂,杂草则表现为幼芽脱色或白色,最后整株萎蔫死亡。The active ingredient diflufenican is a carotenoid biosynthesis inhibitor. Causes chlorophyll destruction and cell rupture, and plant death. Isoflufena is an amide herbicide that can form an anti-leaching medicinal soil layer on the soil surface before and after germination of the weeds to maintain activity throughout the growing period of the crop. When weeds germinate through the shoots or roots of the drug layer, the flirazone can inhibit the carotenoid biosynthesis, and the carotenoid content in the weed plants of the absorption agent decreases, causing the chlorophyll to be destroyed and the cell membrane to rupture. Weeds are characterized by decolorization or whitening of the young shoots, and finally the entire plant is wilted and dead.
嘧啶肟草醚(Pyribenzoxim)为稻田用广谱除草剂,新颖的肟酯类化合物,广谱选择性芽后除草剂。作用机制与磺酰脲类及咪唑呆酮类除草剂相似,均属乙酰乳酸合成酶(ALS)抑制剂。对水稻、普通小麦、结缕草具有选择性超高效芽后除草活性,无芽前除草活性,用于防除稗草、大穗看麦娘、辣蓼等各种禾本科杂草和阔叶杂划效果卓著,对水稻、普通小麦安全。药剂除草速度较慢,施药后能抑制杂草生长,但须在2周后枯死。药剂用药适度较宽,对稗草1.5~6.5叶期均有效。在2.5~3.5叶期,以10g/h剂量即可达100%防除;3.5~4.5叶期增加到20g/h剂量即可达100%防除。Pyribenzoxim is a broad-spectrum herbicide for rice fields, a novel oxime ester compound, and a broad-spectrum selective post-emergence herbicide. The mechanism of action is similar to sulfonylureas and imidazolium herbicides, all of which are acetolactate synthase (ALS) inhibitors. It has selective super-efficient post-emergence herbicidal activity against rice, common wheat and Zoysiagrass, and has no pre-emergence herbicidal activity. It is used to control various grasses and broadleaf weeds such as valerian, big stalk, maiden and spicy sorghum. The effect of the plan is outstanding, and it is safe for rice and common wheat. The herbicide weeding rate is slower and can inhibit weed growth after application, but it must die after 2 weeks. The drug is moderately broad and effective for the 1.5 to 6.5 leaf stage of Valerian. In the 2.5-3.5 leaf stage, 100% control can be achieved at a dose of 10g/h; a dose of 20g/h can be achieved in the 3.5-4.5 leaf stage to achieve 100% control.
实际的农药经验已经表明,重复且专一施用一种活性化合物来防治杂草在很多情况下将导致杂草的快速选择性,目前通常使用不同活性化合物的混合物来防治有害杂草。通过将具有不同作用机理的活性化合物进行组合,可延缓抗性产生,降低施用量,减少防治成本。Practical pesticide experience has shown that repeated and specific application of one active compound to control weeds will in many cases lead to rapid selectivity of weeds, and mixtures of different active compounds are currently commonly used to control harmful weeds. By combining active compounds having different mechanisms of action, resistance can be delayed, application rates can be reduced, and cost of control can be reduced.
发明内容Summary of the invention
本发明的目的是针对除草剂在实际应用中抗性以及土壤残留问题,筛选出含有两种不同除草原理的除草剂进行复配,以提高除草剂防治效果,延缓抗性产生,降低施用量,减少防治成本。The purpose of the invention is to screen the herbicide containing two different weeding principles for the resistance of the herbicide in practical application and the problem of soil residue, so as to improve the control effect of the herbicide, delay the generation of the resistance, and reduce the application amount. Reduce the cost of prevention.
本发明的另一个目的是提供上述组合物在农业领域防治杂草的应用。Another object of the present invention is to provide an application of the above composition for controlling weeds in the agricultural field.
本发明的目的可以通过以下措施达到: The object of the invention can be achieved by the following measures:
本发明提供了一种具有增效作用的除草组合物,该组合物中含有有效成分A和B,其中有效成分A为吡氟酰草胺,有效成分B为嘧啶肟草醚。The present invention provides a synergistic herbicidal composition comprising the active ingredients A and B, wherein the active ingredient A is diflufenic acid and the active ingredient B is pyrimidinyl ether.
发明人通过试验发现,上述除草组合物增效明显,更重要的是施用量减少,降低使用成本。含有组分A与组分B的化合物结构类型不同,作用机制各异,两者复配能够扩大除草谱,并且可以在一定程度上延缓杂草抗性的产生和发展速度,且组分A与组分B之间无交互抗性。The inventors found through experiments that the above herbicidal compositions have obvious synergistic effects, and more importantly, the application amount is reduced, and the use cost is lowered. The compounds containing component A and component B have different structural types and different mechanisms of action. The combination of the two can expand the herbicidal spectrum, and can delay the generation and development of weed resistance to some extent, and component A and There is no cross-resistance between component B.
本发明组合物的有效成分可以只包含A和B,也可以在不影响组合物整体性能的基础上,进一步包含其他有效成分。The active ingredient of the composition of the present invention may contain only A and B, and may further contain other active ingredients without affecting the overall performance of the composition.
在一种方案中,该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的重量比为1~50:50~1。In one embodiment, the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 50:50 to 1.
在另一种方案中,该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的重量比为1~30:30~1。In another embodiment, the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 30:30 to 1.
在另一种方案中,该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的重量比为1~20:20~1。In another embodiment, the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 20:20 to 1.
在一种优选的方案中,A和B两组分之间的重量比可以任意地在下述配比的范围内进行调整:50:1、45:1、40:1、35:1、30:1、29:1、28:1、27:1、26:1、25:1、24:1、23:1、22:1、21:1、20:1、19:1、18:1、17:1、16:1、15:1、14:1、13:1、12:1、11:1、10:1、9:1、8:1、7:1、6:1、5:1、4:1、3:1、2:1、1:1、1:2、1:3、1:4、1:5、1:6、1:7、1:8、1:9、1:10、1:11、1:12、1:13、1:14、1:15、1:16、1:17、1:18、1:19、1:20、1:21、1:22、1:23、1:24、1:25、1:26、1:27、1:28、1:29、1:30,1:35:、1:40、1:45、1:50也可以在以上任意两个配比所组成的范围内进行选择。In a preferred embodiment, the weight ratio between the two components of A and B can be arbitrarily adjusted within the range of the following ratios: 50:1, 45:1, 40:1, 35:1, 30: 1, 29:1, 28:1, 27:1, 26:1, 25:1, 24:1, 23:1, 22:1, 21:1, 20:1, 19:1, 18:1 17:1, 16:1, 15:1, 14:1, 13:1, 12:1, 11:1, 10:1, 9:1, 8:1, 7:1, 6:1, 5: 1, 4:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, 1:20, 1:21, 1: 22, 1:23, 1:24, 1:25, 1:26, 1:27, 1:28, 1:29, 1:30, 1:35:, 1:40, 1:45, 1:50 It is also possible to select within the range consisting of any two of the above ratios.
本发明提供的组合物可以由有效成分与农药助剂共同制成农药上可接受的剂型。The composition provided by the present invention can be formulated into a pesticide-acceptable dosage form together with an active ingredient and an agrochemical adjuvant.
在组合物中,有效成分吡氟酰草胺与嘧啶肟草醚的质量含量为5~85%,优选5~75%。In the composition, the active ingredient pyridoxal and pyrimethoxam has a mass content of 5 to 85%, preferably 5 to 75%.
本发明的组合物还可以包含载体、助剂和/或表面活性剂。在施用的过程中可以混合常用的助剂。The compositions of the present invention may also comprise carriers, adjuvants and/or surfactants. Common auxiliaries can be mixed during the application.
合适的助剂可以是固体或液体,它们通常是剂型加工过程中常用的物质,例如天然的或再生的矿物质,溶剂、分散剂、润湿剂、胶粘剂、增稠剂、粘合剂或肥料。Suitable auxiliaries may be solid or liquid, they are usually materials commonly used in the processing of dosage forms, such as natural or regenerated minerals, solvents, dispersants, wetting agents, adhesives, thickeners, binders or fertilizers. .
本发明组合物的施用方法包括将本发明的组合物用于植物生长的地上部分,特别是叶部或叶面。施用的频率和施用量取决于病原体的生物学和气候生存条件。可以将植物的生 长场所,如稻田,用组合物的液体制剂浸湿,或者将组合物以固体形式施用于土壤中,如以颗粒形式(土壤施用),组合物可以由土壤经植物根部进入植物体内(内吸作用)。The method of application of the compositions of the invention comprises the use of the compositions of the invention for aerial parts of plants, in particular leaves or foliage. The frequency of administration and the amount administered will depend on the biological and climatic conditions of the pathogen. Can produce plants Long sites, such as rice fields, are wetted with a liquid formulation of the composition, or the composition is applied to the soil in solid form, such as in the form of granules (soil application), the composition can be introduced from the soil into the plant through the roots of the plant (inhalation) effect).
这些组合物可以仅仅包含活性成分(又称有效成分)进行施用,也可以与添加剂一起混合使用,因此本发明的组合物可以制备成各种剂型,例如悬浮剂、可分散油悬浮剂、水乳剂、乳油、水分散粒剂等。根据这些组合物的性质以及施用组合物所要达到的目的和环境情况,可以选择将组合物以喷雾、弥雾、喷粉、撒播或泼浇等之类的方法施用。These compositions may be applied only by the active ingredient (also referred to as the active ingredient) or may be used in combination with the additives, so that the composition of the present invention can be prepared into various dosage forms such as a suspending agent, a dispersible oil suspension, and an aqueous emulsion. , emulsifiable concentrate, water-dispersible granules, etc. Depending on the nature of the compositions and the intended purpose and environmental conditions to which the compositions are to be applied, the compositions may be applied by spraying, misting, dusting, spreading or pouring, and the like.
可用已知的方法可以将本发明的组合物制备成各种剂型,如可以将有效成分与助剂,如溶剂、固体载体,需要时可以与表面活性剂一起均匀混合、研磨,制备成所需要的剂型。The composition of the present invention can be prepared into various dosage forms by a known method, for example, the active ingredient and an auxiliary agent such as a solvent, a solid carrier, and if necessary, can be uniformly mixed with a surfactant and ground to prepare a desired form. Formulation.
上述的溶剂可选自芳香烃,优选含8-12个碳原子,如二甲苯混合物或取代的苯,酞酸酯类,如酞酸二丁酯或酞酸二辛酸,脂肪烃类,如环已烷或石蜡,醇和乙二醇和它们的醚和酯,如乙醇,乙二醇,乙二醇单甲基;酮类,如环已酮,强极性的溶剂,如N-甲基-2-吡咯烷酮,二甲基亚砜或二甲基甲酰胺,和植物油或植物油,如大豆油。The above solvent may be selected from aromatic hydrocarbons, preferably containing from 8 to 12 carbon atoms, such as a mixture of xylenes or substituted benzenes, phthalates such as dibutyl phthalate or dicaprylic acid, aliphatic hydrocarbons such as rings. Alkenes or paraffins, alcohols and glycols and their ethers and esters, such as ethanol, ethylene glycol, ethylene glycol monomethyl; ketones, such as cyclohexanone, highly polar solvents such as N-methyl-2 Pyrrolidone, dimethyl sulfoxide or dimethylformamide, and vegetable or vegetable oils such as soybean oil.
上述的固体载体,如用于粉剂和可分散剂的通常是天然矿物填料,例如滑石、高岭土,蒙脱石或活性白土。为了管理组合物的物理性能,也可以加入高分散性硅酸或高分散性吸附聚合物载体,例如粒状吸附载体或非吸附载体,合适的粒状吸附载体是多孔型的,如浮石、皂土或膨润土;合适的非吸附载体如方解石或砂。另外,可以使用大量的无机性质或有机性质的预制成粒状的材料作为载体,特别是白云石。The above solid carriers, such as those used in powders and dispersibles, are typically natural mineral fillers such as talc, kaolin, montmorillonite or activated clay. In order to manage the physical properties of the composition, it is also possible to add a highly dispersible silicic acid or a highly dispersible adsorbent polymer carrier, such as a particulate adsorbent carrier or a non-adsorbing carrier, and a suitable particulate adsorbent carrier is porous, such as pumice, bentonite or Bentonite; a suitable non-adsorbing carrier such as calcite or sand. In addition, a large amount of pre-granulated materials of inorganic or organic nature can be used as a carrier, in particular dolomite.
根据本发明的组合物中的有效成分的化学性质,合适的表面活性剂为木质素磺酸、萘磺酸、苯酚磺酸、碱土金属盐或胺盐,烷基芳基磺酸盐,烷基硫酸盐,烷基磺酸盐,脂肪醇硫酸盐,脂肪酸和硫酸化脂肪醇乙二醇醚,还有磺化萘和萘衍生物与甲醛的缩合物,萘或萘磺酸与苯酚和甲醛的缩合物,聚氧乙烯辛基苯基醚,乙氧基化异辛基酚,辛基酚,壬基酚,烷基芳基聚乙二醇醚,三丁基苯聚乙二醇醚,三硬脂基苯基聚乙二醇醚,烷基芳基聚醚醇,乙氧基化蓖麻油,聚氧乙烯烷基醚,氧化乙烯缩合物、乙氧基化聚氧丙烯,月桂酸聚乙二醇醚缩醛,山梨醇酯,木质素亚硫酸盐废液和甲基纤维素。Suitable surfactants according to the chemical nature of the active ingredient in the composition of the present invention are lignosulfonic acid, naphthalenesulfonic acid, phenolsulfonic acid, alkaline earth metal or amine salts, alkylarylsulfonates, alkyl groups Sulfates, alkyl sulfonates, fatty alcohol sulphates, fatty acids and sulfated fatty alcohol glycol ethers, as well as condensates of sulfonated naphthalene and naphthalene derivatives with formaldehyde, naphthalene or naphthalene sulfonic acid with phenol and formaldehyde Condensate, polyoxyethylene octyl phenyl ether, ethoxylated isooctyl phenol, octyl phenol, nonyl phenol, alkyl aryl polyglycol ether, tributyl benzene polyglycol ether, three Stearyl phenyl polyglycol ether, alkyl aryl polyether alcohol, ethoxylated castor oil, polyoxyethylene alkyl ether, ethylene oxide condensate, ethoxylated polyoxypropylene, lauric acid poly Glycol ether acetal, sorbitol ester, lignin sulfite waste liquor and methyl cellulose.
本发明的组合物中两种有效成分表现为增效效果,该组合物的活性比使用单个化合物的活性预期总和,以及单个化合物的单独活性更为显著。增效效果表现为允许施用量减少、更宽的除草控制谱、见效快、更持久的防治效果、通过仅仅一次或少数几次施用更好的控制杂草、以及加宽了可能的施用间隔时间。这些特性是防除控制杂草实践过程中特别需要的。The two active ingredients in the compositions of the present invention exhibit synergistic effects, the activity of which is more pronounced than the expected sum of activity using a single compound, and the individual activity of a single compound. The synergistic effect is manifested by allowing for a reduced application rate, a broader herbicidal control profile, quicker effect, longer lasting control effect, better control of weeds by only one or a few applications, and widening of possible application intervals . These characteristics are particularly needed to control weed control practices.
本发明的除草组合物可应用在农业领域防治农作物杂草方面,特别是防治稗草、鲤肠 或扁秆藨草等杂草。The herbicidal composition of the invention can be applied to the control of crop weeds in the agricultural field, in particular to control weeds and calves Or weeds such as flat stalks.
本发明的除草组合物的表现出的其它特点主要表现为:1、由于本组合物的两个单剂化学结构差异很大,作用机理完全不同,不存在交互抗性,可延缓两个单剂单独使用所产生的抗性问题;2、本发明的组合物对作物安全、防效好。经试验证明,本发明除草剂组合物化学性质稳定,增效显著,对防治对象表现出明显的增效以及互补作用。The other characteristics exhibited by the herbicidal composition of the present invention are mainly as follows: 1. Since the chemical composition of the two single agents of the present composition is very different, the mechanism of action is completely different, and there is no cross-resistance, and two single agents can be delayed. The resulting resistance problem is used alone; 2. The composition of the present invention is safe and effective against crops. It has been proved by experiments that the herbicide composition of the invention has stable chemical properties, remarkable synergistic effect, and exhibits obvious synergistic effect and complementary effect on the control object.
具体实施方式detailed description
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明,凡在本发明的精神和原则之内所做的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。In order to make the objects, technical solutions and advantages of the present invention more comprehensible, the present invention will be further described in detail below with reference to the embodiments. It is understood that the specific embodiments described herein are intended to be illustrative of the invention and are not to be construed as limiting the scope of the invention. Within the scope of protection of the present invention.
以下实施例所有配方中百分比均为重量百分比。本发明组合物各种制剂的加工工艺均为现有技术,根据不同情况可以有所变化。The percentages in all formulations in the following examples are percentages by weight. The processing techniques of the various formulations of the compositions of the present invention are all prior art and may vary depending on the circumstances.
一、剂型制备实施例First, the dosage form preparation example
(一)水分散粒剂的加工及实施例(1) Processing and examples of water-dispersible granules
将活性成分吡氟酰草胺与嘧啶肟草醚、助剂和填料按配方的比例混合均匀,经气流粉碎成可湿性粉剂,再加入一定量的水混合挤压造粒,经干燥筛分后制得水分散粒剂产品。The active ingredient flufenic acid and pyrimethoxam, auxiliary agent and filler are uniformly mixed according to the formula, pulverized into a wettable powder by air flow, and then added with a certain amount of water to be mixed and granulated, and after being sieved by drying. A water dispersible granule product is obtained.
实施例1:72%吡氟酰草胺·嘧啶肟草醚水分散粒剂Example 1: 72% flufenacetate pyrimidine ether water dispersible granules
吡氟酰草胺70%,嘧啶肟草醚2%,烷基萘磺酸钠3%,十二烷基磺酸钠4%,硫酸铵3%,轻质碳酸钙补足至100%。Pyridoxal 70%, pyrimethoxam 2%, sodium alkylnaphthalene sulfonate 3%, sodium dodecyl sulfate 4%, ammonium sulfate 3%, light calcium carbonate supplemented to 100%.
实施例2:72%吡氟酰草胺·嘧啶肟草醚水分散粒剂Example 2: 72% flufenacetate pyrimidine ether water dispersible granules
吡氟酰草胺2%,嘧啶肟草醚70%,十二烷基硫酸钠3%,甲基萘磺酸钠甲醛缩合物4%,木质素磺酸钠4%,硅藻土补足至100%。2% pyridoxamine, 70% pyrimethoxine, 3% sodium lauryl sulfate, 4% formaldehyde sodium phthalate condensate, 4% sodium lignin sulfonate, diatomaceous earth up to 100 %.
(二)悬浮剂的加工及实施例(2) Processing and examples of suspending agents
将活性成分吡氟酰草胺与嘧啶肟草醚、分散剂、润湿剂、增稠剂和水等各组分按配方的比例混合均匀,经砂磨和/或高速剪切后,得到半成品,分析后补加水混合均匀过滤即得成品。The active ingredient pyripramine and pyrimethoxam, dispersant, wetting agent, thickener and water are mixed uniformly according to the formula, and after sanding and/or high-speed shearing, semi-finished products are obtained. After the analysis, the water is added and uniformly filtered to obtain the finished product.
实施例3:55%吡氟酰草胺·嘧啶肟草醚悬浮剂Example 3: 55% flufenacetate pyrimidine ether suspension
吡氟酰草胺50%,嘧啶肟草醚5%,乙二醇6%,黄原胶0.6%,膨润土3%,木质素磺酸钠6%,硅酸铝镁2%,水补足至100%。50% pyriflufenacetate, 5% pyrithione, 6% ethylene glycol, 0.6% xanthan gum, 3% bentonite, 6% sodium lignosulfonate, 2% magnesium aluminum silicate, water to 100% %.
实施例4:55%吡氟酰草胺·嘧啶肟草醚悬浮剂 Example 4: 55% flufenacetate pyrimidine ether suspension
吡氟酰草胺5%,嘧啶肟草醚50%,丙三醇6%,甲基萘磺酸钠甲醛缩合物5%,膨润土4%,水补足至100%。Pyrfluoxetamine 5%, pyrimidine valerate 50%, glycerol 6%, sodium methylnaphthalene sulfonate formaldehyde condensate 5%, bentonite 4%, water to 100%.
(三)可分散油悬浮剂的加工及实施例(3) Processing and examples of dispersible oil suspension concentrates
将表面活性剂与油基混合等按比例充分混合,在搞度剪切搅拌下加入活性成分吡氟酰草胺、嘧啶肟草醚,在砂磨机中研磨,研磨直到一定范围的粒径即可。The surfactant is mixed with the oil base and mixed in proportion, and the active ingredient piracetamide and pyrimidin are added under shearing and stirring, and ground in a sand mill and ground until a certain range of particle diameter is can.
实施例5:25%吡氟酰草胺·嘧啶肟草醚可分散油悬浮剂Example 5: 25% flufenacetate·pyrimidine ether dispersible oil suspension agent
吡氟酰草胺20%,嘧啶肟草醚5%,木质素磺酸钙8%,黄原胶1%,矿物油补足至100%。20% of flufenacetamide, 5% of pyrithione, 8% of calcium lignosulfonate, 1% of xanthan gum, and 100% of mineral oil.
实施例6:25%吡氟酰草胺·嘧啶肟草醚可分散油悬浮剂Example 6: 25% flufenacetate·pyrimidine ether dispersible oil suspension agent
吡氟酰草胺5%,嘧啶肟草醚20%,烷基聚氧乙基醚磺酸盐2%,N-邻苯二甲酸二甲酯5%,大豆油补足至100%。Pyrfluoxetamine 5%, pyrimethoxam 20%, alkyl polyoxyethyl ether sulfonate 2%, N-phthalic acid dimethyl ester 5%, soy oil supplemented to 100%.
(四)水乳剂的加工及实施例(4) Processing and examples of water emulsion
将活性成分吡氟酰草胺与嘧啶肟草醚、溶剂、助剂在机械搅拌下混合均匀,然后投入乳化剂和稳定剂搅拌均匀,最后加入水,在100-12000转/分钟的转速下搅拌10-30分钟,使之成为均匀乳状的产品。The active ingredient flufenacetamide is mixed with pyrimidine oxalate, solvent and auxiliary agent under mechanical agitation, then added to the emulsifier and stabilizer to be evenly stirred. Finally, water is added and stirred at a speed of 100-12000 rpm. 10-30 minutes to make it a homogeneous milky product.
实施例7:42%吡氟酰草胺·嘧啶肟草醚水乳剂Example 7: 42% flufenacetate pyrimidine ether water emulsion
吡氟酰草胺40%,嘧啶肟草醚2%,N-邻苯二甲酸二甲酯5%,2,6-二叔丁基-4-甲基苯酚3%,聚乙烯醇3%,乙二醇4%,苯甲酸钠1%,有机硅消泡剂0.8%,壬基酚苯氧乙烯醚4%,水补足至100%。40% pyridoxal, 2% pyrithione, 5% N-phthalic acid dimethyl, 2,6-di-tert-butyl-4-methylphenol 3%, polyvinyl alcohol 3%, Ethylene glycol 4%, sodium benzoate 1%, silicone defoamer 0.8%, nonylphenol phenoxy ether 4%, water to 100%.
实施例8:42%吡氟酰草胺·嘧啶肟草醚水乳剂Example 8: 42% flufenacetate pyrimidine ether water emulsion
吡氟酰草胺2%,嘧啶肟草醚40%,乙二醇3%,烷基聚氧乙基醚磺酸盐3%,黄原胶4%,聚乙烯醇2%,聚异丁二酸酐-聚乙二醇共聚物5%,有机硅消泡剂1.2%,水补足至100%。2% pyridoxamine, 40% pyrithione, 3% ethylene glycol, 3% alkyl polyoxyethyl ether sulfonate, 4% xanthan gum, 2% polyvinyl alcohol, polyisobutyl The anhydride-polyethylene glycol copolymer was 5%, the silicone defoamer was 1.2%, and the water was made up to 100%.
实施例9:10%吡氟酰草胺·嘧啶肟草醚水乳剂Example 9: 10% flufenacetate pyrimidine ether water emulsion
吡氟酰草胺5%,嘧啶肟草醚5%,丁基羟基茴香醚5%,丙二醇2%,苯甲酸钠0.8%,聚乙烯醇2%,甲基萘磺酸钠甲醛缩合物4%,有机硅消泡剂1.0%,水补足至100%。Pyrfluoxetamine 5%, pyrimidine 5%, butylhydroxyanisole 5%, propylene glycol 2%, sodium benzoate 0.8%, polyvinyl alcohol 2%, sodium methylnaphthalene sulfonate formaldehyde condensate 4%, The silicone defoamer is 1.0% and the water is made up to 100%.
二、药效验证试验Second, the efficacy test
(一)生物测定实施例1(1) Bioassay Example 1
以吡氟酰草胺作为标准药剂,计算病情指数和防治效果。将防治效果换算成几率值(y),药液浓度(μg/ml)转换成对数值(x),以最小二乘法计算毒力方程和抑制中浓度EC50,依孙云沛法计算药剂的毒力指数级共毒系数(CTC)。毒力测定结果见表1。 Using flufenic acid as a standard agent, the disease index and control effect were calculated. The control effect is converted into the probability value (y), the concentration of the drug solution (μg/ml) is converted into the logarithm value (x), the virulence equation is calculated by the least squares method and the concentration EC50 is suppressed, and the virulence index of the drug is calculated according to the method of Sun Yunpei. Grade Co-toxicity coefficient (CTC). The virulence test results are shown in Table 1.
实测毒力指数(ATI)=(标准药剂EC50/供试药剂EC50)*100Measured virulence index (ATI) = (standard drug EC50 / test drug EC50) * 100
理论毒力指数(TTI)=A药剂毒力指数*混剂中A的百分含量+B药剂毒力指数*混剂中B的百分含量Theoretical virulence index (TTI) = A virulence index * Percentage of A in the mixture + B virulence index * Percentage of B in the mixture
共毒系数(CTC)=[混剂实测毒力指数(ATI)/混剂理论毒力指数(TTI)]*100Co-toxicity coefficient (CTC) = [mixture measured virulence index (ATI) / mixed theory virulence index (TTI)] * 100
CTC≤80,组合物表现为拮抗作用,80<CTC<120,组合物表现为相加作用,CTC≥120,组合物表现为增效作用。CTC ≤ 80, the composition showed antagonism, 80 < CTC < 120, the composition showed an additive effect, CTC ≥ 120, and the composition showed synergistic effect.
1、吡氟酰草胺与嘧啶肟草醚复配对水稻田稗草的毒力测定试验1. The virulence test of piracetamide and pyrimethasone combined with rice sedge
表1吡氟酰草胺与嘧啶肟草醚不同配比复配对稗草的毒力测定分析(一)Table 1 Determination of the virulence of the different ratios of pyridoxal and pyrimethoxam to the valerian (1)
Figure PCTCN2017086260-appb-000001
Figure PCTCN2017086260-appb-000001
结果(表1)表明,吡氟酰草胺与嘧啶肟草醚在配比1~50:1~50之间,尤其是1~30:1~30之间,共毒系数均在126以上,说明吡氟酰草胺与嘧啶肟草醚复配对水稻田稗草的防除具有显著的协同增效作用。实验发现,两种有效成分的配比不在上述范围时对稗草的防除没有协同作用。The results (Table 1) showed that the ratio of flufenacetamide to pyrimethasone was between 1 and 50:1 to 50, especially between 1 and 30:1 to 30, and the co-toxicity coefficient was above 126. It is indicated that the combination of diflufenic acid and pyrimidinide has significant synergistic effect on the control of rice straw. It has been found that there is no synergistic effect on the control of valerian when the ratio of the two active ingredients is out of the above range.
2、吡氟酰草胺与嘧啶肟草醚复配对鲤肠的毒力测定试验(二)2. The virulence test of the combination of piracetamide and pyrimethasone in the sputum (2)
表2吡氟酰草胺与嘧啶肟草醚复配对杂草鲤肠的毒力测定结果分析Table 2 Analysis of the virulence determination results of the combination of pyridoxal and pyrimidin
Figure PCTCN2017086260-appb-000002
Figure PCTCN2017086260-appb-000002
Figure PCTCN2017086260-appb-000003
Figure PCTCN2017086260-appb-000003
结果(表2)表明,吡氟酰草胺与嘧啶肟草醚在配比1~50:1~50之间,共毒系数均在120以上,说明吡氟酰草胺与嘧啶肟草醚复配对杂草鲤肠的防除具有显著的协同增效作用。实验发现,两种有效成分的配比不在上述范围时对鲤肠的防除没有协同作用。The results (Table 2) showed that the ratio of the co-toxicity of the pyridoxamine to the pyrimidinyl ether was between 1 and 50:1 to 50, and the co-toxicity coefficient was above 120, indicating that the pyridoxamide and the pyrimidin are complex. The control of paired weeds has a significant synergistic effect. It has been found that there is no synergistic effect on the control of the calf when the ratio of the two active ingredients is out of the above range.
(二)田间药效试验(2) Field efficacy test
1、利用本发明制得的实施例来验证吡氟酰草胺与嘧啶肟草醚的田间防治效果。1. The field control effect of flufenacetate and pyrimethoxam was verified by the examples prepared by the present invention.
Figure PCTCN2017086260-appb-000004
Figure PCTCN2017086260-appb-000004
预期防效(%)=X+Y-XY/100(其中,X,Y为单剂防效)Expected control effect (%) = X + Y-XY / 100 (where X, Y is a single dose control)
表3.吡氟酰草胺与嘧啶肟草醚复配对扁秆藨草的田间防效试验结果Table 3. Field control trial results of piracetamide and pyrimidine valerate in combination with stalk
Figure PCTCN2017086260-appb-000005
Figure PCTCN2017086260-appb-000005
Figure PCTCN2017086260-appb-000006
Figure PCTCN2017086260-appb-000006
Figure PCTCN2017086260-appb-000007
Figure PCTCN2017086260-appb-000007
测定结果(表3)表明,吡氟酰草胺与嘧啶肟草醚复配对防治杂草鸭舌草和碎米莎草的防效明显提高,说明二者复配对杂草鸭舌草和碎米莎草有显著的协同增效作用。 The results of the determination (Table 3) showed that the synergistic effect of the combination of diflufenic acid and pyrimidin on the control of weeds and shredded sedge was significantly improved, indicating that the two were matched with weeds and broken rice. Sedge has a significant synergistic effect.

Claims (10)

  1. 一种具有增效作用的除草组合物,其特征在于该组合物中含有有效成分吡氟酰草胺与嘧啶肟草醚。A synergistic herbicidal composition characterized in that the composition contains the active ingredients pyrfluoxal and pyricarb.
  2. 根据权利要求1所述的除草组合物,其特征在于该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的重量比为1~50:50~1。The herbicidal composition according to claim 1, wherein the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 50:50 to 1.
  3. 根据权利要求2所述的除草组合物,其特征在于该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的重量比为1~30:30~1。The herbicidal composition according to claim 2, wherein the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 30:30 to 1.
  4. 根据权利要求3所述的除草组合物,其特征在于该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的重量比为1~20:20~1。The herbicidal composition according to claim 3, wherein the weight ratio of the active ingredient flufenic acid to pyrimidinide in the composition is from 1 to 20:20 to 1.
  5. 根据权利要求1所述的除草组合物,其特征在于该组合物由有效成分与农药助剂共同制成农药上可接受的剂型。The herbicidal composition according to claim 1, wherein the composition is formulated into a pesticide-acceptable dosage form together with an active ingredient and an agrochemical adjuvant.
  6. 根据权利要求5所述的除草组合物,其特征在于该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的质量含量为5~85%。The herbicidal composition according to claim 5, wherein the active ingredient pyridoxal and pyrimethoxam in the composition has a mass content of 5 to 85%.
  7. 根据权利要求6所述的除草组合物,其特征在于该组合物中有效成分吡氟酰草胺与嘧啶肟草醚的质量含量为5~75%。The herbicidal composition according to claim 6, wherein the active ingredient pyridoxal and pyrimethoxam in the composition has a mass content of 5 to 75%.
  8. 根据权利要求5所述的除草组合物,其特征在于所述剂型为水分散粒剂、水乳剂、悬浮剂或可分散油悬浮剂。The herbicidal composition according to claim 5, characterized in that the dosage form is a water-dispersible granule, an aqueous emulsion, a suspending agent or a dispersible oil suspending agent.
  9. 权利要求1所述的除草组合物在农业领域防治农作物杂草方面的用途。Use of the herbicidal composition of claim 1 for controlling crop weeds in the agricultural sector.
  10. 权利要求9所述的用途,其特征在于所述杂草选自稗草、鲤肠或扁秆藨草。 The use according to claim 9, characterized in that the weed is selected from the group consisting of valerian, calf or stalk.
PCT/CN2017/086260 2016-05-30 2017-05-27 Weeding composition having synergistic effects WO2017206825A1 (en)

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