WO2018028318A1 - Weeding composition having synergistic effect - Google Patents

Weeding composition having synergistic effect Download PDF

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Publication number
WO2018028318A1
WO2018028318A1 PCT/CN2017/090018 CN2017090018W WO2018028318A1 WO 2018028318 A1 WO2018028318 A1 WO 2018028318A1 CN 2017090018 W CN2017090018 W CN 2017090018W WO 2018028318 A1 WO2018028318 A1 WO 2018028318A1
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active ingredient
sec
butyl
herbicidal composition
composition
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PCT/CN2017/090018
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French (fr)
Chinese (zh)
Inventor
仲汉根
季自华
季红进
花伟
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江苏辉丰农化股份有限公司
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Publication of WO2018028318A1 publication Critical patent/WO2018028318A1/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
    • A01N33/00Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/16Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
    • A01N33/18Nitro compounds

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.
  • Pilofenapamide is an amide herbicide that is applied before and after weed germination to form an anti-leaching soil layer on the soil surface and to maintain activity throughout the growing period of the crop.
  • the penicillin can inhibit the carotenoid biosynthesis, and the content of carotenoids in the weed plants of the absorption agent decreases, causing the chlorophyll to be destroyed, and the cell membrane
  • the worm breaks the weeds show that the young shoots are discolored or white, and finally the whole plant wilted and died.
  • the active ingredient sec-butyl is also known as butralin, which is a contact-killing and topical systemic bud-inhibiting agent. It is a low-toxic dinitroaniline tobacco bud inhibitor. It has high potency for inhibiting axillary bud growth and its efficacy. fast. It can be used without the rain within 2 hours after application.
  • the pure product of bud bud is orange-yellow crystal, melting point 54 ° C ⁇ 58 ° C, soluble in chlorinated hydrocarbons and aromatic hydrocarbon solvents, stable under both alkaline and acidic conditions.
  • Zhong Dingling is a herbicide for selective pre-emergence soil treatment.
  • the agent After entering the plant, the agent mainly inhibits the cell division of the meristem, thereby inhibiting the growth of weed shoots and young roots. It can also be used as a plant growth regulator to control the growth of tobacco axillary buds. Applicable to soybean, cotton, rice, corn, sunflower, potato, peanut, watermelon, sugar beet, sugar cane and vegetable crops, such as annual sedge weeds, goosegrass, crabgrass, foxtail, and other dicotyledonous weeds . It also has a good control effect on the soybean field.
  • 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 active ingredients A and B, active ingredient A being diflufenic acid, and active ingredient B being sec-butyl.
  • 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 of the herbicidal composition of the present invention to pyridoxal and sec-butyl is from 1:0.1 to 50.
  • the weight ratio of the active ingredient of the herbicidal composition of the present invention to pyridoxal and sec-butyl is from 1:1 to 50.
  • the weight ratio of the active ingredient of the herbicidal composition of the present invention to pyridoxal and sec-butyl is from 1:1 to 40.
  • the weight ratio between the two components of A and B can be arbitrarily adjusted within the range of the following ratios: 1:0.1, 1:0.2, 1:0.3, 1:0.4, 1: 0.5, 1:0.6, 1:0.7, 1:0.8, 1:0.9, 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, 1:31, 1:32, 1:33, 1:34, 1:35, 1:36, 1:37, 1:38, 1:39, 1:40, 1:41, 1:42, 1:43, 1:44, 1:45, 1: 46, 1:47, 1:48, 1:49, 1:50, can also be selected within the range of any of the above two ratios, these ratios can be understood as the weight ratios: 0.5,
  • composition of the present invention can be formulated into a pesticide-acceptable dosage form together with an active ingredient and an agrochemical adjuvant.
  • the mass of the active ingredient in the composition of the present invention may be from 2 to 95%, preferably from 5 to 80%.
  • a carrier, an adjuvant and/or a surfactant may be included in the composition of the present invention.
  • 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 composition of the invention comprises the use of the composition of the invention for aerial parts of plants, in particular leaves Department or leaf surface.
  • the frequency of administration and the amount administered will depend on the biological and climatic conditions of the pathogen.
  • the plant growth site such as rice fields, may be wetted with a liquid formulation of the composition, or the composition may be applied to the soil in solid form, such as in the form of granules (soil application), the composition may be passed from the soil to the plant through the roots of the plant. In vivo (systemic action).
  • compositions may be applied only by the active ingredient (also referred to as the active ingredient), or may be used in combination with an additive or an auxiliary agent, so that the composition of the present invention can be prepared into various dosage forms such as a wettable powder, a suspending agent, or the like.
  • Dispersing oil suspending agents, water emulsions, emulsifiable concentrates, water-dispersible granules, and the like 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 special in controlling weed practices needs.
  • the herbicidal composition of the present invention can be applied to the control of crop weeds in the agricultural field, in particular to control goosegrass, foxtail, valerian or crabgrass.
  • 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 is fully mixed with the active ingredient sec-butyl spirit, various auxiliaries and fillers, etc., and pulverized by an ultrafine pulverizer to obtain a wettable powder.
  • Example 1 42% flufenacetin zhongdingling wettable powder
  • Example 2 51% flufenacetin zhongdingling wettable powder
  • the active ingredient pyripramine and zhongdingling, an emulsifier, an organic solvent and the like are uniformly mixed in a ratio of the formulation to obtain a finished product.
  • Example 3 11% flufenacetate sec-butyl emulsifiable concentrate
  • Example 5 31% flufenacetate sec-butyl emulsifiable concentrate
  • the active ingredient pyripramine and zhongdingling, an emulsifier, a dispersing agent, an organic solvent, an antifreezing agent and the like are uniformly mixed in a ratio of the formulation to obtain a finished product.
  • 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.

Abstract

Provided is a weeding composition having a synergistic effect, said composition containing the active ingredients of diflufenican and butralin. The weight ratio of the active ingredient diflufenican to butralin may be 1:0.1~50. Pharmacodynamic tests have shown that the composition has positive features of having strong complementarity, evident synergistic effect, increased weed control spectrum, reduced application amount, prolonged appropriate application time, high crop safety, reduced environmental pollution, good environmental compatibility, and so on.

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。吡氟酰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,吡氟酰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. Pilofenapamide is an amide herbicide that is applied before and after weed germination to form an anti-leaching soil layer on the soil surface and to maintain activity throughout the growing period of the crop. When weeds germinate through the shoots or roots of the soil, the penicillin can inhibit the carotenoid biosynthesis, and the content of carotenoids in the weed plants of the absorption agent decreases, causing the chlorophyll to be destroyed, and the cell membrane When the worm breaks, the weeds show that the young shoots are discolored or white, and finally the whole plant wilted and died.
活性组分仲丁灵又名止芽素(butralin),为触杀兼局部内吸性抑芽剂,属于低毒性的二硝基苯胺类烟草抑芽剂,对抑制腋芽的生长效力高,药效快。在施药后2小时内不下雨其药效便可发挥。止芽素的纯品为橙黄色结晶,熔点54℃~58℃,易溶于氯代烃及芳香烃类溶剂中,在碱性及酸性条件下均稳定。仲丁灵为选择性芽前土壤处理的除草剂,药剂进入植物体后,主要抑制分生组织的细胞分裂,从而抑制杂草幼芽及幼根生长。亦可作植物生长调节剂使用,控制烟草腋芽生长。适用于大豆、棉花、水稻、玉米、向日葵、马铃薯、花生、西瓜、甜菜、甘蔗和蔬菜等作物田中防除稗草、牛筋草、马唐,狗尾草等一年生单子叶杂草及部分双子叶杂草。对大豆田菟丝子也有较好的防除效果。The active ingredient sec-butyl is also known as butralin, which is a contact-killing and topical systemic bud-inhibiting agent. It is a low-toxic dinitroaniline tobacco bud inhibitor. It has high potency for inhibiting axillary bud growth and its efficacy. fast. It can be used without the rain within 2 hours after application. The pure product of bud bud is orange-yellow crystal, melting point 54 ° C ~ 58 ° C, soluble in chlorinated hydrocarbons and aromatic hydrocarbon solvents, stable under both alkaline and acidic conditions. Zhong Dingling is a herbicide for selective pre-emergence soil treatment. After entering the plant, the agent mainly inhibits the cell division of the meristem, thereby inhibiting the growth of weed shoots and young roots. It can also be used as a plant growth regulator to control the growth of tobacco axillary buds. Applicable to soybean, cotton, rice, corn, sunflower, potato, peanut, watermelon, sugar beet, sugar cane and vegetable crops, such as annual sedge weeds, goosegrass, crabgrass, foxtail, and other dicotyledonous weeds . It also has a good control effect on the soybean field.
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.
本发明的另一目的是提供一种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,有效成分A为吡氟酰草胺,有效成分B为仲丁灵。The present invention provides a synergistic herbicidal composition comprising active ingredients A and B, active ingredient A being diflufenic acid, and active ingredient B being sec-butyl.
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,本发明除草组合物的有效成分吡氟酰草胺和仲丁灵的重量比为1:0.1~50。In one embodiment, the weight ratio of the active ingredient of the herbicidal composition of the present invention to pyridoxal and sec-butyl is from 1:0.1 to 50.
在另一种方案中,本发明除草组合物的有效成分吡氟酰草胺和仲丁灵的重量比为1:1~50。In another embodiment, the weight ratio of the active ingredient of the herbicidal composition of the present invention to pyridoxal and sec-butyl is from 1:1 to 50.
在另一种方案中,本发明除草组合物的有效成分吡氟酰草胺和仲丁灵的重量比为1:1~40。In another embodiment, the weight ratio of the active ingredient of the herbicidal composition of the present invention to pyridoxal and sec-butyl is from 1:1 to 40.
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:1:0.1、1:0.2、1:0.3、1:0.4、1:0.5、1:0.6、1:0.7、1:0.8、1:0.9、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、1:31、1:32、1:33、1:34、1:35、1:36、1:37、1:38、1:39、1:40、1:41、1:42、1:43、1:44、1:45、1:46、1:47、1:48、1:49、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,这些比例可以理解为重量比,也可以包括摩尔比。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: 1:0.1, 1:0.2, 1:0.3, 1:0.4, 1: 0.5, 1:0.6, 1:0.7, 1:0.8, 1:0.9, 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, 1:31, 1:32, 1:33, 1:34, 1:35, 1:36, 1:37, 1:38, 1:39, 1:40, 1:41, 1:42, 1:43, 1:44, 1:45, 1: 46, 1:47, 1:48, 1:49, 1:50, can also be selected within the range of any of the above two ratios, these ratios can be understood as the weight ratio, can also include the molar ratio.
本发明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 of the present invention can be formulated into a pesticide-acceptable dosage form together with an active ingredient and an agrochemical adjuvant.
本发明的组合物中有效成分的质量含量可以为2~95%,优选5~80%。The mass of the active ingredient in the composition of the present invention may be from 2 to 95%, preferably from 5 to 80%.
本发明组合物中可以包含载体、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。A carrier, an adjuvant and/or a surfactant may be included in the composition of the present invention. 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 composition of the invention comprises the use of the composition of the invention for aerial parts of plants, in particular leaves Department or leaf surface. The frequency of administration and the amount administered will depend on the biological and climatic conditions of the pathogen. The plant growth site, such as rice fields, may be wetted with a liquid formulation of the composition, or the composition may be applied to the soil in solid form, such as in the form of granules (soil application), the composition may be passed from the soil to the plant through the roots of the plant. In vivo (systemic action).
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,也可以与添加剂或助剂一起混合使用,因此本发明的组合物可以制备成各种剂型,例如可湿性粉剂、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 an additive or an auxiliary agent, so that the composition of the present invention can be prepared into various dosage forms such as a wettable powder, a suspending agent, or the like. Dispersing oil suspending agents, water emulsions, emulsifiable concentrates, water-dispersible granules, and the like. 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 special in controlling weed practices needs.
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,特别是防治牛筋草、狗尾草、稗草或马唐草。The herbicidal composition of the present invention can be applied to the control of crop weeds in the agricultural field, in particular to control goosegrass, foxtail, valerian or crabgrass.
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)可湿性粉剂的加工及实施例(1) Processing and examples of wettable powders
将活性成分吡氟酰草胺与活性成分仲丁灵与各种助剂及填料等按比例充分混合,经超细粉碎机粉碎后制得可湿性粉剂。The active ingredient flufenic acid is fully mixed with the active ingredient sec-butyl spirit, various auxiliaries and fillers, etc., and pulverized by an ultrafine pulverizer to obtain a wettable powder.
实施例1: 42%吡氟酰草胺·仲丁灵可湿性粉剂Example 1: 42% flufenacetin zhongdingling wettable powder
吡氟酰草胺2%,仲丁灵40%,膨润土4%,木质素磺酸钠5%,甲基萘磺酸钠甲醛缩合物4%,高岭土补足至100%。2% diflufenic acid, 40% sec-butyl, 4% bentonite, 5% sodium lignosulfonate, 4% formaldehyde sodium methoxide sulfonate, and kaolin up to 100%.
实施例2: 51%吡氟酰草胺·仲丁灵可湿性粉剂Example 2: 51% flufenacetin zhongdingling wettable powder
吡氟酰草胺1%,仲丁灵50%,脂肪醇硫酸钾4%,苯磺酸钠4%,皂土4%,白炭黑补足至100%。1% pyridoxamine, 50% sec-butyl, 4% potassium sulphate, 4% sodium benzene sulfonate, 4% bentonite, and 100% silica.
(二)乳油的加工及实施例(2) Processing and examples of emulsifiable concentrate
将活性成分吡氟酰草胺与仲丁灵、乳化剂、有机溶剂等各组分按配方的比例混合均匀即得成品。The active ingredient pyripramine and zhongdingling, an emulsifier, an organic solvent and the like are uniformly mixed in a ratio of the formulation to obtain a finished product.
实施例3: 11%吡氟酰草胺·仲丁灵乳油Example 3: 11% flufenacetate sec-butyl emulsifiable concentrate
吡氟酰草胺10%,仲丁灵1%,辛基酚5%,甲苯补足至100%。10% piracetamide, 1% sec-butyl, 5% octylphenol, and 100% toluene.
实施例4: 5.5%吡氟酰草胺·仲丁灵乳油Example 4: 5.5% flufenacetate sec-butyl emulsifiable concentrate
吡氟酰草胺0.5%,仲丁灵5%,三丁基苯聚乙二醇醚4%,二甲苯补足至100%。 Pyrfluoxetamine 0.5%, sec-butyl 5%, tributyl phenyl polyglycol ether 4%, xylene up to 100%.
实施例5: 31%吡氟酰草胺·仲丁灵乳油Example 5: 31% flufenacetate sec-butyl emulsifiable concentrate
吡氟酰草胺1%,仲丁灵30%,山梨醇酯8%,二甲苯补足至100%。1% diflufenic acid, 30% sec-butyl, 8% sorbitol, and 100% xylene.
(三)水乳剂的加工及实施例(III) Processing and examples of water emulsion
将活性成分吡氟酰草胺与仲丁灵、乳化剂、分散剂、有机溶剂、抗冻剂等各组分按配方的比例混合均匀即得成品。The active ingredient pyripramine and zhongdingling, an emulsifier, a dispersing agent, an organic solvent, an antifreezing agent and the like are uniformly mixed in a ratio of the formulation to obtain a finished product.
实施例6: 20%吡氟酰草胺·仲丁灵水乳剂Example 6: 20% flufenacetate sec-butyl spirit water emulsion
吡氟酰草胺10%,仲丁灵10%,甲基纤维素8%,聚乙烯醇4%,乙二醇5%,二甲苯8%,冰乙酸0.2%,水补足至100%。10% piracetamide, 10% sec-butyl, 8% methylcellulose, 4% polyvinyl alcohol, 5% ethylene glycol, 8% xylene, 0.2% glacial acetic acid, and 100% water.
实施例7: 41%吡氟酰草胺·仲丁灵水乳剂Example 7: 41% flufenacetate sec-butyl spirit water emulsion
吡氟酰草胺1%,仲丁灵40%,甲基萘磺酸钠甲醛缩合物5%,甲苯8%,环己酮10%,硫酸铵5%,冰乙酸0.5%,水补足至100%。1% pyridoxamine, 40% sec-butyl, sodium methoxide sulfonate 5%, toluene 8%, cyclohexanone 10%, ammonium sulfate 5%, glacial acetic acid 0.5%, water to 100 %.
二、药效验证试验Second, the efficacy test
(一)生物测定实施例(1) Bioassay examples
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、吡氟酰草胺与仲丁灵复配对水稻青稗的毒力测定试验1. The virulence test of penicillin and zhongdingling combined with rice barley
表1 吡氟酰草胺与仲丁灵不同配比复配对水稻青稗的毒力测定分析(一)Table 1 Determination of virulence of different ratios of pyridoxamide and sec-butyl ping to rice sorghum (1)
Figure PCTCN2017090018-appb-000001
Figure PCTCN2017090018-appb-000001
Figure PCTCN2017090018-appb-000002
Figure PCTCN2017090018-appb-000002
结果(表1)表明,吡氟酰草胺与仲丁灵在配比1:0.1~50之间,共毒系数均在127以上,说明吡氟酰草胺与仲丁灵复配对水稻青稗的防除具有显著的协同增效作用。实验发现,吡氟酰草胺与仲丁灵的复配比例不在本发明的范围内时难以具有协同增效作用。The results (Table 1) showed that the ratio of flufenacetin to sec-butyl was between 1:0.1 and 50, and the co-toxicity coefficient was above 127, indicating that the combination of flufenacetin and sec-butyl ping was combined with rice sorghum. The control has a significant synergistic effect. It has been found that it is difficult to have a synergistic effect when the compounding ratio of flufenacetin to sec-butyl is not within the scope of the present invention.
2、吡氟酰草胺与仲丁灵复配对双穗雀稗的毒力测定试验(二)2. The virulence test of diflufenic acid and zhongdingling paired with double-spotted gar. (2)
表2 吡氟酰草胺与仲丁灵复配对双穗雀稗的毒力测定结果分析Table 2 Analysis of virulence determination results of diflufenic acid and zhongdingling complex
Figure PCTCN2017090018-appb-000003
Figure PCTCN2017090018-appb-000003
结果(表2)表明,吡氟酰草胺与仲丁灵在配比1:0.1~50之间,共毒系数均在130以上,说明吡氟酰草胺与仲丁灵复配对双穗雀稗的防除具有显著的协同增效作用。实验发现,吡氟酰草胺与仲丁灵的复配比例不在本发明的范围内时难以具有协同增效作用。The results (Table 2) showed that the ratio of pyridoxal to sec-butyl was between 1:0.1 and 50, and the co-toxicity coefficient was above 130, indicating that the combination of flufenacet and zhongdingling The control of cockroaches has a significant synergistic effect. It has been found that it is difficult to have a synergistic effect when the compounding ratio of flufenacetin to sec-butyl is not within the scope of the present invention.
(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仲丁灵的田间防治效果。1. The field control effect of flufenyl and sec-butyl is verified by the examples prepared by the present invention.
Figure PCTCN2017090018-appb-000004
Figure PCTCN2017090018-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.吡氟酰草胺与仲丁灵复配对鸭舌草和红根稗草的田间防效试验结果Table 3. Field control trial results of pyriflufen and zhongdingling in combination with ragweed and red radish
Figure PCTCN2017090018-appb-000005
Figure PCTCN2017090018-appb-000005
Figure PCTCN2017090018-appb-000006
Figure PCTCN2017090018-appb-000006
测定结果(表3)表明,吡氟酰草胺与仲丁灵复配对防治鸭舌草和红根稗草的防效明显提高,说明二者复配对杂鸭舌草和红根稗草有显著的协同增效作用。 The results of the determination (Table 3) showed that the control effect of flufenacet and zhongdingling on the control of ragweed and red radish was significantly improved, indicating that the combination of the two pairs of sage and red geranium was significant. Synergistic synergy.

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和仲丁灵。A synergistic herbicidal composition characterized by comprising the active ingredients pyrfluoxal and sec-butyl.
  2. 根据权利要求1所述的除草组合物,其特征在于所述有效成分吡氟酰草胺和仲丁灵的重量比为1:0.1~50。The herbicidal composition according to claim 1, wherein the weight ratio of the active ingredient flufenic acid to sec-butyl is 1:0.1 to 50.
  3. 根据权利要求2所述的除草组合物,其特征在于所述有效成分吡氟酰草胺和仲丁灵的重量比为1:1~50。The herbicidal composition according to claim 2, wherein the weight ratio of the active ingredient of diflufenic acid to sec-butyl is from 1:1 to 50.
  4. 根据权利要求3所述的除草组合物,其特征在于所述有效成分吡氟酰草胺和仲丁灵的重量比为1:1~40。The herbicidal composition according to claim 3, wherein the weight ratio of the active ingredient of diflufenic acid to sec-butyl is from 1:1 to 40.
  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的质量含量为2~98%。The herbicidal composition according to claim 5, wherein the active ingredient has a mass content of from 2 to 98%.
  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的质量含量为5~80%。The herbicidal composition according to claim 6, wherein the active ingredient in the composition has a mass content of from 5 to 80%.
  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可湿性粉剂、水乳剂或乳油。The herbicidal composition according to claim 5, characterized in that the dosage form is a wettable powder, an aqueous emulsion or an emulsifiable concentrate.
  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. 根据权利要求9所述的用途,其特征在于所述杂草选自牛筋草、狗尾草、稗草或马唐草。 The use according to claim 9, characterized in that the weed is selected from the group consisting of goosegrass, foxtail, valerian or crabgrass.
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CN106259345A (en) * 2016-08-08 2017-01-04 江苏辉丰农化股份有限公司 There is the Herbicidal combinations of potentiation

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CN101485319A (en) * 2009-02-19 2009-07-22 山东省农业科学院植物保护研究所 Herbicidal composition containing oxadiazon and butralin
CN104304254A (en) * 2014-09-25 2015-01-28 南京华洲药业有限公司 Mixed herbicide containing diflufenican and ethhoxyfen-ethyl and preparation method thereof
CN106212465A (en) * 2016-05-30 2016-12-14 江苏辉丰农化股份有限公司 A kind of Herbicidal combinations comprising diflufenican and butralin
CN106259345A (en) * 2016-08-08 2017-01-04 江苏辉丰农化股份有限公司 There is the Herbicidal combinations of potentiation

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US4875925A (en) * 1986-07-21 1989-10-24 May & Baker Limited Herbicidal method using diflufenican
CN101485319A (en) * 2009-02-19 2009-07-22 山东省农业科学院植物保护研究所 Herbicidal composition containing oxadiazon and butralin
CN104304254A (en) * 2014-09-25 2015-01-28 南京华洲药业有限公司 Mixed herbicide containing diflufenican and ethhoxyfen-ethyl and preparation method thereof
CN106212465A (en) * 2016-05-30 2016-12-14 江苏辉丰农化股份有限公司 A kind of Herbicidal combinations comprising diflufenican and butralin
CN106259345A (en) * 2016-08-08 2017-01-04 江苏辉丰农化股份有限公司 There is the Herbicidal combinations of potentiation

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