CN113383780B - Weeding preparation and application thereof - Google Patents
Weeding preparation and application thereof Download PDFInfo
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- CN113383780B CN113383780B CN202010165330.1A CN202010165330A CN113383780B CN 113383780 B CN113383780 B CN 113383780B CN 202010165330 A CN202010165330 A CN 202010165330A CN 113383780 B CN113383780 B CN 113383780B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
Abstract
The invention belongs to the field of herbicides, and relates to an ethyl 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridine-2-yl) -N-methylbenzenesulfonamide) acetate herbicide and a use method thereof. The active component is a compound with the structure shown in the specification, and the active component is mixed with at least one carrier and at least one surfactant to prepare powder, wettable powder, granules, water dispersible granules, emulsifiable powder (granules), effervescent granules, effervescent tablets, micro-capsules, slow-release granules or medical fertilizers. In any case, the choice of formulation type depends on the physical, chemical and biological properties of the active ingredient. The preparation variety of the invention can prevent and remove broadleaf weeds, grassy weeds and nutgrass flatsedge in paddy fields more efficiently.
Description
Technical Field
The invention belongs to the technical field of agricultural herbicides, and relates to a herbicide composition for paddy fields, in particular to a 2- (2-chloro-5- (3-chloro-5-trifluoromethyl pyridine-2-yl) -N-methylbenzenesulfonamide) ethyl acetate herbicide preparation and a use method thereof.
Background
Rice is a large important grain crop, and the planting area is wide. The novel weeding compound ethyl 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridin-2-yl) -N-methylbenzenesulfonamide) (patent numbers: CN 102464611A and CN 103003240A, WO 2012059050A 1) developed by Shenyang neutralization pesticide chemical industry research and development limited company has extremely high weeding activity, can effectively control weeds such as barnyard grass, piemarker, snakehead intestines, green bristlegrass, zinnia, cocklebur, long-rain flower, glossoside, arrowhead and the like, and indoor and field pesticide effect results show that the compound can have application prospect as a novel herbicide. However, the use of herbicides at the present stage is generally two ways, one way is: firstly, the active ingredients are dissolved by an organic solvent (such as acetone) (the content of the acetone in the total solution is not more than 10 percent), then, a solution with the required concentration is prepared by using a 0.1 percent Tween 80 aqueous solution as a spraying liquid for use, and the method has great defects: the preparation must be carried out at present, the application is troublesome, the pollution to the environment is large, and the cost is high. Alternatively, the active ingredient may be formulated according to methods well known in the pesticide arts, which, although making up for the deficiencies of the first method, generally does not perform as well as the effect of the active ingredient is not as good as the biological activity of the first method. The pesticide is a special chemical with extremely strong biological activity, and different active components have very large differences in structure, active groups, physicochemical properties, action modes and action targets, and the biological activity plays a role and has very large relation with an auxiliary agent system matched with the pesticide. That is, the biological activity of the herbicide active ingredient is generally responsible for the undesirable effects. The main problems of the herbicide industry at present are how to select an auxiliary agent system suitable for the effective components, control the dynamic surface tension of sprayed liquid medicine and the particle size of fog drops, so that the liquid medicine has small drift, slow evaporation, good spreading, wetting and adhesion on a target and long residence time, thereby improving the utilization rate of pesticides and simultaneously reducing the phytotoxicity problem caused by drift.
Disclosure of Invention
The invention aims to develop a weeding preparation taking ethyl 2- (2-chloro-5- (3-chloro-5-trifluoromethyl pyridine-2-yl) -N-methylbenzenesulfonamide) acetate as an active component and a using method thereof.
In order to achieve the above purpose, the invention adopts the technical scheme that:
a weeding preparation comprises the following active components:
the preparation is powder, wettable powder, granules, water dispersible granules, emulsifiable powder (granules), effervescent granules, effervescent tablets, microcapsule granules, slow release granules or medical fertilizers.
The preparation is wettable powder, water dispersible granules, slow release granules or emulsifiable powder (granule).
The active component is combined with at least one carrier and at least one surfactant; wherein the weight percentage of the active components is 0.1-99%.
The herbicidal formulations according to the invention can be prepared by customary processes, i.e. by mixing the active substances with liquid solvents and/or solid carriers, adding one or more surfactants, such as emulsifiers, dispersants, stabilizers, wetting agents, and also adding binders or defoamers. In each case, a uniform distribution of the active components of the compositions according to the invention should be ensured.
The water dispersible granule is prepared by mixing raw materials, a surfactant and a carrier, and crushing, kneading and granulating. The granules are generally prepared into granules of 10 to 100 international standard mesh (1.676 to 0.152 mm) and can be prepared by extrusion, dipping or spray granulation methods. Typically containing 20 to 90% active ingredient and 5 to 20% surfactant such as stabilizers, wetting dispersants, disintegrants and binders, and inert carrier balance.
The wettable powder is prepared by mixing raw materials, a surfactant and a carrier and crushing. Typically, it contains 10 to 85% active ingredient, 3 to 15% dispersant, and the balance of solid inert carrier.
The emulsifiable powder (or granule) is prepared by mixing active components, organic solvent and surfactant together to form a uniform transparent oil phase, then uniformly spraying the oil phase on a pre-crushed carrier, wherein the active components are usually 5-30%, the surfactant is 10-40%, the organic solvent is 5-15%, and the rest is the carrier.
The slow release granule is prepared by mixing and pulverizing active components, surfactant and carrier, and coating with adhesive. Usually, the effective component is 0.5-10%, the surfactant is 2-10%, and the rest is carrier.
Effervescent granules (or tablets) are prepared by mixing and crushing active components, surfactant and carrier, and then kneading and granulating (or tabletting). Usually, the effective component is 0.5-30%, the surfactant is 2-15%, and the rest is carrier.
The granule is prepared by mixing active components and carrier together, drying, and coating. The effective component is usually 0.1-10%, and the rest is carrier.
The powder is prepared by mixing the active components and the carrier together, and pulverizing. The effective component is usually 0.1-10%, and the rest is carrier.
The medicine fertilizer is prepared by mixing active components, surfactant and carrier together, drying and coating. Usually, the effective component is 0.1-10%, the surfactant is 0.5-3%, and the rest is carrier.
Preferably, in the wettable powder, the active component is 10-85%, the surface activity is 3-15%, and the rest is carrier; in the water dispersible granule, the active component is 20-90%, the surfactant is 5-20%, and the carrier is the rest; in the emulsifiable powder (or granule), the active component is 5-30%, the surfactant is 10-40%, the solvent is 5-15%, and the rest is carrier; in the slow release granule, the active component is 0.5-10%, the surfactant is 2-10%, and the rest is carrier.
The surfactant of the wettable powder is one or more of wetting agent Morwet EFW, dispersing agent Supragil MNS/90, alkyl naphthalene sulfonic acid polycondensate sodium salt, alkyl naphthalene sulfonate formaldehyde condensate, sodium dodecyl sulfate, polycarboxylate dispersing agent GY-D02, sodium methylene naphthalene sulfonate, sodium lignin sulfonate, wetting agent TENSIOFIX BCZ, dispersing agent SK-24R, wetting agent Rhodasurf 860/p, dispersing agent Morwet D-400, dispersing agent YUS-WP1, wetting agent YUS-A51G, dispersing agent SD819, dispersing agent SK-12WP, dispersing agent SK-20TX, dispersing agent YUS-WP2, wetting agent YUS-NV1203, TANEMUL DA2883, dispersing agent SP-2836, dispersing agent YUS-FS7PG and wetting agent YUS-LXC; preferably wetting agent Morwet EFW, dispersant Supragil MNS/90, alkyl naphthalene sulfonic acid polycondensate sodium salt, alkyl naphthalene sulfonate formaldehyde condensate, sodium dodecyl sulfate, polycarboxylate dispersant GY-D02, sodium methylene naphthalene sulfonate, sodium lignin sulfonate, wetting agent TENSIOFIX BCZ, dispersant SK-24, wetting agent Rhodasurf 860/p, dispersant Morwet D-400, wetting agent YUS-A51G; the carrier comprises: white carbon black, diatomite, kaolin, attapulgite and light calcium carbonate.
The surfactant of the water dispersible granule is one or a mixture of a plurality of dispersing agents YUS-WG4, sodium salt of alkyl naphthalene sulfonic acid polycondensate, dispersing agent SK-20TX, soluble starch, dispersing agent YUS-WG5, wetting agent TENSIOFIX BCZ, dispersing agent SP2836, dispersing agent Supragil MNS/90, wetting agent YUS-SXC, dispersing agent soprofor FD, dispersing agent PICO-WG7, wetting agent PICO-NW1, wetting agent PICO-NW2, calcium lignosulfonate, alkyl naphthalene sulfonate formaldehyde condensate (NNO), dispersing agent YUS-FS7PG, dispersing agent YUS-FS1, dispersing agent PICO-JK, preferably dispersing agent YUS-WG4, sodium salt of alkyl naphthalene sulfonic acid polycondensate, dispersing agent SK-20TX, dispersing agent YUS-WG5, wetting agent TENSIOFIX BCZ, dispersing agent SP2836, dispersing agent soprogil MNS/90, alkyl naphthalene sulfonate formaldehyde condensate, wetting agent YUS-SXC and sopor dispersing agent sopor; and (3) a carrier: one or more of diatomite, kaolin and attapulgite are mixed.
The surfactant of the emulsifiable powder (granule) is emulsifier 1601, emulsifier OX-2681, emulsifier OX-8686, emulsifier 0201B, emulsifier 700#, emulsifier SK-33H, emulsifier 500#, emulsifier YUS-110, emulsifier YUS-135B, emulsifier SK-5026ECH, emulsifier SK-5208T and the like; solvent: n-methylpyrrolidone, 10 parts of solvent oil S-150, armid DM10, rhodiasolv Green SV-92, rhodiasolv Green SV-33 and Rhodiasolv Green 25. Preferably, emulsifier 1601, emulsifier OX-2681, emulsifier OX-8686, emulsifier 700#, emulsifier SK-33H, and emulsifier 500#; and (3) a carrier: one or more of attapulgite, activated clay, kaolin and kaolin are mixed.
The surfactant of the slow release granule is one or more of calcium lignosulfonate, dispersant alkyl naphthalene sulfonate polycondensate sodium salt, methyl naphthalene sulfonate sodium formaldehyde condensate, wetting agent TENSIOFIX BCZ, polyvinyl alcohol, ethylene oxide propylene oxide block copolymer, diphenylmethane-4`4-diisocyanate, ethylenediamine, chitosan and carboxymethyl starch sodium. Preferably calcium lignosulfonate, dispersant alkyl naphthalene sulfonic acid polycondensate sodium salt, methyl naphthalene sulfonic acid sodium formaldehyde condensate, wetting agent TENSIOFIX BCZ and polyvinyl alcohol; the carrier is one or more of white carbon black, attapulgite, kaolin and bentonite.
The formulation of the finished formulation of the composition of the present invention may employ (liquid or solid) carriers and various adjuvants well known to those skilled in the art. Examples include, but are not limited to, the following types of substances.
The surfactant contained in the herbicidal formulation composition of the present invention may be an emulsifier, a dispersant or a wetting agent; may be nonionic or ionic. The anionic surfactant comprises sulfonates, sulfates, carboxylates, phosphates, succinates, lignosulfonates, acrylamide acrylic acid copolymers and the like, and the nonionic surfactant comprises fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ether, acid alcohol ester and polyoxyethylene ether thereof, fatty amide and polyoxyethylene ether thereof, alkanolamide and polyoxyethylene ether thereof, polyoxyethylene polyoxypropylene ether block copolymer, sodium alkyl naphthalene sulfonate fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether and the like. For example: wetting agent Morwet EFW, dispersant Supragil MNS/90, dispersant alkyl naphthalene sulfonic acid polycondensate sodium salt, alkyl naphthalene sulfonate formaldehyde condensate (NNO), sodium dodecyl sulfate, polycarboxylate dispersant GY-D02, sodium methylene naphthalene sulfonate, sodium lignin sulfonate, wetting agent TENSIOFIX BCZ, dispersant SK-24R, wetting agent Rhodasurf 860/p, dispersant Morwet D-400, dispersant YUS-WP1, emulsifier YUS-110, emulsifier YUS-135B, wetting agent YUS-A51G, dispersant SD819, dispersant SK-12WP, dispersant SK-20TX, dispersant YUS-WP2, wetting agent YUS-NV1203, TANEMUL DA2883, dispersant SP-2836, dispersant YUS-FS7PG, dispersant YUS-WG4, dispersant YUS-WP sodium salt of alkyl naphthalene sulfonic acid polycondensate, dispersant YUS-WG5, wetting agent YUS-SXC, dispersant Soprophor FD, dispersant PICO-WG7, wetting agent PICO-NW1, wetting agent PICO-NW2, calcium lignosulfonate, dispersant YUS-FS1, dispersant PICO-JK, emulsifier 1601, emulsifier SK-5208T, emulsifier OX-2681, emulsifier OX-8686, emulsifier 0201B, emulsifier 700#, emulsifier-33H, emulsifier 500#, emulsifier SK-5026ECH, sodium methyl naphthalene sulfonate formaldehyde condensate, dodecanol-1, tetradecanol-1, sorbitol, sucrose or fatty acid esters of pentaerythritol and their block copolymers with ethylene oxide propylene oxide, sodium salt of sulfonated castor oil, polyoxyethylene (n) 20 ) Styrene (Phenylethylene)Alkylphenol ether oleate, alkylaryl polyoxyethylene polyoxypropylene ether, alkylaryl formaldehyde resin polyoxyethylene ether, calcium isothiokoxide oleate, emulsifier 2201, emulsifier # 600, alkylaryl phenyl ether (YUS-SC 3), calcium isothiokoxide oleate, polycarboxylate dispersant GY-D800, polycarboxylate dispersant GY-D04, sodium naphthalene sulfonate formaldehyde condensate, sodium naphthol sulfonate formaldehyde condensate, castor oil ethylene oxide adduct, alkylphenol polyoxyethylene polyoxypropylene ether, methyl naphthalene sulfonate formaldehyde condensate, alkyl-glycol ether-sodium sulfonate, N-methyl-oleoyl-sodium taurate, detergent LS, sodium methylaminoethyl oleate, darlinger D909S, alkylaryl polyoxyethylene ether, dodecyl polyoxyethylene ether phosphate, polyarylphenol polyoxyethylene ether para-tertiary butyl ether, piperonyl butoxide, ethylene oxide-propylene oxide block copolymer alkylphenol ethoxylate formaldehyde condensate, sodium N-methyl-fatty acyl-taurate, alkylphenol ethoxylate formaldehyde condensate, sodium dibutylnaphthalene sulfonate (nekal BX), dibutylnaphthalene sulfonate formaldehyde condensate, alkylphenol ethoxylate formaldehyde condensate sulfate, alkylphenol polyoxyethylene phosphate, dispersant YUS-5050PB, dispersant YUS-NV1420, dispersant YUS-CH7000, dispersant PICO-CS300M, dispersant Geropon Ultrasperse, dispersant Geropon Extra, dispersant Geropon DA1349, dispersant TENSIOFIX LX SPECIAL, dispersant TENSIOFIX DB08, dispersant Tensiofix AMS303, dispersant Tensiofix XA265, dispersant Tensiofix 96DB10, dispersant SK-92FS1, dispersant SK-541, dispersant YUS-2010 CX, SP-4302 (moisturizing synergist), dispersant VE/10, dispersant OE/02, dispersant OE/03, dispersant OE/08, dispersant OE/09, dispersant OE150, dispersant Emulson CO40, dispersant Emulson AG/1100, emulsifier Emulson AG/18C, dispersant Soprophor TSP/461, dispersant Soprophor 796/P, dispersant Morwet D-360, dispersant Morwet D-390, dispersant Geronol ODessa 01, dispersant Geronol ODessa 05, YUS-D935, octylphenol polyoxyethylene ether sulfate, wetting agent Igepal BC/10, wetting agent GEOPONL-WET/P, wetting agent Supragil WP, wetting agent Supragil GN, wetting agent YUS-LXC, wetting agent SK-551, sodium isopropylnaphthalene sulfonate, sodium alkyl alcohol polyoxyethylene ether sulfate, alkyl alcohol polyoxyethylene ether sulfateAlkylphenol ethoxylate formaldehyde condensate sulfate, alkyl succinic sulfonate, sodium laureth sulfonate, sodium dodecyl benzene sulfonate, calcium dodecyl benzene sulfonate, alkylamidyl taurate, and the like.
The carrier contained in the herbicidal formulation composition of the present invention, any carrier commonly used for herbicide compounds can be used.
Suitable solvents include petroleum fractions, cyclohexane, light mineral oil, ethylene glycol methyl ether, propylene glycol, glycerol, sorbitol, benzyl alcohol, acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, N-methyl-pyrrolidone, tributyl phosphate, methyl oleate, dimethylformamide, N, dimethylsunflower amide, dimethyl sulfoxide, armid DM10, armid FMPC, rhodiasolv Green SV-92, rhodiasolv Green SV-33, rhodiasol Green 25, solvent oil S-150, solvent oil S-200, and the like; also vegetable oils and methyl soluble fibers. Mixtures of different liquids are often suitable.
Suitable solid carriers include natural or synthetic, for example: clay, rock powder, chalk, quartz, clay, montmorillonite, sodium sulfate, silica, diatomaceous earth, pumice, gypsum, talc, bentonite, kaolin, attapulgite, light calcium carbonate, china clay, montmorillonite, aluminum magnesium silicate, activated clay, white carbon, ammonium sulfate, urea, monoammonium phosphate, potassium chloride, ammonium chloride, benzofuran resins, perphosphate, alumina, calcite, marble, pumice, and the like, suitable particulate carriers include crushed and fractionated natural rocks such as sepiolite and dolomite and synthetic particulates made from organic and inorganic powders.
Suitable binders may be synthetic (e.g. carbomethyl alcohol, polyvinyl acetate) or natural water-soluble polymers (e.g. xanthan gum, gelatin, gum arabic, polyvinylpyrrolidone, magnesium aluminum silicate, polyethylene glycol, phenolic resins, shellac, methylcellulose, soluble starch, sodium carboxymethyl starch, carboxymethyl cellulose, sodium alginate, etc.), added to the formulation in powder, granular or latex form.
Suitable preservatives are: EQ, kathon, sodium benzoate, etc.
Suitable defoamers are bufadienolide, defoamers SAG1522, WJX-1, silicone, C 8～10 Fatty alcohols, phosphates, C 10～20 Saturated fatty acids (e.g., capric acid) and amides, and the like.
Effervescent disintegrants: the acidic component is an organic acid, an inorganic acid, for example: tartaric acid, citric acid, salicylic acid, phosphoric acid, and the like; the alkaline component is a basic carbonate, for example: sodium bicarbonate, sodium carbonate, urea, potassium bicarbonate, potassium carbonate, ammonium bicarbonate, and the like.
The wall material is as follows: natural polymeric materials such as: gelatin, acacia, agar, alginate, chitosan, fibrin, zein, etc.; semi-synthetic polymeric materials, for example: methyl (ethyl) cellulose, carboxymethyl cellulose (sodium), cellulose acetate, esters and partial glycerides thereof, and the like; total synthetic polymeric materials, for example: polyacrylic resin, polylactic acid, melamine resin, urea resin, polyamide, polyester, polymethyl methacrylate, polyurea, polyurethane, diphenylmethane-4`4-diisocyanate, ethylene diamine, and the like.
The herbicidal composition of the present invention may be diluted by the user or sprayed directly with water before use, or may be used directly.
The technical scheme of the invention also comprises the application of the weeding preparation: the herbicide composition is used for preventing and removing broadleaf weeds, grassy weeds and sedge after transplanting rice paddy seedlings and seedling reviving or after direct seeding rice paddy seedlings emerge.
The invention has the advantages that:
according to the biological activity specificity of the pesticide, the invention uses theoretical knowledge as guidance, selects an auxiliary agent system suitable for the active components by researching the structure active groups and the action mode of the active components, achieves the purposes of controlling the dynamic surface tension of the sprayed liquid medicine and the particle size of fog drops, leading the liquid medicine to drift little, evaporating slowly, spreading on a target, wetting and attaching well and having long retention time, thereby improving the utilization rate of the pesticide and solving the problem of poor drug effect of the pesticide prepared according to the common processing method. The auxiliary agent system can assist the active components to be rapidly, uniformly and stably dispersed in a spray carrier, has small particle size, narrow distribution and proper surface tension of the pesticide liquid, further ensures the distribution and adhesion of the pesticide liquid on the surface of organisms, promotes the absorption of the pesticide by the organisms, even increases the transmission of the pesticide in the organisms, achieves the purposes of increasing the retention quantity of the pesticide on the plant surface, prolonging the retention time and improving the penetration capability of the pesticide on the plant epidermis, further improves the efficacy of the obtained herbicide active component, reduces the dosage, reduces the cost, hits the target to the greatest extent with the minimum dosage, improves the compatibility with the environment, and reduces the harm of the pesticide to human bodies and the pollution to the environment.
Detailed Description
The following specific examples are given to illustrate the present invention in further detail, but the present invention is by no means limited to these examples, and methods well known to those skilled in the art are intended to be included within the scope of the present invention.
According to the invention, according to the action target and the application mode, theoretical knowledge is used as guidance, and an experimental result is combined to find an auxiliary agent variety matched with the effective components, so that the problems are better solved, the biological activity is improved, the dosage is reduced, the cost is reduced, the target is hit to the maximum extent with the least dosage, and the compatibility with the environment is improved; the preparation is a preparation variety containing 2- (2-chloro-5- (3-chloro-5-trifluoromethyl pyridine-2-yl) -N-methylbenzenesulfonamide) ethyl acetate as an active component (hereinafter simply referred to as a compound A), the dynamic surface tension of the liquid medicine is proper, the particle size of the fog drops is large, the evaporation is slow, the fog drops spread on a target, the wetting and the adhesion are good, and the retention time is long, so that the aims of greatly improving the wetting, the drifting, the bouncing, the spreading, the dispersing, the retention and the permeability of the active component on a growing medium are fulfilled, and the practical effects are that: increase the retention of the effective components of the pesticide on the plant surface, prolong the retention time and improve the penetration capability of the effective components of the pesticide on the plant surface, thereby improving the biological activity of the pesticide and reducing the dosage.
The percentages and parts in the formulations of the examples below are by weight. The active component of 2- (2-chloro-5- (3-chloro-5-trifluoromethyl-pyridin-2-yl) -N-methylbenzenesulfonamide) ethyl acetate (hereinafter referred to as compound A) is prepared (content is 98%), and is added in a dosage after folding, and other raw materials are all commercial products.
Example 1, formulation of 75% Compound A wettable powder
According to the formula requirement, 75 parts of compound A, 1.5 parts of Morwet EFW, 4 parts of Supragil MNS/90, 4 parts of alkyl naphthalene sulfonic acid polycondensate sodium salt, 3 parts of alkyl naphthalene sulfonate formaldehyde condensate, 5 parts of white carbon black and diatomite are fully mixed until the concentration reaches 100%, and the mixture is crushed by a superfine crusher to obtain 75% wettable powder of compound A. Physical property index measurement results: active component content, 75.2%; fineness (passing through a 45 μm standard sieve) of 99.5%; the suspension rate is 92.9%; wetting time, 30s; heat storage (54±2 ℃/14 d): content, 74.5%, fineness (passing through 45 μm standard sieve) 98.1%; suspension rate, 90.5%; wetting time, 35s.
EXAMPLE 2 preparation of 35% Compound A wettable powder
According to the formula requirement, 35 parts of compound A, 2 parts of sodium dodecyl sulfate, 4 parts of SUPRAGIL MNS/90, 3 parts of polycarboxylate dispersant GY-D02, 4 parts of sodium methylenenaphthalene sulfonate, 4 parts of sodium lignin sulfonate, 5 parts of white carbon black and diatomite are fully mixed to be complemented to 100%, and the mixture is crushed by a superfine crusher to obtain 35% compound A wettable powder. Physical property index measurement results: active component content, 35.1%; fineness (passing through a 45 μm standard sieve) of 99.8%; suspension rate, 95.3%; wetting time, 15s; heat storage (54±2 ℃/14 d): active component content, 34.6%; fineness (passing through a 45 μm standard sieve) of 99.1%; the suspension rate is 92.5%; wetting time, 15s.
EXAMPLE 3 preparation of 60% Compound A wettable powder
According to the formula requirement, 60 parts of compound A, 2 parts of wetting agent TENSIOFIX BCZ, 4 parts of dispersing agent SK-24, 5 parts of polycarboxylate dispersing agent GY-D02, 5 parts of white carbon black and diatomite are fully mixed until the content is 100%, and the mixture is crushed by a superfine crusher to obtain the 60% compound A wettable powder. Physical property index measurement results: active component content, 60.3%; fineness (passing through 45 μm standard sieve) 99.7%; suspension rate, 93.1%; wetting time, 20s; heat storage (54±2 ℃/14 d): active component content, 59.5%; fineness (passing through 45 μm standard sieve) 98.2%; suspension rate, 91.1%; wetting time, 20s.
EXAMPLE 4 preparation of 50% Compound A wettable powder
According to the formula requirement, 50 parts of compound A, 2 parts of wetting agent Rhodasurf 860/p, 4 parts of dispersing agent Morwet D-400, 4 parts of dispersing agent YUS-WP1, 5 parts of white carbon black and diatomite are fully mixed to 100%, and the mixture is crushed by a superfine crusher to obtain 50% compound A wettable powder. Physical property index measurement results: active component content, 50.1%; fineness (passing through a 45 μm standard sieve) of 99.1%; suspension rate, 95.8%; wetting time, 25s; heat storage (54±2 ℃/14 d): the content of active components is 48.9%; fineness (passing through a 45 μm standard sieve) 98.3%; the suspension rate is 92.3%; wetting time, 28s.
EXAMPLE 5 preparation of 60% Compound A wettable powder
According to the formula requirement, 60 parts of compound A, 1.5 parts of wetting agent YUS-A51G, 4 parts of dispersing agent SD819, 3 parts of Supragil MNS/90, 3 parts of polycarboxylate dispersing agent GY-D02, 5 parts of white carbon black and diatomite are fully mixed until the content is 100%, and the mixture is crushed by a superfine crusher to obtain the 60% compound A wettable powder. Physical property index measurement results: active component content, 60.5%; fineness (passing through 45 μm standard sieve) 99.2%; suspension rate, 93.6%; wetting time, 22s; heat storage (54±2 ℃/14 d): active component content, 59.1%; fineness (passing through 45 μm standard sieve) 98.1%; suspension rate, 90.9%; wetting time, 25s.
Example 6 preparation of 40% Compound A Water dispersible granule
According to the formula requirement, 40 parts of compound A, 1 part of wetting agent TENSIOFIX BCZ, 4 parts of dispersing agent YUS-WG4, 4 parts of sodium salt of alkyl naphthalene sulfonic acid polycondensate, 3 parts of dispersing agent SK-20TX, 10 parts of soluble starch, 10 parts of sodium sulfate and bentonite are added together to complement 100%, mixed and crushed, and then added into a granulator with a screen of a certain specification for granulation after being kneaded by adding water. And then drying and screening (according to the screen range) to obtain the 40% compound A water dispersible granule. Physical property index measurement results: the content of the active component is 40.1 percent; suspension rate, 96.2%; wetting time, 8s; dispersibility, 96.2%; wear resistance, 95%; heat storage (54±2 ℃/14 d): active component content, 39.1%; the dispersibility is 95.3%; suspension rate, 94.8%; wetting time, 10s; wear resistance, 93%.
Example 7 preparation of 60% Compound A Water dispersible granule
According to the formula requirement, 60 parts of compound A, 1 part of wetting agent TENSIOFIX BCZ, 4 parts of dispersing agent YUS-WG5, 4 parts of alkyl naphthalene sulfonate formaldehyde condensate, 10 parts of soluble starch, 6 parts of sodium sulfate and bentonite are added together to complement 100%, mixed and crushed, and then added into a granulator with a screen of a certain specification for granulation after being kneaded by adding water. And then drying and screening (according to the screen range) to obtain the 60% compound A water dispersible granule. Physical property index measurement results: the content of the active component is 60.2%; suspension rate, 97.1%; wetting time, 9s; dispersibility, 97.5%; abrasion resistance, 96%; heat storage (54±2 ℃/14 d): active component content, 58.9%; the dispersibility was 96.1%; suspension rate, 95.6%; wetting time, 12s; wear resistance, 94%.
Example 8 preparation of 85% Compound A Water dispersible granule
According to the formula requirement, 85 parts of compound A, 1 part of wetting agent TENSIOFIX BCZ, 4 parts of dispersing agent YUS-WG5, 4 parts of dispersing agent SP2836, 2 parts of soluble starch and bentonite are added together to complement 100%, mixed and crushed, then water is added for kneading, and the mixture is added into a granulator with a screen of a certain specification for granulation. And then drying and screening (according to the screen range) to obtain the 85% compound A water dispersible granule. Physical property index measurement results: the content of active components is 85.1%; suspension rate, 95.8%; wetting time, 10s; dispersibility, 95.1%; wear resistance, 93%; heat storage (54±2 ℃/14 d): the active component content is 84.1%; the dispersibility is 93.8%; suspension rate, 93.5%; wetting time, 13s; wear resistance, 92%.
Example 9 preparation of 55% Compound A Water dispersible granule
According to the formula requirement, 55 parts of compound A, 2 parts of wetting agent TENSIOFIX BCZ, 4 parts of dispersant Supragil MNS/90, 4 parts of alkyl naphthalene sulfonate formaldehyde condensate, 5 parts of soluble starch and bentonite are complemented to 100 percent and added together, mixed and crushed, and then added into a granulator with a screen mesh of certain specification for granulation after being kneaded by adding water. And then drying and screening (according to the screen range) to obtain 55% compound A water dispersible granule. Physical property index measurement results: the content of the active component is 55.5%; suspension rate, 97.2%; wetting time, 9s; dispersibility of 98.1%; abrasion resistance, 96%; heat storage (54±2 ℃/14 d): active component content, 55.1%; the dispersibility was 96.9%; suspension rate, 96.3%; wetting time, 11s; abrasion resistance, 95%.
Example 10 preparation of 40% Compound A Water dispersible granule
According to the formula requirement, 40 parts of compound A, 1 part of wetting agent YUS-SXC, 4 parts of dispersing agent Soprophor FD, 4 parts of dispersing agent YUS-WG5, 2 parts of alkyl naphthalene sulfonate formaldehyde condensate, 5 parts of soluble starch, 6 parts of sodium sulfate and bentonite are added together to complement to 100%, mixed and crushed, and then added into a granulator with a screen of a certain specification for granulation after being kneaded by adding water. And then drying and screening (according to the screen range) to obtain the 40% compound A water dispersible granule. Physical property index measurement results: the content of the active component is 40.3 percent; suspension rate, 97.1%; wetting time, 8s; dispersibility, 95.2%; abrasion resistance, 96%; heat storage (54±2 ℃/14 d): active component content, 39.8%; the dispersibility was 94.6%; suspension rate, 96.3%; wetting time, 12s; abrasion resistance, 95%.
EXAMPLE 11 preparation of 10% emulsifiable powder of Compound A
According to the formula requirement, 10 parts of compound A, 1.5 parts of emulsifier 1601, 6 parts of emulsifier 2201, 5 parts of emulsifier 0201B, 2 parts of N-methyl pyrrolidone and 10 parts of solvent oil S-150 are added into a mixing kettle, stirred and mixed uniformly, heated and dissolved by a hot water bath when necessary, and the oil base is sprayed uniformly onto a mixture which is formed by 20 parts of white carbon black and attapulgite and is complemented to 100% under the stirring condition, and the mixture is crushed by a superfine crusher, so that 10% of emulsifiable powder of compound A is obtained. Physical property index measurement results: active component content, 10.3%; wetting time, 15s; persistent foamability (1 min), 20mL, dispersion stability (2 h, oil slick) and no oil slick.
EXAMPLE 12 preparation of 15% emulsifiable powder of Compound A
According to the formula requirement, 15% of compound A, 1.5 parts of emulsifier 1601, 3 parts of emulsifier OX-8686, 8 parts of emulsifier 2201, 5 parts of emulsifier 0201B, 10 parts of N-methylpyrrolidone and 10 parts of dimethylbenzene are added into a mixing kettle, uniformly stirred and mixed, heated and dissolved by a hot water bath when necessary, and under the stirring condition, the oil base is uniformly sprayed onto a mixture which is formed by 20 parts of white carbon black and attapulgite and is complemented to 100%, and the mixture is crushed by a superfine crusher, so that 15% of emulsifiable powder of compound A is obtained. Physical property index measurement results: active component content, 15.2%; wetting time, 10s; long-lasting foamability (1 min), 15mL, dispersion stability (2 h, oil slick) and no oil slick.
Example 13 preparation of 5% emulsifiable granules of Compound A
According to the formula requirement, adding 5 parts of a compound A, 1 part of an emulsifying agent 1601, 3.5 parts of an emulsifying agent OX-2681, 4 parts of an emulsifying agent 0201B, 2 parts of an emulsifying agent 700#, 10 parts of N-methylpyrrolidone and 10 parts of dimethylbenzene into a mixing kettle, stirring and uniformly mixing, heating and dissolving by using a hot water bath when necessary, uniformly spraying the oil base onto a mixture which is formed by 25 parts of white carbon black and attapulgite and is complemented to 100% under the stirring condition, crushing by a superfine crusher, adding water and kneading, and adding into a granulator with a screen mesh with a certain specification for granulating. And then drying and screening (according to the screen range) to obtain the 5% compound A emulsifiable granules. Physical property index measurement results: active component content, 5.05%; wetting time, 15s; persistent foamability (1 min), 20mL, dispersion stability (2 h, oil slick) and no oil slick.
EXAMPLE 14 preparation of 10% emulsifiable granules of Compound A
According to the formula requirement, 10 parts of compound A, 4 parts of emulsifier 33H, 3 parts of emulsifier 500#, 4 parts of emulsifier 0201B, 1 part of emulsifier 700#, and 10 parts of solvent oil S-150 are added into a mixing kettle, uniformly stirred and mixed, heated and dissolved by a hot water bath when necessary, and uniformly sprayed onto a mixture which is formed by 25 parts of white carbon black and attapulgite and is complemented to 100% under the stirring condition, crushed by a superfine crusher, kneaded by adding water, and added into a granulator with a screen mesh with certain specification for granulation. And then drying and screening (according to the screen range) to obtain 10% of compound A emulsifiable granules. Physical property index measurement results: active component content, 10.3%; wetting time, 10s; persistent foamability (1 min), 15mL; dispersion stability (2 h, oil slick) with no oil slick.
Example 15 formulation of 5% Compound A tablet
According to the formula requirement, 5 parts of compound A, 2 parts of SK-24R, 1 part of sodium dodecyl sulfate, 4 parts of Supragil MNS/90, 20 parts of soluble starch, 10 parts of sodium sulfate, 5 parts of white carbon black and diatomite are fully mixed until reaching 100 percent, and after being crushed by a superfine crusher, the mixture is tabletted, thus obtaining 5 percent compound A tablets. Physical property index measurement results: active component content, 5.03%; disintegration time, 2.5min; suspension rate, 93.5%; persistent foamability (1 min), 10mL.
EXAMPLE 16 formulation of 5% Compound A sustained release pellet
According to the formula requirement, 5 parts of compound A, 2 parts of calcium lignosulfonate, 2 parts of dispersant alkyl naphthalene sulfonic acid polycondensate sodium salt, 3 parts of methyl naphthalene sulfonic acid sodium formaldehyde condensate, 1 part of wetting agent TENSIOFIX BCZ, 5 parts of white carbon black, 5 parts of carboxymethyl starch sodium, 1 part of 1% chitosan water-soluble and bentonite which are complemented to 100% are added together, mixed and crushed, then kneaded by adding water, and then added into a granulator with a screen with a certain specification for granulation. Then drying and screening (according to the screen range), then coating by 1 part of 1% chitosan water solution, and airing to obtain 5% compound A slow release granules. Physical property index measurement results: active component content, 4.98%; moisture, 2.8%; the falling rate is 1.1 percent.
EXAMPLE 17 formulation of 5% Compound A granules
According to the formula requirement, 5 parts of compound A, 3 parts of dispersant methyl naphthalene sulfonate sodium formaldehyde condensate, 2 parts of SK-24, 4 parts of dispersant Supragil MNS/90, 10 parts of sodium sulfate and bentonite are added together to complement 100%, mixed and crushed, and then added into a granulator with a screen of a certain specification for granulation after being kneaded by adding water. And then drying and screening (according to the screen range) to obtain 5% compound A granules. Physical property index measurement results: active component content, 5.06%; moisture, 2.1%; the falling rate is 0.9 percent.
EXAMPLE 18 preparation of 20% Compound A effervescent granules
According to the formula requirement, 20 parts of compound A, 4 parts of sodium salt of alkyl naphthalene sulfonic acid polycondensate, 2 parts of methyl naphthalene sulfonic acid sodium formaldehyde condensate, 1 part of wetting agent YUS-A51G, 20 parts of soluble starch, 15 parts of citric acid, 15 parts of sodium bicarbonate, 10 parts of sodium sulfate and diatomite are fully mixed to be 100%, crushed by a superfine crusher, and then kneaded and granulated to obtain 20% compound A effervescent granules. Physical property index measurement results: active component content, 20.2%; suspension rate, 95.2%; wetting time, 15s; disintegration time, 1.2min; persistent foamability (1 min), 8mL.
EXAMPLE 19 formulation of 2% Compound A granules
According to the formula requirement, firstly adding 2 parts of compound A, 3 parts of N-methyl pyrrolidone and 6 parts of solvent oil S-150 into a mixing kettle for dissolution, fully mixing with silica sand to be complemented by 100%, airing, then coating by using 1 part of 1% chitosan water solution, airing, and obtaining 2% compound A granules. Physical property index measurement results: active component content, 2.02%; moisture, 1.9%; the falling rate is 0.6 percent.
EXAMPLE 20 preparation of 40% Compound A microcapsules
Into 1000 ml plastic (with baffle) bottle, adding 600 ml 0.5% polyvinyl alcohol aqueous solution, using tetrafluoroethylene stirrer, adding 20 parts of compound A, 9 g ethylene oxide propylene oxide block copolymer, 6 g epoxidized soybean oil, 3 g diphenylmethane-4`4-diisocyanate, 1.5 g ethylene diamine, 5 g sodium carbonate and 150 ml water under high speed stirring, after the addition, slowing down the speed to continue stirring for 1 hour, standing for 1 hour, filtering, vacuum drying, and obtaining 40% compound A microcapsule. Physical property index measurement results: active component content, 40.3%; encapsulation efficiency of 90.1%.
Example 21 preparation of 0.5% Compound A fertilizer
According to the formula requirement, 0.5 part of compound A, 0.1 part of polyvinyl alcohol and urea are added together to be complemented to 100, and then the mixture is uniformly mixed in a closed blending kettle, granulated by a coating method and naturally dried, thus obtaining the 0.5% compound A medical fertilizer. Physical property index measurement results: active component content, 0.51%; moisture, 2.0%; the falling rate is 0.3 percent.
Comparative example 1, preparation of 60% Compound A wettable powder
According to the formula requirement, 60 parts of compound A, 2 parts of sodium dodecyl sulfate, 4 parts of calcium lignosulfonate, 4 parts of alkyl naphthalene sulfonate formaldehyde condensate (NNO), 5 parts of white carbon black and light calcium carbonate are fully mixed to be complemented to 100%, and the mixture is crushed by a superfine crusher to obtain the 60% compound A wettable powder. Physical property index measurement results: content, 60.5%; fineness (passing through 45 μm standard sieve) 98.2%; suspension rate, 83.1%; wetting time, 25s; after heat storage (54.+ -. 2 ℃ C./14 d): content, 59.6%; fineness (passing through 45 μm standard sieve) 85.2%; suspension rate, 65.1%; wetting time, 75s.
Preparation of comparative example 2, 40% Compound A Water dispersible granule
According to the formula requirement, 40 parts of compound A, 2 parts of sodium dodecyl sulfate, 4 parts of sodium lignin sulfonate, 2 parts of urea, 5 parts of soluble starch, 6 parts of sodium sulfate and bentonite are added together to complement 100%, mixed and crushed, and then added into a granulator with a screen mesh with certain specification for granulation after being kneaded by adding water. And then drying and screening (according to the screen range) to obtain the 40% compound A water dispersible granule. Physical property index measurement results: the content is 40.6 percent; suspension rate, 90.2%; wetting time, 25s; dispersibility, 83.7%; wear resistance, 92%; after heat storage (54.+ -. 2 ℃ C./14 d): the content is 39.5%; suspension rate, 62.9%; wetting time, 80s; dispersibility, 63.5%.
Biological Activity test examples
Sowing quantitative barnyard grass and snakehead intestine seeds into 9cm high disposable paper cup, covering with 0.5cm soil, flattening, sprinkling water, culturing in a greenhouse according to conventional method, spraying soil (spraying pressure 1.95 kg/cm) on crawler-type crop sprayer (UK Engineer Research Ltd.) at test dosage for 24 hr 2 The spraying amount is 500L/ha, and the crawler speed is 1.48 km/h). The test was repeated 3 times. The test materials are treated and then are placed in a greenhouse for management according to a conventional method. The response of the weeds to the agents was observed and recorded, and the control effect of the agents on weeds was examined by visual inspection on a regular basis (see table below). Obtaining a linear regression equation and ED of each medicament on weeds to be tested by using DPS2000 data processing system 90 The value, the herbicidal activity of the test agent was evaluated.
Visual ED of different dosage forms for barnyard grass and snakehead intestines 90 Value (21 days after treatment)
From the data, the preparation varieties developed by the invention have proper dynamic surface tension and proper fog drop particle size, so that the liquid medicine spreads, wets and adheres well on a target, the detention time is long, the liquid medicine drift is small, and the evaporation is slow, thereby promoting the rapid conduction of active ingredients and improving the biological activity of the active ingredients, and the preparation has obvious synergistic effect. The preparation prepared by the invention not only improves the biological activity, reduces the dosage, reduces the cost, hits the target to the maximum extent with the least dosage, but also improves the compatibility with the environment.
Claims (2)
1. A herbicidal formulation characterized in that: the active component is a compound A, wherein the compound A is 2- (2-chloro-5- (3-chloro-5-trifluoromethyl pyridine-2-yl) -N-methylbenzenesulfonamide) ethyl acetate, and the structural formula is as follows:
the specific weeding preparation comprises the following components:
35% wettable powder of compound a: 35 parts of compound A, 2 parts of sodium dodecyl sulfate, 4 parts of SUPRAGILMNS/90, 3 parts of polycarboxylate dispersant GY-D02, 4 parts of sodium methylenenaphthalene sulfonate, 4 parts of sodium lignin sulfonate, 5 parts of white carbon black and diatomite to 100 percent;
or, 60% compound a wettable powder: 60 parts of compound A, 1.5 parts of wetting agent YUS-A51G, 4 parts of dispersing agent SD819, 3 parts of Supragil MNS/90, 3 parts of polycarboxylate dispersing agent GY-D02, 5 parts of white carbon black and diatomite to 100%;
or, 40% of compound a water dispersible granule: 40 parts of compound A, 1 part of wetting agent YUS-SXC, 4 parts of dispersant Soprophor FD, 4 parts of dispersant YUS-WG5, 2 parts of alkyl naphthalene sulfonate formaldehyde condensate, 5 parts of soluble starch, 6 parts of sodium sulfate and bentonite, and the balance is up to 100%.
2. A herbicidal formulation as claimed in claim 1 for controlling broadleaf weeds in transplanted paddy fields or grassy weeds in direct seeding paddy fields after seedling transplanting and seedling reviving.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464611B (en) * | 2010-11-03 | 2014-01-01 | 中国中化股份有限公司 | Substitutional biaryl base benzene sulfonamide compound and application |
| CN105707076A (en) * | 2014-12-05 | 2016-06-29 | 沈阳中化农药化工研发有限公司 | Herbicidal composition and applications thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102464611B (en) * | 2010-11-03 | 2014-01-01 | 中国中化股份有限公司 | Substitutional biaryl base benzene sulfonamide compound and application |
| CN105707076A (en) * | 2014-12-05 | 2016-06-29 | 沈阳中化农药化工研发有限公司 | Herbicidal composition and applications thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《Synthesis and evaluation of substituted 3-(pyridin-2-yl)benzenesulfonamide derivatives as potent herbicidal agents》;YongXie;《Bioorganic & Medicinal Chemistry》;20160201;第429页化合物2h * |
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