CN113383780A

CN113383780A - Weeding preparation and application thereof

Info

Publication number: CN113383780A
Application number: CN202010165330.1A
Authority: CN
Inventors: 丑靖宇; 张国生; 关爱莹; 刘长令
Original assignee: Jiangsu Yangnong Chemical Co Ltd; Shenyang Sinochem Agrochemicals R&D Co Ltd
Current assignee: Jiangsu Yangnong Chemical Co Ltd; Shenyang Sinochem Agrochemicals R&D Co Ltd
Priority date: 2020-03-11
Filing date: 2020-03-11
Publication date: 2021-09-14
Anticipated expiration: 2040-03-11
Also published as: CN113383780B

Abstract

The invention belongs to the field of herbicides, and relates to a 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridine-2-yl) -N-methylbenzenesulfonamide) ethyl acetate herbicide preparation and a using method thereof. The active component is a compound with the structure shown as the following, and the active component is mixed with at least one carrier and at least one surfactant to be prepared into powder, wettable powder, granules, water dispersible granules, emulsifiable powder (granules), effervescent granules, effervescent tablets, micro-capsule granules, slow-release granules or medicinal fertilizers. In any case, the choice of the type of formulation depends on the physical, chemical and biological characteristics of the active ingredient. The preparation of the invention can effectively prevent and kill broadleaf weeds, gramineous weeds and nutgrass flatsedge in paddy fields.

Description

Weeding preparation and application thereof

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-trifluoromethylpyridine-2-yl) -N-methylbenzenesulfonamide) ethyl acetate herbicide preparation and a use method thereof.

Background

Rice is an important grain crop, and the planting area of the rice is wide. A new herbicidal compound 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridin-2-yl) -N-methylbenzenesulfonamide) ethyl acetate (patent number: CN 102464611A, CN 103003240A, WO 2012059050A 1) developed by Shenyang chemical pesticide chemical research and development Limited company has extremely high herbicidal activity, can effectively control weeds such as cockspur grass, piemarker, eclipta, green bristlegrass, zinnia elegans, cocklebur, monochoria sinensis, monochoria vaginalis and arrowhead in paddy fields, and has application prospect as a new herbicide as shown by indoor and field efficacy results. However, at the present time, herbicides are generally used in two ways, one of which is: firstly, the effective components are dissolved by an organic solvent (such as acetone) (the content of the acetone in the total solution is not more than 10 percent), and then 0.1 percent of Tween 80 aqueous solution is prepared into a solution with the required concentration to be used as a spraying solution, and the method has the following defects: must be prepared at present, is relatively troublesome to apply, has large environmental pollution and high cost. Alternatively, the active ingredient may be formulated according to methods well known in the pesticide art which, while compensating for the deficiencies of the first mode, generally do not exert the desired effect and are not as biologically active as the first mode. The pesticide is a special chemical with extremely strong biological activity, the structure, active groups, physicochemical properties, action modes and action targets of different active components are greatly different, and the effect exerted by the biological activity is greatly related to the selection of an auxiliary agent system matched with the biological activity. That is, often the reason why the biological activity of the herbicide active ingredient is not desirable. The main problem in the herbicide industry at present is how to select an auxiliary agent system suitable for active ingredients, control the dynamic surface tension and the droplet particle size of the sprayed liquid medicine well, ensure that the liquid medicine has small drift, slow evaporation, good spreading, wetting and attachment on a target and long retention time, thereby improving the utilization rate of the pesticide and simultaneously reducing the problem of phytotoxicity caused by drift.

Disclosure of Invention

The invention aims to develop a weeding preparation taking 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridine-2-yl) -N-methylbenzenesulfonamide) ethyl acetate as an active component and a using method thereof.

In order to achieve the purpose, the invention adopts the technical scheme that:

a weeding preparation, wherein the active components in the weeding preparation are compounds with the following structures:

the preparation is powder, wettable powder, granules, water dispersible granules, emulsifiable powder (granules), effervescent granules, effervescent tablets, micro-capsule granules, slow release granules or medicinal fertilizers.

The preparation is wettable powder, water dispersible granules, sustained-release granules or emulsifiable powder (granules).

The active ingredient is mixed with at least one carrier and at least one surfactant; wherein, the weight percentage of the active components is 0.1 to 99 percent.

The herbicidal formulations of the present invention can be prepared by conventional processes, i.e. by mixing the active substance with a liquid solvent and/or a solid carrier, adding one or more surfactants, such as emulsifiers, dispersants, stabilizers, wetting agents, and optionally binders or defoamers. In each case, a homogeneous distribution of the active ingredients of the compositions according to the invention should be ensured.

The water dispersible granule is prepared by mixing the original drug, the surfactant and the carrier, and crushing, kneading and granulating the mixture. The granules are usually prepared into granules with 10-100 international standard meshes (1.676-0.152 mm), and can be prepared by extrusion, dipping or spray granulation. Generally, the active component is 20-90%, the surfactant such as stabilizer, wetting dispersant, disintegrant and adhesive is 5-20%, and the rest is inert carrier.

The wettable powder is prepared by mixing the original medicine, the surfactant and the carrier and crushing. The active component is 10-85%, the dispersant is 3-15%, and the balance is solid inert carrier.

The emulsifiable powder (or particle) agent is prepared by mixing active components, an organic solvent and a surfactant together to form a uniform transparent oil phase, and then uniformly spraying the uniform transparent oil phase on a pre-crushed carrier, wherein the active components are 5-30%, the surfactant is 10-40%, the organic solvent is 5-15%, and the balance is the carrier.

The sustained-release granule is prepared by mixing and pulverizing active ingredient, surfactant and carrier, and coating with binder. Generally, the active ingredient is 0.5-10%, the surfactant is 2-10%, and the balance is carrier.

The effervescent granules (or tablets) are prepared by mixing and crushing active ingredients, surfactants and carriers, and then kneading and granulating (or tabletting). Generally, the active ingredient is 0.5-30%, the surfactant is 2-15%, and the balance is carrier.

The granule is prepared by mixing active ingredients and carrier, drying, and coating. Usually 0.1-10% of active ingredient and the balance of carrier.

The powder is prepared by mixing active ingredients and carrier, and pulverizing. Usually 0.1-10% of active ingredient and the balance of carrier.

The fertilizer is prepared by mixing active components, surfactant and carrier, drying, and coating. Usually, the active ingredient is 0.1-10%, the surfactant is 0.5-3%, and the balance is carrier.

Preferably, in the wettable powder, the active component accounts for 10-85%, the surface activity accounts for 3-15%, and the balance is carrier; in the water dispersible granule, 20-90% of active component, 5-20% of surfactant and the balance of carrier; in the emulsifiable powder (or granule) agent, 5-30% of active component, 10-40% of surfactant, 5-15% of solvent and the rest is carrier; in the sustained-release granules, 0.5-10% of active component, 2-10% of surfactant and the balance of carrier.

The surfactant of the wettable powder is one or a mixture of a wetting agent Morwet EFW, a dispersant Supergil MNS/90, an alkyl naphthalene sulfonic acid polycondensate sodium salt, an alkyl naphthalene sulfonate formaldehyde condensate, sodium dodecyl sulfate, a polycarboxylate dispersant GY-D02, methylene naphthalene sodium sulfonate, sodium lignosulfonate, a wetting agent TENSIOFIX BCZ, a dispersant SK-24R, a wetting agent Rhodasurf 860/p, a dispersant Morwet D-400, a dispersant YUS-WP1, a wetting agent YUS-A51G, a dispersant SD819, a dispersant SK-12WP, a dispersant SK-20TX, a dispersant YUS-WP2, a wetting agent YUS-NV1203, TANEMULL DA2883, a dispersant SP-2836, a dispersant YUS-FS7PG and a wetting agent YUS-LXC; preferably wetting agent Morwet EFW, dispersant Supergil MNS/90, alkyl naphthalene sulfonic acid polycondensate sodium salt, alkyl naphthalene sulfonate formaldehyde condensate, sodium dodecyl sulfate, polycarboxylate dispersant GY-D02, methylene naphthalene sodium sulfonate, sodium lignosulfonate, wetting agent TENSIOFIX BCZ, dispersant SK-24, wetting agent Rhodasurf 860/p, dispersant Morwet D-400, wetting agent YUS-A51G; the carrier comprises: one or more of white carbon black, diatomite, kaolin, attapulgite and light calcium carbonate.

The surfactant of the water dispersible granule is one or a mixture of more than one of dispersant YUS-WG4, sodium salt of alkyl naphthalene sulfonate polycondensate, dispersant SK-20TX, soluble starch, dispersant YUS-WG5, wetting agent TENSILOFIX BCZ, dispersant SP2836, dispersant Supergil MNS/90, wetting agent YUS-SXC, dispersant Soprophor FD, dispersant PICO-WG7, wetting agent PICO-NW1, wetting agent PICO-NW2, calcium lignosulfonate, alkyl naphthalene sulfonate formaldehyde condensate (NNO), dispersant YUS-FS7PG, dispersant YUS-FS1 and dispersant PICO-JK, preferably dispersant YUS-WG4, sodium salt of alkyl naphthalene sulfonate polycondensate, dispersant SK-20TX, dispersant YUS-WG5, wetting agent TENSILIX BCZ, dispersant SP2836, dispersant Supergil MNS/90, alkyl naphthalene sulfonate formaldehyde condensate, Wetting agent YUS-SXC, dispersant Soprophor FD; carrier: one or more of diatomite, kaolin and attapulgite.

The surfactant of the emulsifiable powder (particle) agent 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-methyl pyrrolidone, 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 #; carrier: one or more of attapulgite, activated clay, kaolin and kaolin.

The surfactant of the sustained-release granules is one or a mixture of more of calcium lignosulfonate, alkyl naphthalene sulfonic acid polycondensate sodium salt serving as a dispersing agent, a sodium methyl naphthalene sulfonate formaldehyde condensate, a wetting agent TENSIOFIX BCZ, polyvinyl alcohol, an ethylene oxide propylene oxide block copolymer, diphenylmethane-4' 4-diisocyanate, ethylenediamine, chitosan and sodium carboxymethyl starch. Preferably calcium lignosulfonate, alkyl naphthalene sulfonic acid polycondensate sodium salt serving as a dispersant, a sodium methyl naphthalene sulfonate formaldehyde condensate, a wetting agent TENSIOFIX BCZ and polyvinyl alcohol; the carrier is one or a mixture of more of white carbon black, attapulgite, kaolin and bentonite.

The compositions of the invention may be formulated in finished formulations using (liquid or solid) carriers and various adjuvants well known to those skilled in the art. Examples include, but are not limited to, the following classes of materials.

The surfactant contained in the herbicidal formulation composition of the present invention may be an emulsifier, a dispersant or a wetting agent; may be non-ionic 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 ethoxylates, 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 Supergil MNS/90, dispersant alkyl naphthalene sulfonic acid polycondensate sodium salt, alkyl naphthalene sulfonate formaldehyde condensate (NNO), sodium dodecyl sulfate, polycarboxylate dispersant GY-D02, methylene naphthalene sodium 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-12WP20TX, dispersant YUS-WP2, wetting agent YUS-NV1203, TANEMULL DA2883, dispersant SP-2836, dispersant YUS-FS7PG, dispersant YUS-WG4, 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 methylnaphthalenesulfonate formaldehyde condensate, dodecanol-1, tetradecanol-1, sorbitol, sucrose or pentaerythritol, fatty acid esters of sucrose or pentaerythritol, and block copolymers thereof with ethylene oxide and propylene oxide, Sodium salt of sulfonated castor oil, polyoxyethylene (n)₂₀) Phenethyl phenol ether oleate, alkylaryl polyoxyethylene polyoxypropylene ether, alkylaryl formaldehyde resin polyoxyethylene ether, calcium isothionate oleate, emulsifier 2201, emulsifier 600#, alkylaryl phenyl ether (YUS-SC3), calcium isothionate 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-diethylene glycol ether-sodium sulfonate, N-methyl-oleoyl-taurate, detergent LS, methyl aminoethyl sulfonate oleate, dispersant D909S, alkylaryl polyoxyethylene ether, dodecyl polyoxyethylene ether phosphate, polyarylphenol polyoxyethylene ether, polyoxyethylene ether phosphate, sodium N-methyl-oleyl-taurate, sodium oleate, polyoxyethylene glycol ether, polyoxyethylene ether phosphate, polyoxyethylene ether, sodium oleate, sodium lauryl ether, sodium oleate, sodium stearate, P-tert-butyl ether, piperonyl butoxide, an ethylene oxide-propylene oxide block copolymer alkylphenol polyoxyethylene ether formaldehyde condensate, sodium N-methyl-fatty acyl-taurate, an alkylphenol polyoxyethylene ether formaldehyde condensate, sodium dibutylnaphthalenesulfonate (nekal BX), a dibutylnaphthalenesulfonate formaldehyde condensate, an alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, an alkylphenol polyoxyethylene phosphate, a dispersant YUS-5050PB, a dispersant YUS-1420 NV, a dispersant YUS-CH7000, a dispersant PICO-CS300M, a dispersant Geropon Ultrasperse, a dispersant Geropon Extra, a dispersant Geropon DA1349, a dispersant TENSILOX AMS LX SPECIAL, a dispersant TENSILOX DB08, a dispersant Tensiofix 303. Tensiofix XA265, Tensiofix 96DB10, SK-92FS1, SK-541, YUS-2010 CX, SP-4302 (moisturizing synergist), VE/10, OE/02, OE/03, OE/08, OE/09, OE150, Emulson CO40, Emulson AG/1100, Emulson AG/18C, Soprophor TSP/461, Soprophor 796/P, Morwet D-360, Morwet D-390, Geronol ODessa 01, Geronol ODessa 05, YUS-D935, octylphenol polyoxyethylene ether sulfate, Igepal ROPONL/10, LXPOL-WET/P, Super WP, humectant RAGIL, YNGN-C, humectant, Wetting agent SK-551, sodium isopropyl naphthalene sulfonate, sodium alkyl alcohol polyoxyethylene ether sulfate, alkyl phenol polyoxyethylene ether formaldehyde condensate sulfate, alkyl succinic acid sulfonate, sodium lauryl alcohol polyoxyethylene ether sulfonate, sodium dodecyl benzene sulfonate, calcium dodecyl benzene sulfonate, alkylamido taurate, etc.

The carrier included in the herbicidal formulation composition of the present invention, and any carrier generally used for herbicidal compounds can be used.

Suitable solvents include petroleum distillates, 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, dimethyl pelargonamide, dimethyl sulfoxide, Armid DM10, Armid FMPC, Rhodiasolv Green SV-92, Rhodiasolv Green SV-33, Rhodiasolv Green 25, mineral spirits S-150, mineral spirits S-200, and the like; also vegetable oils and methyl cellulose. Mixtures of different liquids are often suitable.

Suitable solid supports include natural or synthetic, for example: clays, rock powders, chalk, quartz, clays, montmorillonite, sodium sulfate, silica, diatomaceous earth, pumice, gypsum, talc, bentonite, kaolin, attapulgite, precipitated calcium carbonate, china clay, montmorillonite, magnesium aluminum silicate, activated clay, white carbon black, ammonium sulfate, urea, monoammonium phosphate, potassium chloride, ammonium chloride, coumarone resins, perphosphates, alumina, calcite, marble, pumice, and the like, suitable particulate carriers include crushed and fractionated natural rocks such as sepiolite and dolomite and synthetic particles made from organic and inorganic powders.

Suitable binders may be synthetic (e.g. carboxymethyl alcohol, polyvinyl acetate) or natural water soluble polymers (e.g. xanthan gum, gelatin, gum arabic, polyvinyl pyrrolidone, magnesium aluminum silicate, polyethylene glycol, phenolic resins, shellac, methyl cellulose, soluble starch, sodium carboxymethyl starch, carboxymethyl cellulose and sodium alginate, etc.) added to the formulation in powder, granule or latex form.

Suitable preservatives are: EQ, cason, sodium benzoate, and the like.

Suitable antifoams are antifoams, SAG1522, WJX-1, silicones, C_8～10Fatty alcohol, phosphoric acid esters, C_10～20Saturated fatty acids (such as capric acid) and amides, etc.

Effervescent disintegrant: the acidic component is an organic acid, an inorganic acid, for example: tartaric acid, citric acid, salicylic acid, phosphoric acid, and the like; basic components are basic carbonates, such as: sodium bicarbonate, sodium carbonate, urea, potassium bicarbonate, potassium carbonate, ammonium bicarbonate, and the like.

The wall material is as follows: natural high molecular materials, for example: gelatin, acacia, agar, alginate, chitosan, fibrin, zein, etc.; semi-synthetic polymeric materials, for example: cellulose acetate, esters thereof, partial glycerides, etc.; fully synthetic polymeric materials, such as: polyacrylic acid resins, polylactic acid, melamine resins, urea resins, polyamides, polyesters, polymethyl methacrylate, polyureas, polyurethanes, diphenylmethane-4' 4-diisocyanate, ethylene diamine, and the like.

The herbicidal composition of the present invention may be diluted by the user or sprayed with water directly 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 killing broadleaf weeds, gramineous weeds and nutgrass flatsedge after transplanting seedlings and delaying seedlings in a transplanted paddy field or after emergence of seedlings in a direct-seeding paddy field.

The invention has the advantages that:

according to the invention, according to the particularity of the biological activity of the pesticide per se and under the guidance of theoretical knowledge, an auxiliary agent system suitable for the active components is selected by researching the active groups and the action modes of the structures of the active components, so that the purposes of controlling the dynamic surface tension of the sprayed liquid medicine, controlling the particle size of fog drops, ensuring that the liquid medicine has small drift, slow evaporation, good spreading, wetting and adhesion on a target and long retention time are achieved, the utilization rate of the pesticide is improved, and the problem of poor pesticide effect of the pesticide prepared by a common processing method is solved. The auxiliary agent system can assist the active components to be quickly, uniformly and stably dispersed in the spray carrier, the active components have small particle size and narrow distribution, and the surface tension of the liquid medicine is proper, so that the distribution and the attachment of pesticide liquid medicine on the surface of an organism are ensured, the absorption of the organism to the agent is promoted, even the conductance of the agent in the organism is increased, and the purposes of increasing the retention of the pesticide on the surface of a plant, prolonging the retention time and improving the penetrating power on the epidermis of the plant are achieved, so that the efficacy of the active ingredients of the herbicide obtained by the invention is fully improved, the dosage is reduced, the cost is reduced, the target is hit to the maximum extent with the minimum dosage, the compatibility with the environment is improved, and the harm of the pesticide to a human body and the pollution to the environment are reduced.

Detailed Description

The following specific examples are intended to illustrate the invention in further detail, but the invention is by no means limited to these examples, and methods known to those skilled in the art are intended to be included within the scope of the invention.

According to the invention, theoretical knowledge is taken as guidance according to the action target and the application mode, and the experimental result is combined to search for the auxiliary variety matched with the active ingredients, so that the problems are well solved, the bioactivity is improved, the dosage is reduced, the cost is reduced, the target is hit to the maximum extent with the minimum dosage, and the compatibility with the environment is improved; the preparation is a preparation variety containing 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridine-2-yl) -N-methylbenzenesulfonamide) ethyl acetate (hereinafter referred to as a compound A) as an active component, and the dynamic surface tension of the liquid medicine is appropriate, the particle size of fog drops is large, the evaporation is slow, the liquid medicine is spread, wetted and attached on a target and the retention time is long, so that the purposes of greatly improving the wetting, drifting, bouncing, spreading, dispersing, retaining and permeating performances of the effective components on a growing medium are achieved, and the actual effects are as follows: the retention amount of the effective components of the pesticide on the surface of the plant is increased, the retention time is prolonged, the penetration capacity to the surface skin of the plant is improved, the biological activity of the pesticide is improved, and the using dosage is reduced.

The percentages and parts in the formulations of the examples described below are by weight. The active component ethyl 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridine-2-yl) -N-methylbenzenesulfonamide) acetate (hereinafter referred to as compound A) is self-prepared (with the content of 98 percent) and added after the dosage of hundreds, and other raw materials are all commercial products.

EXAMPLE 1 preparation 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 sodium alkyl naphthalene sulfonate polycondensate, 3 parts of alkyl naphthalene sulfonate formaldehyde condensate, 5 parts of white carbon black and diatomite are fully mixed until the mixture is 100 percent, and the mixture is crushed by an ultrafine crusher to obtain 75 percent compound A wettable powder. Physical property index measurement results: active ingredient content, 75.2%; fineness (passing through 45 μm standard sieve) 99.5%; suspension rate, 92.9%; wetting time, 30 s; heat storage (54. + -. 2 ℃/14 d): content, 74.5%, fineness (passing through 45 μm standard sieve) 98.1%; suspension rate, 90.5%; wetting time, 35 s.

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 methylene naphthalene sulfonate, 4 parts of sodium lignosulfonate, 5 parts of white carbon black and diatomite are fully mixed until the mixture is 100 percent, and the mixture is crushed by a superfine crusher to obtain 35 percent compound A wettable powder. Physical property index measurement results: active ingredient content, 35.1%; fineness (passing through 45 μm standard sieve) 99.8%; suspension percentage, 95.3%; wetting time, 15 s; heat storage (54. + -. 2 ℃/14 d): active ingredient content, 34.6%; fineness (passing through 45 μm standard sieve) 99.1%; suspension rate, 92.5%; wetting time, 15 s.

Example 3 preparation of 60% Compound A wettable powder

According to the formula requirement, 60 parts of compound A, 2 parts of wetting agent TENSILOFIX 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 mixture is 100 percent, and the mixture is crushed by an ultrafine crusher to obtain 60 percent compound A wettable powder. Physical property index measurement results: active component content, 60.3%; fineness (passing through 45 μm standard sieve) 99.7%; suspension ratio, 93.1%; wetting time, 20 s; heat storage (54. + -. 2 ℃/14 d): active component content, 59.5%; fineness (passing through a 45 μm standard sieve) 98.2%; suspension rate, 91.1%; wetting time, 20 s.

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 until the mixture is 100 percent, and the mixture is crushed by a superfine crusher to obtain 50 percent compound A wettable powder. Physical property index measurement results: active component content, 50.1%; fineness (passing through 45 μm standard sieve) 99.1%; suspension percentage, 95.8%; wetting time, 25 s; heat storage (54. + -. 2 ℃/14 d): active component content, 48.9%; fineness (passing through a 45 μm standard sieve) 98.3%; suspension percentage, 92.3%; wetting time, 28 s.

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 mixture is 100 percent, and the mixture is crushed by an ultrafine crusher to obtain 60 percent 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, 22 s; heat storage (54. + -. 2 ℃/14 d): active component content, 59.1%; fineness (passing through a 45 μm standard sieve) 98.1%; suspension percentage, 90.9%; wetting time, 25 s.

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 TENSILOFIX 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 until the total content is 100%, mixed and crushed, and then added with water for kneading, and then added into a granulator with a screen of a certain specification for granulation. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 40% compound A water dispersible granule. Physical property index measurement results: the content of active components is 40.1 percent; suspension rate, 96.2%; wetting time, 8 s; dispersibility, 96.2%; abrasion resistance, 95%; heat storage (54. + -. 2 ℃/14 d): active ingredient content, 39.1%; the dispersity is 95.3%; suspension percentage, 94.8%; wetting time, 10 s; abrasion 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 TENSILOFIX 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 until the total content is 100%, mixed and crushed, and then added into a granulator with a screen with a certain specification for granulation after being kneaded by adding water. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 60% compound A water dispersible granule. Physical property index measurement results: the content of active components is 60.2 percent; suspension rate, 97.1%; wetting time, 9 s; dispersibility, 97.5%; abrasion resistance, 96%; heat storage (54. + -. 2 ℃/14 d): active component content, 58.9%; the dispersity is 96.1%; suspension percentage, 95.6%; wetting time, 12 s; abrasion resistance, 94%.

Example 8 preparation of 85% Compound A Water dispersible granules

According to the formula requirement, 85 parts of compound A, 1 part of wetting agent TENSILOFIX BCZ, 4 parts of dispersing agent YUS-WG5, 4 parts of dispersing agent SP2836, 2 parts of soluble starch and bentonite are added together until the content is 100%, mixed and crushed, and then added into a granulator with a certain specification of sieve for granulation after being kneaded by adding water. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 85% compound A water dispersible granule. Physical property index measurement results: the content of active components is 85.1 percent; suspension percentage, 95.8%; wetting time, 10 s; dispersibility, 95.1%; abrasion resistance, 93%; heat storage (54. + -. 2 ℃/14 d): active ingredient content, 84.1%; the dispersity is 93.8%; suspension rate, 93.5%; wetting time, 13 s; abrasion 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 TENSILOFIX BCZ, 4 parts of dispersant Supergil MNS/90, 4 parts of alkyl naphthalene sulfonate formaldehyde condensate, 5 parts of soluble starch and bentonite are added together until the total content is 100%, mixed and crushed, and then added into a granulator with a screen mesh with a certain specification for granulation after being kneaded by adding water. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 55% compound A water dispersible granule. Physical property index measurement results: the content of active components is 55.5 percent; suspension rate, 97.2%; wetting time, 9 s; dispersibility, 98.1%; abrasion resistance, 96%; heat storage (54. + -. 2 ℃/14 d): active component content, 55.1%; the dispersity is 96.9%; suspension rate, 96.3%; wetting time, 11 s; 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 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 are added together until the mixture is up to 100 percent, mixed and crushed, added with water and kneaded, and then added into a granulator with a screen of a certain specification for granulation. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 40% compound A water dispersible granule. Physical property index measurement results: the content of active components is 40.3 percent; suspension rate, 97.1%; wetting time, 8 s; dispersibility, 95.2%; abrasion resistance, 96%; heat storage (54. + -. 2 ℃/14 d): active ingredient content, 39.8%; the dispersity is 94.6%; suspension rate, 96.3%; wetting time, 12 s; abrasion resistance, 95%.

EXAMPLE 1110% formulation of Compound A emulsifiable powder

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-methylpyrrolidone and 10 parts of solvent oil S-150 are added into a mixing kettle, stirred and mixed uniformly, heated and dissolved by using a hot water bath if necessary, the oil base is uniformly sprayed on a mixture consisting of 20 parts of white carbon black and attapulgite until the mixture is 100 percent under the stirring condition, and the mixture is crushed by a superfine crusher to obtain the compound A emulsifiable powder with the concentration of 10 percent. Physical property index measurement results: active component content, 10.3%; wetting time, 15 s; persistent foaming (1min), 20mL, dispersion stability (2h, oil slick), no oil slick on.

EXAMPLE 12 preparation of 15% Compound A emulsifiable powder

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, stirred and mixed uniformly, heated and dissolved by a hot water bath if necessary, the oil base is uniformly sprayed on a mixture consisting of 20 parts of white carbon black and attapulgite which are complemented to 100% under the stirring condition, and the mixture is crushed by a superfine crusher to obtain 15% of compound A emulsifiable powder. Physical property index measurement results: active component content, 15.2%; wetting time, 10 s; persistent foaming (1min), 15mL, dispersion stability (2h, oil slick), no oil slick on.

Example 13 preparation of 5% Compound A emulsifiable granules

According to the formula requirement, 5 parts of compound A, 1 part of emulsifier 1601, 3.5 parts of emulsifier OX-2681, 4 parts of emulsifier 0201B, 2 parts of emulsifier 700#, 10 parts of N-methyl pyrrolidone and 10 parts of xylene are added into a mixing kettle, stirred and mixed uniformly, heated and dissolved by a hot water bath if necessary, the oil base is uniformly sprayed on a mixture consisting of 25 parts of white carbon black and attapulgite which are complemented to 100 percent under the stirring condition, crushed by an ultrafine crusher, kneaded by adding water, and added into a granulator provided with a screen mesh with a certain specification for granulation. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 5% compound A emulsifiable granules. Physical property index measurement results: 5.05 percent of active component; wetting time, 15 s; persistent foaming (1min), 20mL, dispersion stability (2h, oil slick), no oil slick on.

EXAMPLE 1410% formulation of Compound A emulsifiable granules

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, stirred and mixed uniformly, heated and dissolved by using a hot water bath if necessary, the oil base is uniformly sprayed on a mixture consisting of 25 parts of white carbon black and attapulgite which are complemented to 100% under the stirring condition, crushed by an ultrafine crusher, kneaded by adding water, and then added into a granulator with a sieve of a certain specification for granulation. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the compound A emulsifiable granules with 10 percent. Physical property index measurement results: active component content, 10.3%; wetting time, 10 s; permanent foaming (1min), 15 mL; dispersion stability (2h, oil slick) and no oil slick on.

EXAMPLE 155% formulation of Compound A tablets

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 the mixture is 100 percent, and the mixture is crushed by a superfine crusher and then tableted to obtain the 5 percent compound A tablet. Physical property index measurement results: 5.03 percent of active component; disintegration time, 2.5 min; suspension rate, 93.5%; permanent foaming (1min), 10 mL.

EXAMPLE 165% formulation of Compound A extended Release pellets

According to the formula requirements, 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 TENSILOXIX BCZ, 5 parts of white carbon black, 5 parts of sodium carboxymethyl starch, 1 part of 1% chitosan water-soluble, and bentonite are added together until the total content is 100%, mixed and crushed, and then added into a granulator provided with a screen mesh with a certain specification for granulation after being kneaded by adding water. Then drying and screening (according to the range of a screen), then coating by using 1 part of 1% chitosan water solution, and airing to obtain the 5% compound A sustained-release granules. Physical property index measurement results: active component content, 4.98%; 2.8 percent of water; the shedding rate was 1.1%.

EXAMPLE 175 formulation of Compound A granules

According to the formula requirement, 5 parts of compound A, 3 parts of a dispersant sodium methyl naphthalene sulfonate formaldehyde condensate, 2 parts of SK-24, 4 parts of a dispersant Supragil MNS/90, 10 parts of sodium sulfate and bentonite are added together until the mixture is 100 percent, mixed and crushed, added with water and kneaded, and then added into a granulator with a screen of a certain specification for granulation. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 5% compound A granules. Physical property index measurement results: 5.06 percent of active component; 2.1 percent of water; the shedding rate was 0.9%.

EXAMPLE 1820% formulation of 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 until the mixture is 100 percent, and the mixture is crushed by an ultrafine crusher and then kneaded and granulated to obtain 20 percent of compound A effervescent granules. Physical property index measurement results: active component content, 20.2%; suspension percentage, 95.2%; wetting time, 15 s; disintegration time, 1.2 min; permanent foaming (1min), 8 mL.

EXAMPLE 192% formulation of Compound A granules

According to the formula requirement, 2 parts of compound A, 3 parts of N-methyl pyrrolidone and 6 parts of solvent oil S-150 are added into a mixing kettle to be dissolved, are fully mixed with silica sand until the silica sand is 100 percent, are dried, are coated by dissolving 1 part of 1 percent chitosan in water, and are dried to obtain 2 percent compound A granules. Physical property index measurement results: active component content, 2.02%; moisture, 1.9%; the shedding rate was 0.6%.

EXAMPLE 2040% formulation of Compound A microencapsulated granules

Adding 600 ml of 0.5% polyvinyl alcohol aqueous solution into a 1000 ml plastic bottle (with a baffle), adding 20 parts of compound A, 9 g of ethylene oxide propylene oxide block copolymer, 6 g of epoxidized soybean oil, 3 g of diphenylmethane-4' 4-diisocyanate, 1.5 g of ethylene diamine, 5 g of sodium carbonate and 150 ml of water under high-speed stirring by using a tetrafluoroethylene stirrer, after the addition is finished, continuing stirring at a slow speed for 1 hour, standing for 1 hour, filtering, and drying in vacuum to obtain the 40% compound A microcapsule granule. Physical property index measurement results: active component content, 40.3%; encapsulation efficiency, 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 complemented to 100 parts and added together, the mixture is uniformly mixed in a closed blending kettle, and the mixture is granulated by a coating method and naturally aired to obtain the 0.5% compound A medical fertilizer. Physical property index measurement results: active component content, 0.51%; 2.0% of water; the shedding rate was 0.3%.

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 until the mixture is 100 percent, and the mixture is crushed by an ultrafine crusher to obtain 60 percent compound A wettable powder. Physical property index measurement results: content, 60.5%; fineness (passing through a 45 μm standard sieve) 98.2%; suspension percentage, 83.1%; wetting time, 25 s; after heat storage (54. + -. 2 ℃/14 d): content, 59.6%; fineness (passing through 45 μm standard sieve) 85.2%; suspension percentage, 65.1%; wetting time, 75 s.

Comparative example 2, preparation of 40% Compound A Water dispersible granule

According to the formula requirements, 40 parts of compound A, 2 parts of sodium dodecyl sulfate, 4 parts of sodium lignosulfonate, 2 parts of urea, 5 parts of soluble starch, 6 parts of sodium sulfate and bentonite are added together until the total amount is 100%, mixed and crushed, added into a granulator with a screen of a certain specification after being kneaded by adding water, and granulated. Then drying and screening (according to the range of a screen) are carried out, thus obtaining the 40% compound A water dispersible granule. Physical property index measurement results: the content is 40.6%; suspension rate, 90.2%; wetting time, 25 s; dispersibility, 83.7%; abrasion resistance, 92%; after heat storage (54. + -. 2 ℃/14 d): content 39.5%; suspension percentage, 62.9%; wetting time, 80 s; dispersibility, 63.5%.

Examples of biological Activity test

Sowing quantitative barnyard grass and eclipta prostrata seeds in a disposable paper cup with the height of 9cm, covering soil with 0.5cm after sowing, flattening and sprinkling water, putting the paper cup in a greenhouse for culturing according to a conventional method, and performing soil spraying treatment (the spraying pressure is 1.95 kg/cm) on a crawler-type crop sprayer (designed and produced by Engineer Research Ltd. in British) according to the experimental design dosage 24 hours after sowing²The liquid spraying amount is 500L/ha, and the crawler speed is 1.48 km/h). The experiment was repeated 3 times. And (5) after the test material is treated, placing the treated test material in a greenhouse for management according to a conventional method. The reaction of the weeds to the herbicide was observed and recorded, and the effect of the herbicide on weed control was periodically investigated visually (see table below). Solving the linear regression equation and ED of each medicament on the tested weeds by applying a DPS2000 data processing system₉₀And (4) evaluating the herbicidal activity of the test agent.

Visual ED of barnyard grass and snakehead intestine for different formulations₉₀Value (21 days after treatment)

The data show that the preparation variety developed by the invention has proper dynamic surface tension and proper droplet particle size, so that the liquid medicine is well spread, wetted and attached on a target, the retention time is long, the liquid medicine has small drift and slow evaporation, the rapid conduction of active ingredients can be promoted, and the biological activity of active ingredients can be improved, therefore, the preparation has a remarkable 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

1. A herbicidal formulation characterized by: the active component is ethyl 2- (2-chloro-5- (3-chloro-5-trifluoromethylpyridin-2-yl) -N-methylbenzenesulfonamide) acetate, and the structural formula is as follows:

2. a herbicidal formulation according to claim 1, characterized in that: the preparation is powder, wettable powder, granules, water dispersible granules, emulsifiable powder (granules), effervescent granules, effervescent tablets, micro-capsule granules, slow release granules or medicinal fertilizers.

3. A herbicidal formulation according to claim 2, characterized in that: the preparation is wettable powder, water dispersible granules, sustained-release granules or emulsifiable powder (granules).

4. A herbicidal formulation according to claims 1, 2, characterized in that: the preparation comprises an active component, at least one carrier and at least one surfactant; wherein, the weight percentage of the active components is 0.1 to 99 percent.

5. A herbicidal formulation according to claim 4, characterized in that: in the wettable powder, 10-85% of active component, 3-15% of surface activity and the balance of carrier; in the water dispersible granule, 20-90% of active component, 5-20% of surfactant and the balance of carrier; in the emulsifiable powder (or granule) agent, 5-30% of active component, 10-40% of surfactant, 5-15% of solvent and the rest is carrier; in the sustained-release granules, 0.5-10% of active component, 2-10% of surfactant and the balance of carrier.

6. A herbicidal formulation according to claim 5, characterized in that:

the surfactant of the wettable powder is one or a mixture of a wetting agent Morwet EFW, a dispersant Supergil MNS/90, an alkyl naphthalene sulfonic acid polycondensate sodium salt, an alkyl naphthalene sulfonate formaldehyde condensate, sodium dodecyl sulfate, a polycarboxylate dispersant GY-D02, methylene naphthalene sodium sulfonate, sodium lignosulfonate, a wetting agent TENSIOFIX BCZ, a dispersant SK-24R, a wetting agent Rhodasurf 860/p, a dispersant Morwet D-400, a dispersant YUS-WP1, a wetting agent YUS-A51G, a dispersant SD819, a dispersant SK-12WP, a dispersant SK-20TX, a dispersant YUS-WP2, a wetting agent YUS-NV1203, TANEMULL DA2883, a dispersant SP-2836, a dispersant YUS-FS7PG and a wetting agent YUS-LXC; the carrier comprises: one or more of white carbon black, diatomite, kaolin, attapulgite and light calcium carbonate;

the surfactant of the water dispersible granule is one or a mixture of more of dispersant YUS-WG4, sodium salt of alkyl naphthalene sulfonic acid polycondensate, dispersant SK-20TX, dispersant YUS-WG5, wetting agent TENSIOFIX BCZ, dispersant SP2836, dispersant Supergil MNS/90, wetting agent YUS-SXC, dispersant Soprophor FD, dispersant PICO-WG7, wetting agent PICO-NW1, wetting agent PICO-NW2, calcium lignosulfonate, alkyl naphthalene sulfonate formaldehyde condensate (NNO), dispersant YUS-FS7PG, dispersant YUS-FS1 and dispersant PICO-JK; carrier: one or more of diatomite, kaolin and attapulgite are mixed;

the surfactant of the emulsifiable powder (particle) agent 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-methyl pyrrolidone, 10 parts of solvent oil S-150, Armid DM10, Rhodiasolv Green SV-92, Rhodiasolv Green SV-33 and/or Rhodiasolv Green 25; carrier: one or more of attapulgite, activated clay, kaolin and kaolin are mixed;

the surfactant of the sustained-release granules is one or a mixture of more of calcium lignosulfonate, alkyl naphthalene sulfonic acid polycondensate sodium salt serving as a dispersing agent, a sodium methyl naphthalene sulfonate formaldehyde condensate, a wetting agent TENSIOFIX BCZ, polyvinyl alcohol, an ethylene oxide propylene oxide block copolymer, diphenylmethane-4' 4-diisocyanate, ethylenediamine, chitosan and sodium carboxymethyl starch; the carrier is one or a mixture of more of white carbon black, attapulgite, kaolin and bentonite.

7. A herbicidal preparation as claimed in claim 1, which is useful for controlling broad-leaved weeds and grassy weeds in transplanted or direct-seeded rice fields.