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CN116267936B - A herbicidal composition and its application - Google Patents

A herbicidal composition and its application Download PDF

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Publication number
CN116267936B
CN116267936B CN202310318259.XA CN202310318259A CN116267936B CN 116267936 B CN116267936 B CN 116267936B CN 202310318259 A CN202310318259 A CN 202310318259A CN 116267936 B CN116267936 B CN 116267936B
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sodium
propanil
picloram
weight ratio
composition according
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CN116267936A (en
Inventor
李志清
刘兰花
袁冰
王建伟
孙鹏
何金栓
魏斌斌
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Shandong Weifang Rainbow Chemical Co Ltd
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Shandong Weifang Rainbow Chemical Co Ltd
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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
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/22Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01GHORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00Protection of plants
    • 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/30Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
    • 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
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P13/00Herbicides; Algicides

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

Abstract

本发明公开了一种除草组合物及其应用,涉及农药领域,其包括如下重量百分含量的原料:敌稗5‑60%、绿草定1‑40%、毒莠定0.1‑22%、分散剂3‑15%、润湿剂2‑10%、崩解剂10‑40%,填料余量。本发明的三元复配组合物的水分散粒剂,经过筛选合适分散剂、润湿剂和填料,可最终解决热储后崩解和悬浮问题,所制备的水分散粒剂具有崩解快、分散性好、悬浮率高、稳定性好的特点,更有利于药效的发挥。The invention discloses a herbicidal composition and its application, and relates to the field of pesticides. The composition comprises the following raw materials in percentage by weight: 5-60% of propanil, 1-40% of triclopyr, 0.1-22% of picloram, 3-15% of dispersant, 2-10% of wetting agent, 10-40% of disintegrant, and the rest of filler. The water-dispersible granules of the ternary composite composition of the invention can ultimately solve the problems of disintegration and suspension after heat storage by screening suitable dispersants, wetting agents and fillers. The prepared water-dispersible granules have the characteristics of fast disintegration, good dispersibility, high suspension rate and good stability, and are more conducive to the exertion of drug efficacy.

Description

Weeding composition and application thereof
Technical Field
The invention relates to the technical field of pesticides, in particular to a weeding composition and application thereof.
Background
The rice is used as the first large grain crop in China, the rice field has more than 200 weeds in the whole rice area, wherein 40 main weeds with common and serious harm are commonly generated, the area of the main weeds which are generated by barnyard grass is the largest, and the main weeds also comprise heterogenous nutgrass, glossoside, semen euphorbiae, euonymus alatus and amaranth.
Propanil (chemical name N- (3 ',4' -dichlorophenyl) propanamide) Propanil pure product is white needle-like crystal. m.p.92-93℃and vapor pressure 1.2X10 -2 Pa (60 ℃). The solubility is 54% of ethanol, 60% of dimethylformamide, 35% of cyclohexanone, 25% of methyl ethyl ketone, 3% of toluene and 3% of dimethylbenzene, and the water is 225mg/L. Hydrolysis to 3, 4-dichloroaniline and propionic acid in strongly acidic and strongly basic media. It is easy to decompose in soil, so it is not suitable for soil treatment. Propanil is an amide-type, highly selective contact herbicide that is barely transmitted in plants, but acts at the site of contact of the agent. The action mechanism plays a role in many aspects, not only damaging photosynthesis of plants, but also inhibiting respiration and oxidative phosphorylation, interfering nucleic acid and protein synthesis, and the like. So that the physiological function of the sensitive plant is influenced, the water loss is accelerated, the leaves are gradually dried, and finally the plant dies. The composition is mainly used for seedling fields or direct seeding fields, is a special-effect drug for preventing and killing barnyard grass, and can also be used for preventing and killing various grass weeds and dicotyledonous weeds, such as glossodes anatipestifer, cress, crabgrass, green bristlegrass and the like.
Triclopyr (Triclopyr, 3,5, 6-trichloro-2-pyridyloxyacetic acid), triclopyr, systemic herbicide, pure white solid, decomposition temperature 208 ℃, melting point 150.5 ℃, relative density 1.85 (21 ℃), vapor pressure 0.2mPa (25 ℃), solubility (25 DEG Cg/L) water 0.408, acetone 581, toluene 19.2, acetonitrile 92.1, dichloromethane 24.9, methanol 665, ethyl acetate 271, hexane 0.09. Is acidic (pK.3.97), and is stable to hydrolysis. Acting on nucleic acid metabolism to make plant produce excessive nucleic acid, converting some tissues into raw tissues, causing abnormal growth of leaf, stem and root, exhaustion of storage substance, embolism or rupture of vascular bundle tissue and death of plant. The triclopyr is a conduction herbicide which can be quickly absorbed by leaf surfaces and root systems and is transmitted to the whole body of plants, and the triclopyr is a broadleaf herbicide which is ineffective against grassy weeds and sedge weeds and is used for preventing and killing broadleaf weeds and shrubs in young forest lands of conifer trees.
Picloram (piclor am, 4-amino-3, 5, 6-trichloropyridine-2-carboxylic acid) is an auxinic herbicide, picloram is a white powder, has a chlorine odor, a melting point of 215 ℃ and a vapor pressure of 0.082mPa (35 ℃). Solubility in water 430mg/L and acetone 19.8g/L. The solubility of the potassium salt in water at 25 ℃ is 400g/L. Is stable to acid and alkali. The stable period is 28 days under the condition of 50 ℃, and the half life period in soil is 30-330 days. Hormone herbicides. Can be absorbed and conducted by leaves, roots and stems of plants. Can be quickly conducted to a growing point to cause deformity, wilting, defoliation and necrosis of the upper part of a plant, and the xylem catheter is blocked and discolored to finally cause death. The mechanism of action is to inhibit respiration of the mitochondrial system and nucleic acid metabolism. Can be widely used for preventing and controlling broadleaf weeds. Picloram and its salts are rapidly absorbed and transmitted by leaves and roots, to which most broadleaf crops except for cruciferous crops are sensitive, and most gramineous crops are resistant. Is used for weeding in wheat fields, corn fields and forest lands.
Herbicide varieties containing a single active component often have defects of different degrees in agricultural weed control, such as narrow weeding spectrum, easy generation of drug resistance of weeds after continuous use, and increased environmental pollution after frequent use. The proper compound herbicide has the positive characteristics of strong complementation, obvious synergistic effect, expanded control spectrum, reduced application amount, prolonged application period, high safety to crops, reduced environmental pollution, strong compatibility with the environment and the like, and is also increasingly popular in the market. The recent years have seen problems with the widespread use of two-component combinations of propanil and triclopyr, in that weeds gradually exhibit resistance and the dosage increases.
Therefore, there is a need for new herbicides that solve the above problems.
Disclosure of Invention
Object of the Invention
In order to overcome the defects, the invention aims to provide the weeding composition and the application thereof, and the water dispersible granule of the ternary compound composition can finally solve the problems of disintegration and suspension after heat storage by screening proper dispersing agents, wetting agents and fillers, and the prepared water dispersible granule has the characteristics of quick disintegration, good dispersibility, high suspension rate and good stability, and is more beneficial to the exertion of drug effects. The ternary compound composition can expand the control range, complement and synergize, reduce the product consumption, and has the advantages of low application cost, synergy, drug resistance delay and the like.
Solution scheme
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
In a first aspect, the invention provides a weeding composition, which comprises, by weight, 5-60% of propanil, 1-40% of triclopyr, 0.1-22% of picloram, 3-15% of a dispersing agent, 2-10% of a wetting agent, 10-40% of a disintegrating agent and the balance of a filler.
Further, the composition comprises, by weight, 30-60% of propanil, 2-10% of triclopyr, 1-6% of picloram, 3-15% of a dispersing agent, 2-10% of a wetting agent, 10-40% of a disintegrating agent and the balance of a filler.
Further, the composition comprises, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 3-9% of a dispersing agent, 3-6% of a wetting agent, 10-30% of a disintegrating agent and the balance of a filler.
Further, the composition comprises, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 5-8% of a dispersing agent, 3-5% of a wetting agent, 10-30% of a disintegrating agent and the balance of a filler.
Further, the composition comprises, by weight, 30-50% of propanil, 4-9% of triclopyr, 2-4.5% of picloram, 6-8% of a dispersing agent, 3-5% of a wetting agent, 10-30% of a disintegrating agent and the balance of a filler.
Further, the herbicide composition comprises, by weight, 45-50% of propanil, 8-9% of triclopyr, 4-4.5% of picloram, 6-8% of a dispersing agent, 3-4% of a wetting agent, 20-30% of a disintegrating agent and the balance of a filler.
Further, the dispersing agent is selected from one or more of sodium lignin sulfonate, maleic acid-acrylic acid copolymer salt, polyoxyethylene-polyoxypropylene block copolymer, sodium alkylphenol sulfonate, sodium salt of alkyl naphthalene sulfonate formaldehyde condensate, sodium salt of naphthalene sulfonate formaldehyde condensate, and sodium salt of polycarboxylic acid.
Further, the dispersant comprises sodium lignin sulfonate and sodium polycarboxylate salt in a weight ratio of (2-8): 1, optionally sodium lignin sulfonate and sodium polycarboxylate salt in a weight ratio of (3-6): 1, optionally (3-5): 1, optionally 5:1 or 3:1, optionally one or more of maleic acid-acrylic acid copolymer salt, polyoxyethylene-polyoxypropylene block copolymer, sodium alkylphenol sulfonate, sodium alkyl naphthalene sulfonate formaldehyde condensate and sodium naphthalene sulfonate formaldehyde condensate.
Further, the wetting agent is selected from one or more of sodium dodecyl sulfate, alpha-sulfo fatty acid methyl ester, sodium tetradecyl sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, sodium alkylphenol ethoxylate sulfate, sodium lignin sulfonate, pull-open powder BX, fatty acid sulfate and fatty acid ester sulfate.
Further, the wetting agent comprises (1-5) 1 of alkylphenol ethoxylate sodium sulfate and alkyl naphthalene sulfonate, optionally (2-4) 1 of alkylphenol ethoxylate sodium sulfate and alkyl naphthalene sulfonate, optionally (2-3) 1, optionally 3:1 or 2:1, and optionally one or more of sodium dodecyl sulfate, alpha-sulfo fatty acid methyl ester, sodium tetradecyl sulfate, sodium dodecyl benzene sulfonate, sodium lignin sulfonate, pull-open powder BX, fatty acid sulfate and fatty acid ester sulfate.
Further, the disintegrating agent is one or more of potassium sulfate, diammonium phosphate, urea, sodium sulfate, ammonium nitrate, corn starch, calcium chloride and sodium chloride.
Further, the disintegrating agent comprises sodium sulfate and corn starch in a weight ratio of (1-6): 1, optionally sodium sulfate and corn starch in a weight ratio of (2-4): 1, optionally (2-3): 1, optionally 3:1 or 2:1, and optionally one or more of potassium sulfate, diammonium hydrogen phosphate, urea, ammonium sulfate, ammonium nitrate, calcium chloride and sodium chloride.
Further, the filler is one or two or more of kaolin, bentonite, talcum powder, attapulgite, diatomite, white carbon black, starch and light calcium carbonate.
Optionally, the filler comprises kaolin, and optionally, the filler can further comprise one or two or more of bentonite, talcum powder, attapulgite, diatomite, white carbon black and light calcium carbonate.
Further, the composition is in the form of water dispersible granules.
Further, the herbicide composition comprises, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 4-8% of sodium lignin sulfonate, 1-2% of sodium polycarboxylate, 2-5% of alkylphenol ethoxylate sodium sulfate, 1-2% of sodium alkyl naphthalene sulfonate, 8-20% of sodium sulfate, 4-10% of corn starch and the balance of filler. The weight ratio of the sodium lignin sulfonate to the sodium polycarboxylate salt is (2-8): 1, optionally (3-6): 1, optionally (3-5): 1, optionally 5:1 or 3:1, optionally (2-4): 1, optionally (2-3): 1, optionally 3:1 or 2:1, optionally (2-4): 1, optionally (2-3): 1, optionally 3:1 or 2:1, and 3:1, optionally 3:1 or 2:1.
Further, the herbicide composition comprises, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 4-6% of sodium lignin sulfonate, 1-2% of sodium polycarboxylate, 2-4% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 8-20% of sodium sulfate, 4-10% of corn starch and the balance of filler. Optionally, the weight ratio of the sodium lignin sulfonate to the sodium polycarboxylate salt is (3-6), the weight ratio is (3-5) 1, the weight ratio is 5:1 or 3:1, the weight ratio of the alkylphenol polyoxyethylene sodium sulfate to the sodium alkyl naphthalene sulfonate is (2-4) 1, the weight ratio is (2-3) 1, the weight ratio is 3:1 or 2:1, the weight ratio of the sodium sulfate to the corn starch is (2-4) 1, the weight ratio is (2-3) 1, and the weight ratio is 3:1 or 2:1.
Further, the herbicide composition comprises, by weight, 45-50% of propanil, 8-9% of triclopyr, 4-4.5% of picloram, 5-6% of sodium lignin sulfonate, 1-2% of polycarboxylate sodium salt, 2-3% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 15-20% of sodium sulfate, 5-10% of corn starch and the balance of filler. Optionally, the weight ratio of the sodium lignin sulfonate to the sodium polycarboxylate salt is (3-5): 1, optionally the weight ratio is 5:1 or 3:1, optionally the weight ratio of the sodium sulfate to the corn starch is (2-4): 1, optionally the weight ratio is (2-3): 1, optionally the weight ratio is 3:1 or 2:1.
Further, the herbicide composition comprises the following raw materials, by weight, 45% of propanil, 9% of triclopyr, 4.5% of picloram, 5% of sodium lignin sulfonate, 1% of sodium polycarboxylate, 3% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 15% of sodium sulfate, 5% of corn starch and the balance of filler.
Further, the herbicide composition comprises the following raw materials, by weight, 50% of propanil, 8% of triclopyr, 4% of picloram, 6% of sodium lignin sulfonate, 2% of sodium polycarboxylate, 2% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 20% of sodium sulfate, 10% of corn starch and the balance of filler.
The invention overcomes the defects of difficult suspension and easy sedimentation by combining the dispersing agent and the filler, overcomes the defect of difficult disintegration of particles by combining the wetting agent and the disintegrating agent, and overcomes the defect of easy agglomeration of suspended particles by selecting different types of dispersing agents for combination and screening out the optimal dispersing agent combination.
In a second aspect, there is provided a method for preparing the herbicidal composition of the first aspect, comprising:
Uniformly mixing the triclopyr, the propanil, the picloram, the dispersing agent, the wetting agent, the disintegrating agent and the filler according to a proportion, crushing the mixture to a particle size D 98 of 15-25 mu m by a jet mill, and uniformly mixing the crushed mixture to prepare a dry material, adding water into the dry material to extrude and granulate, wherein the water adding amount is 10-25wt% of the dry material, and drying the dry material at a temperature of 40-50 ℃ to prepare the water dispersible granule containing the propanil, the triclopyr and the picloram;
Optionally, the crushing pressure of the jet mill is 0.5-0.8 Mpa, optionally 0.7Mpa.
In a third aspect, there is provided a herbicidal composition as described in the first aspect or a herbicidal composition prepared by a method as described in the second aspect for controlling farmland weeds, optionally the plant weeds include grassy weeds and/or broadleaf weeds, optionally the grassy weeds include one or more of barnyard grass, anisotropic nutgrass galingale, moleplant seed, green bristlegrass, crabgrass and goosegrass,
Optionally, the broadleaf weeds comprise one or more of herba Oenanthes Javanicae, herba Andrographitis, herba Ocular, herba Portulacae, herba Amaranthi Tricoloris, herba Polygoni Avicularis, and herba Chenopodii.
Advantageous effects
(1) According to the water dispersible granule, propanil, triclopyr and picloram are compounded according to a specific proportion, so that the weeding effect of the preparation can be improved, the weeding spectrum can be expanded, the safety of crops can be improved, and the disintegration performance, the suspension rate and the stability of the preparation are improved through the selection of the auxiliary agent. The water dispersible granule has good application prospect in preventing barnyard grass, anisotropic nutgrass, glossodes and amaranthus manihot in paddy fields. The ternary compound composition can expand the control range, complement and synergize, reduce the product consumption, and has the advantages of low application cost, synergy, drug resistance delay and the like. Can prevent and remove broadleaf weeds on the basis of preventing and removing gramineous weeds, and expands the weeding spectrum. Preventing and treating Gramineae weeds and most broadleaf weeds with serious harm, and is not easy to generate drug resistance.
(2) The water dispersible granule of the ternary compound composition can finally solve the problems of disintegration and suspension after heat storage by screening the proper dispersing agent, wetting agent and filler, and the prepared water dispersible granule has the characteristics of quick disintegration, good dispersibility, high suspension rate and good stability, and is more beneficial to the exertion of drug effects. The screening of the specific dispersing agent, wetting agent and filler not only ensures that the physical property of the formulation is good, but also can improve the drug effect of the composition.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, numerous specific details are set forth in the following description in order to provide a better illustration of the invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, protocols, methods, means, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present invention.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
The herbicide composition provides a new choice for preventing and controlling weeds. The present disclosure is further illustrated by the following examples, but the present disclosure is not limited thereby.
In the following examples, propanil, triclopyr and picloram are added as raw materials, which are commercially available, and other auxiliary agents are commercially available.
The invention is illustrated in further detail by the following examples.
In the preparation of the water dispersible granule, organic salt or inorganic salt is mostly adopted as a dispersing agent, a wetting agent, a disintegrating agent and the like, the triclopyr and picloram raw medicines can form water soluble salts with metal ions or ammonium ions and the like in an auxiliary agent, the propanil has high lipophilicity, the lipophilic propanil and the hydrophilic triclopyr salt and picloram salt generated by the auxiliary agent are both required to be compatible in the same water dispersible granule formula, and the conventional dispersing agent is easy to desorb with the propanil, so that the ternary water dispersible granule with high speed disintegration and high suspension dispersibility is difficult to prepare.
In order to obtain the ternary water dispersible granule with rapid disintegration and good suspension dispersibility, the inventor performs a large amount of screening work on an auxiliary agent system, and the partially screened formula is shown in table 1.
Table 1 raw material compositions of examples and comparative examples
The water dispersible granules of the above examples and comparative examples were prepared according to the following preparation method:
The preparation method comprises the steps of mixing the triclopyr, the propanil, the picloram, the dispersing agent, the wetting agent, the disintegrating agent and the filler uniformly in a mixer, crushing the mixture to the particle size D 98 of 15-25 mu m through an airflow crusher, uniformly mixing the crushed mixture to prepare a dry material, adding water into the dry material to extrude and granulate, adding water accounting for 10-25wt% of the dry material, and drying the dry material at the temperature of 40-50 ℃ to prepare the water dispersible granule containing the propanil, the triclopyr and the picloram. Wherein the crushing pressure of the jet mill is 0.7Mpa.
In the preparation method, after crushing, the powder is detected by a laser particle size distribution instrument until the particle diameter D 98 is between 15 and 25 mu m.
The properties of the water dispersible granules prepared in the above examples and comparative examples were tested, and the results are shown in Table 2.
Wherein, the suspension rate is detected according to the method for detecting the suspension rate of the GB/T14825-2006 pesticide, the wet sieve is detected according to the method for detecting the fineness of 2.2 sections of wet sieve method (suitable for wettable powder) in GB/T16150-1995 pesticide powder, and the heat storage stability is detected according to the method for detecting the heat storage stability of the GB/T19136-2003 pesticide.
Table 2 Water dispersible granule product Properties of examples 1 to 9 and comparative example 1
As can be seen from Table 2, the products of examples 2-6 were stable in quality before and after heat storage, maintained high suspension rate and good wet sieving, indicating that the auxiliary agent formulation of examples 2-6 was better, while the heat storage stability of the products of examples 7-9 was slightly worse than that of examples 2-6, but the performance was also better. In comparative example 1, the dispersing agent, the wetting agent and the disintegrating agent are not properly selected, the preparation has poor dispersion stability, low suspension rate, greatly reduced stability after heat storage, more fine powder and large particles are obtained by screening, and in comparative examples 2-6, the auxiliary agent is properly selected, the suspension rate is higher, and the heat storage stability is better. The variety and the proportion of the auxiliary agent play a key role in the quality of the product.
The invention determines the system with the best matching degree among the components through a large amount of screening work on the components. The dispersing agent and the wetting agent are selected particularly as key, wherein the dispersing agent sodium lignin sulfonate and the polycarboxylic acid sodium salt are preferably selected to ensure the dispersing effect, and the wetting agent sodium alkylphenol ethoxylate sulfate and the alkyl naphthalene sulfonate are preferably selected to ensure the disintegrating and dispersing effects of the active ingredients. The dosage and cost of the product auxiliary agent are greatly reduced, and meanwhile, the product auxiliary agent has excellent disintegration and dispersion properties.
The invention overcomes the defects of difficult suspension and easy sedimentation by combining a specific dispersing agent and a filler, overcomes the defect of difficult disintegration of particles by combining a specific wetting agent and a disintegrating agent, and overcomes the defect of easy agglomeration of suspended particles by selecting different types of dispersing agents for combination and screening out the optimal dispersing agent combination.
Field test example 1 field test Rice field annual weed efficacy test
The application method comprises spraying the herbicide to prevent and treat paddy field weeds in 4-6 leaf stage, diluting with water according to usage times, and applying at maximum temperature of 25deg.C and minimum temperature of 15deg.C in the day of the herbicide application at 9-11 am. A total of 5 treatments were set up, treatment 1 as a clear water spray, a blank control, treatment 2 as examples 1 to 9 and comparative example 1, treatment 3 as comparative example 2 (50% propanil water dispersible granule), treatment 4 as comparative example 3 ((propanil 45% + viridin 9%) water dispersible granule), treatment 5 as comparative example 4 ((propanil 45% + picloram 4.5%) water dispersible granule), treatment 6 as comparative example 5 (viridin 9% water dispersible granule), treatment 7 as comparative example 6 (picloram 4.5% water dispersible granule), treatment 8 as comparative example 7 (viridin 9% + picloram 4.5%) water dispersible granule. The preparations of examples 1 to 9 and comparative examples 1 to 7 were all ready-to-use.
Wherein, the water dispersible granules containing propanil, triclopyr and picloram are prepared in examples 1-9, respectively, and are subjected to stem and leaf spraying treatment according to the dosage of the active ingredients of 130 g/mu, the stem and leaf spraying treatment according to the dosage of the active ingredients of 130 g/mu in comparative example 1, the stem and leaf spraying treatment according to the dosage of the active ingredients of 180 g/mu in comparative example 2 (propanil 50% water dispersible granules), and the stem and leaf spraying treatment according to the dosage of the active ingredients of 180 g/mu in comparative example 3 ((propanil 45% + triclopyr 9%). Comparative example 4 ((propanil 45% + picloram 4.5%) water dispersible granule was subjected to stem and leaf treatment at an active ingredient amount of 180 g/mu, comparative example 5 (triclopyr 9% water dispersible granule) was subjected to stem and leaf treatment at an active ingredient amount of 180 g/mu, comparative example 6 (picloram 4.5%) water dispersible granule was subjected to stem and leaf treatment at an active ingredient amount of 180 g/mu, and comparative example 7 (triclopyr 9% + picloram 4.5%) water dispersible granule was subjected to stem and leaf treatment at an active ingredient amount of 180 g/mu.
The pesticide is applied by a worker pesticide-16 knapsack manual sprayer for 1 time, 450kg of water is added according to the dosage of each hectare preparation to prepare the pesticide liquid, and the pesticide liquid is sprayed uniformly. The weather was good during the test period and the daily average air temperature was 20-25 ℃. The application day is rain-free, and the drug does not rain within 10 days after the drug is applied.
30 Days after application, the fresh weight control effect of each treatment on weeds and the safety of the treatment on rice are investigated. The results are shown in Table 3.
Table 3 results of annual weed efficacy test in paddy fields with various treatments
From the test results of the table, it can be seen that the propanil, the triclopyr and the picloram have good control effects on grassy weeds and broadleaf weeds in paddy fields, and the examples 1 to 9 and the comparative example 1 show obvious synergistic effect compared with the control medicines (treatments 3 to 8), and especially the synergistic effect of the examples 1 to 6 is more remarkable. The special expression is that the treatment 2 is compared with the control medicament treatments 3, 4, 5, 6, 7 and 8, the ternary combination has excellent effect of preventing and killing barnyard grass and heterocyperus, and has synergistic effect on preventing and controlling broadleaf weeds. Compared with the control agent treatment 4, 5 and 8, the treatment 2 has the advantages that the drug effect of the ternary combination on the malignant weeds such as barnyard grass and heterocymbidium faberi with drug resistance is improved, the synergistic effect is achieved, and the control of broadleaf weeds also has the synergistic effect. And compared with the control agent treatment 4, 5 and 8, the treatment 2 has synergistic effect on the control of broadleaf weeds, and the expanded weeding spectrum has excellent control effect on barnyard grass and heterocyperus.
From the comparison of the drug effects of the examples and the comparative examples, the selection of the auxiliary agent has an important effect on the exertion of the effective components, and the improper selection of the auxiliary agent can affect the compounding effect of propanil, triclopyr and picloram. Examples 2 to 6 using the preferred auxiliaries have significantly better control than examples 1, 8, 9.
In addition, according to the whole-course observation of field experiments, the rice field grows well within the range of the experimental dosage, and no phytotoxicity phenomenon appears, which indicates that the compound medicament has no phytotoxicity to the rice field.
According to the invention, through the synergistic combination of the auxiliary agents, particularly the synergistic combination of 3 auxiliary agents including the dispersing agent, the wetting agent, the disintegrating agent and the filler, the processing difficulty of the dosage form is greatly reduced, the stability of the dosage form is improved, and the finally obtained water dispersible granule has the advantages of fast disintegration, good dispersibility, high suspension rate and good stability, and the problems of non-disintegration, poor thermal storage stability and the like of the preparation are effectively solved or reduced.
The ternary compound composition can expand weed control spectrum, increase efficiency and reduce the dosage of the preparation. The water dispersible granule provided by the invention does not use an organic solvent, avoids the adverse factors such as inflammability, explosiveness, environmental hazard and the like, is convenient to weigh and package, thereby avoiding the problems of wall sticking, cleaning and recycling package in the use process, has certain strength and easy disintegration characteristics, basically does not generate dust, and is safe to use.
The invention improves the stability of the product by screening the proper auxiliary agent, can endure the high and low temperature range from 10 ℃ to 54 ℃, effectively solves the influence of environmental change in the transportation process, satisfies the use of different countries and regions, is beneficial to popularization and application in a large range and has excellent drug effect expression.
It should be noted that the above-mentioned embodiments are merely for illustrating the technical solution of the present invention, and not for limiting the same, and although the present invention has been described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that the technical solution described in the above-mentioned embodiments may be modified or some technical features may be equivalently replaced, and these modifications or substitutions do not make the essence of the corresponding technical solution deviate from the spirit and scope of the technical solution of the embodiments of the present invention.

Claims (28)

1. The weeding composition is characterized by comprising, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 3-9% of a dispersing agent, 3-6% of a wetting agent, 10-30% of a disintegrating agent and the balance of a filler;
The dispersing agent comprises sodium lignin sulfonate and sodium polycarboxylate salt in a weight ratio of (2-8): 1;
The wetting agent comprises sodium alkylphenol ethoxylate sulfate and sodium alkyl naphthalene sulfonate with the weight ratio of (2-4) 1;
the disintegrating agent comprises sodium sulfate and corn starch with the weight ratio of (1-6) 1;
The filler is kaolin.
2. The weeding composition according to claim 1, wherein the weeding composition comprises, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 5-8% of a dispersing agent, 3-5% of a wetting agent, 10-30% of a disintegrating agent and the balance of a filler.
3. The weeding composition according to claim 1, wherein the weeding composition comprises, by weight, 30-50% of propanil, 4-9% of triclopyr, 2-4.5% of picloram, 6-8% of a dispersing agent, 3-5% of a wetting agent, 10-30% of a disintegrating agent and the balance of a filler.
4. The weeding composition according to claim 1, which is characterized by comprising, by weight, 45-50% of propanil, 8-9% of triclopyr, 4-4.5% of picloram, 6-8% of a dispersing agent, 3-4% of a wetting agent, 20-30% of a disintegrating agent and the balance of a filler.
5. The herbicidal composition according to claim 1, wherein the weight ratio of sodium lignin sulfonate to sodium polycarboxylate salt in the dispersant is (3-6): 1.
6. The herbicidal composition according to claim 1, wherein the weight ratio of sodium lignin sulfonate to sodium polycarboxylate salt in the dispersant is (3-5): 1.
7. The herbicidal composition of claim 1 wherein the weight ratio of sodium lignin sulfonate to sodium polycarboxylate salt in the dispersant is 5:1.
8. The herbicidal composition of claim 1 wherein the weight ratio of sodium lignin sulfonate to sodium polycarboxylate salt in the dispersant is 3:1.
9. The herbicidal composition according to claim 1, wherein the weight ratio of sodium alkylphenol ethoxylate sulfate to sodium alkylnaphthalene sulfonate is (2-3): 1.
10. The herbicidal composition of claim 1 wherein the weight ratio of sodium alkylphenol ethoxylate sulfate to sodium alkylnaphthalene sulfonate is 3:1.
11. The herbicidal composition of claim 1 wherein the weight ratio of sodium alkylphenol ethoxylate sulfate to sodium alkylnaphthalene sulfonate is 2:1.
12. The herbicidal composition according to any of claims 1 to 11, characterized in that the weight ratio of sodium sulphate to corn starch is (2-4): 1.
13. A herbicidal composition according to any of claims 1 to 11, characterized in that the weight ratio of sodium sulphate to corn starch is (2-3): 1.
14. A herbicidal composition according to any of claims 1 to 11, characterized in that the weight ratio of sodium sulphate to corn starch is 3:1.
15. A herbicidal composition according to any of claims 1 to 11, characterized in that the weight ratio of sodium sulphate to corn starch is 2:1.
16. The herbicidal composition according to any of claims 1 to 11, wherein the formulation of the composition is a water dispersible granule.
17. The weeding composition according to any one of claims 1 to 11, wherein the weeding composition comprises, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 4-8% of sodium lignin sulfonate, 1-2% of sodium polycarboxylate, 2-5% of alkylphenol ethoxylate sodium sulfate, 1-2% of sodium alkyl naphthalene sulfonate, 8-20% of sodium sulfate, 4-10% of corn starch, and the balance of filler.
18. The weeding composition according to any one of claims 1 to 11, which comprises, by weight, 30-50% of propanil, 2-9% of triclopyr, 2-4.5% of picloram, 4-6% of sodium lignin sulfonate, 1-2% of sodium polycarboxylate, 2-4% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 8-20% of sodium sulfate, 4-10% of corn starch, and the balance of filler.
19. The weeding composition according to any one of claims 1 to 11, which comprises, by weight, 45-50% of propanil, 8-9% of triclopyr, 4-4.5% of picloram, 5-6% of sodium lignin sulfonate, 1-2% of sodium polycarboxylate, 2-3% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 15-20% of sodium sulfate, 5-10% of corn starch, and the balance of filler.
20. The weeding composition according to any one of claims 1 to 11, wherein the weeding composition comprises, by weight, 45% of propanil, 9% of triclopyr, 4.5% of picloram, 5% of sodium lignin sulfonate, 1% of polycarboxylate sodium salt, 3% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 15% of sodium sulfate, 5% of corn starch, and the balance of filler.
21. The weeding composition according to any one of claims 1 to 11, wherein the weeding composition comprises, by weight, 50% of propanil, 8% of triclopyr, 4% of picloram, 6% of sodium lignin sulfonate, 2% of sodium polycarboxylate, 2% of alkylphenol ethoxylate sodium sulfate, 1% of sodium alkyl naphthalene sulfonate, 20% of sodium sulfate, 10% of corn starch, and the balance of filler.
22. A method for producing the herbicidal composition as claimed in any one of claims 1 to 21, comprising:
Uniformly mixing the chlorpyrifos, the propanil, the picloram, the dispersing agent, the wetting agent, the disintegrating agent and the filler according to a proportion, crushing the mixture to the particle size D 98 between 15 and 25 mu m through a jet mill, uniformly mixing the mixture to prepare a dry material, adding water into the dry material, extruding and granulating the dry material, adding water accounting for 10 to 25 weight percent of the dry material, and drying the dry material at the temperature of 40 to 50 ℃ to prepare the water dispersible granule containing the propanil, the chlorpyrifos and the picloram.
23. The method according to claim 22, wherein the pulverizing pressure of the jet mill is 0.5 to 0.8mpa.
24. The method according to claim 22, wherein the pulverizing pressure of the jet mill is 0.7Mpa.
25. Use of a herbicidal composition according to any one of claims 1 to 21 or a herbicidal composition prepared by a method according to any one of claims 22 to 24 for controlling crop injury in farmland.
26. The use according to claim 25, wherein the plant weed comprises grassy weeds and/or broadleaf weeds.
27. The use according to claim 25, wherein the grass weeds comprise one or more of barnyard grass, cyperus alternifolius, euphorbia lathyris, green bristlegrass, crabgrass and goosegrass.
28. The use according to claim 25, wherein the broadleaf weeds comprise one or more of cress, glossoside, euonymus alatus, purslane, amaranth, knotweed, and quinoa.
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