CN111165498A - Bactericidal composition containing Dichlorobentiazox and fluorophenyletheramide, and application and preparation method thereof - Google Patents
Bactericidal composition containing Dichlorobentiazox and fluorophenyletheramide, and application and preparation method thereof Download PDFInfo
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- CN111165498A CN111165498A CN201811339148.2A CN201811339148A CN111165498A CN 111165498 A CN111165498 A CN 111165498A CN 201811339148 A CN201811339148 A CN 201811339148A CN 111165498 A CN111165498 A CN 111165498A
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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
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
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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
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
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Abstract
The application relates to a bactericidal composition containing dichlobeniazox and fluorobenzene ether amide; specifically, the application relates to a bactericidal composition containing Dichlorobenthiazox and fluorobenzene ether amide, a preparation and application thereof, wherein the mass ratio of the effective components Dichlorobenthiazox and fluorobenzene ether amide is 1:15-15:1, and the total content of Dichlorobenthiazox and fluorobenzene ether amide in the bactericidal composition or the preparation is 1-90% by mass. The bactericidal composition can be prepared into any acceptable dosage form in pesticide application, such as a suspending agent, an emulsion in water, wettable powder and water dispersible granules. The bactericidal composition and the preparation are suitable for preventing and treating powdery mildew, banded sclerotial blight, gibberellic disease, fusarium wilt, leaf spot disease, late blight, rust disease, sclerotinia rot and rice blast of cereal crops or anthracnose or leaf spot disease of melon, fruit and vegetable crops.
Description
Technical Field
The application belongs to the technical field of pesticide compositions, and particularly relates to a bactericidal composition containing Dichlorobentiazox and fluorobenzene ether amide, and application and a preparation method thereof.
Background
The fluorobenzene ether amide is a succinate dehydrogenase inhibitor and has certain systemic conductivity. The fluophenylamide has a control effect on rice sheath blight, and also has a control effect on wheat powdery mildew and potato late blight. The structural formula of the fluorophenylene ether amide is as follows:
dichlobeniazox is a benzothiazole bactericide and is mainly used for preventing and treating rice diseases. Under the using dosage of 30g/hm2, the bactericidal composition has good control effect on rice blast and sheath blight, and the control effect on cucumber anthracnose reaches over 90 percent under the mass concentration of 1 mg/L. CAS registry number 957144-77-3, its structural formula is:
because of the non-standard use of the existing pesticide, the resistance of the disease to the pesticide is stronger and stronger, so that the use amount of the pesticide is increased year by year, and the environmental pollution is more and more serious. Therefore, the rational use of agricultural chemicals and fungicides for preparing compositions to expand the fungicidal spectrum and reduce the resistance to diseases is imminent.
Disclosure of Invention
The invention aims to provide a bactericidal composition, the active ingredients of the composition are Dichlorobenthiazox and fluorophenyletheramide, the composition has an obvious synergistic effect on rice sheath blight disease, the using amount of the active ingredients can be reduced, the use cost can be reduced, and the generation of disease resistance can be delayed.
In order to solve the technical problem, the following technical scheme is adopted in the application:
in one aspect, the present application provides a germicidal composition comprising dichlobenizox and fluorophenyletheramide.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:15 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:5 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is 1:2 to 3: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 5: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 15: 1.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenyletheramide in the germicidal composition is 1 to 90% by mass.
In one or more embodiments, the total content of dichlobenizox and fluorophenyletheramide in the germicidal composition is 10 to 60% by mass.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenyletheramide in the germicidal composition is 15-60% by mass.
In another aspect, the present application provides a formulation prepared from the germicidal composition of the present application.
In one or more embodiments, the formulation is in the form of a suspension, an aqueous emulsion, a wettable powder, a water dispersible granule, a microemulsion, or an oil suspension.
In another aspect, the present application provides a use of the fungicidal composition of the present application for controlling powdery mildew, banded sclerotial blight, gibberellic disease, fusarium wilt, leaf spot, late blight, rust disease, sclerotinia, rice blast, or anthracnose or leaf spot of melon, fruit and vegetable crops of cereal crops.
In a further aspect, the present application provides the use of the formulations of the present application for controlling powdery mildew, banded sclerotial blight, head blight, late blight, rust, sclerotinia, rice blast, or anthracnose or leaf spot of melon, fruit and vegetable crops of cereals.
In yet another aspect, the present application provides a method of controlling powdery mildew, banded sclerotial blight, head blight, leaf spot, late blight, rust, sclerotinia, rice blast, or anthracnose or leaf spot of melon and vegetable crops of cereal crops comprising applying the fungicidal composition of the present application and/or the formulation of the present application to the cereal crops or melon and vegetable crops.
In one or more embodiments of the present application, "preventing" refers to prophylaxis and/or treatment.
In one or more embodiments herein, the germicidal compositions herein are compositions having a controlling effect on bacteria and/or fungi.
In yet another aspect, the present application provides a method of preparing the germicidal composition of the present application comprising combining dichlobeniazox with a fluorophenylether amide.
In one or more embodiments, the mass ratio of Dichlobentiazox to fluorophenylether amide is from 1:15 to 15: 1.
In one or more embodiments, the mass ratio of Dichlobentiazox to fluorophenylether amide is from 1:5 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 15: 1.
In one or more embodiments, the mass ratio of Dichlobentiazox to fluorophenylether amide is from 1:2 to 3: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 5: 1.
In yet another aspect, the present application provides a method of making a formulation of the present application, the method comprising combining the germicidal composition of the present application with one or more carriers, adjuvants and/or vehicles.
In one or more embodiments, the total content of dichlobenizox and fluorophenylether amide in the formulation is 1 to 90 mass%, preferably 10 to 60 mass%, more preferably 15 to 60 mass%.
In one or more embodiments, the formulation is prepared as a suspension, an aqueous emulsion, a wettable powder, a water dispersible granule, a microemulsion, or an oil suspension.
Detailed description of the invention
One or more embodiments of the present application provide a bactericidal composition or a formulation containing dichlobenizox and fluorophenyletheramide, which can produce a synergistic effect, maintain good effects while reducing the application amount of dichlobenizox and fluorophenyletheramide, broaden the bactericidal spectrum, and improve the safety in use.
In one aspect, the present application provides a germicidal composition comprising dichlobenizox and fluorophenyletheramide.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:15 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:5 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is 1:2 to 3: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 5: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorophenylether amide in the germicidal composition is 15:1, 10:1, 5:1, 3:1, 2:1, 1:2, 1:3, 1:5, 1:10, or 1: 15.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenyletheramide in the germicidal composition is 1 to 90% by mass.
In one or more embodiments, the total content of dichlobenizox and fluorophenyletheramide in the germicidal composition is 10 to 60% by mass.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenyletheramide in the germicidal composition is 15-60% by mass.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenyletheramide in the germicidal composition is 3.2, 16, 30, 33, 60, or 64 mass%.
In another aspect, the present application provides the use of a fungicidal composition for the control of powdery mildew, sheath blight, leaf spot, rust, sclerotinia, rice blast, or anthracnose or leaf spot of melon, fruit, and vegetable crops.
On the other hand, the preparation is in the form of a suspending agent, an aqueous emulsion, a wettable powder, a water dispersible granule, a microemulsion or an oil suspending agent.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorophenylether amide in the formulations herein is from 1:15 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorophenylether amide in the formulations herein is from 1:5 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 15: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorophenylether amide in the formulations herein is from 1:2 to 3: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorobenzene ether amide in the germicidal composition is from 1:1 to 5: 1.
In one or more embodiments, the mass ratio of dichlobeniazox to fluorophenylether amide in the formulations herein is 15:1, 10:1, 5:1, 3:1, 2:1, 1:2, 1:3, 1:5, 1:10, or 1: 15.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenylether amide in the formulation of the present application is 1 to 90% by mass.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenylether amide in the formulation of the present application is 10 to 60% by mass.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenylether amide in the formulation of the present application is 15 to 60% by mass.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenylether amide in the formulation of the present application is 30 to 60% by mass.
In one or more embodiments, the total content of Dichlobentiazox and fluorophenylether amide in the formulation of the present application is 3.2 mass%, 16 mass%, 30 mass%, 33 mass%, 60 mass%, or 64 mass%.
In a further aspect, the present application provides the use of the formulation for controlling powdery mildew, banded sclerotial blight, leaf spot, rust, sclerotinia, rice blast, or anthracnose or leaf spot of melon, fruit and vegetable crops of cereals.
In yet another aspect, the present application provides a method for controlling plant disease comprising applying to the plant or plant part an effective amount of a fungicidal composition and/or formulation of the present application.
The terms "comprising", "including" or "containing" are open-ended expressions that include what is specified in the application, but do not exclude other aspects.
The composition can be prepared into various suitable dosage forms according to actual agricultural use, and comprises the following components: water suspending agent, oil suspending agent, water dispersible granule, microemulsion, emulsion in water and the like. In the preparation, besides active ingredients, the preparation contains a surfactant, and can also contain diluents such as organic solvents or cosolvents, carriers (fillers) or water and the like according to different formulations. If necessary, other functional additives such as wetting agent, antifreezing agent, thickener, stabilizer, defoaming agent, or disintegrating agent can be added.
The wetting agent is selected from one or more of sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, sodium dibutyl naphthalene sulfonate, dioctyl sodium sulfosuccinate, Morwet EFW, GY-WS10, etc.
The dispersing agent is selected from one or more of naphthalene or alkyl naphthalene formaldehyde condensate sulfonate, fatty alcohol ethylene oxide adduct sulfonate, lignin and derivative sulfonate thereof, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, fatty alcohol polyoxyethylene ether sulfate, acrylic acid homopolymer sodium salt, maleic acid disodium salt and the like.
The emulsifier is selected from one or more of sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene formaldehyde condensate, fatty alcohol polyoxyethylene ether, triphenylethyl phenol polyoxyethylene polyoxypropylene ether, alkyl naphthalene sulfonate, fatty acid polyoxyethylene ester, AEO series and the like.
The thickening agent is selected from one or more of white carbon black, kaolin, bentonite, xanthan gum, sodium carboxymethyl cellulose and the like.
The disintegrating agent is selected from one or more of urea, bentonite, aluminum chloride, ammonium sulfate, succinic acid, sodium bicarbonate, etc.
The antifreezing agent is one or more selected from glycerol, ethylene glycol, propylene glycol and the like.
The defoaming agent is selected from one or more of silicone defoaming agent, C8-C10 fatty alcohol defoaming agent and the like.
The solvent is one or more of toluene, xylene, cyclohexanone, aromatic solvent, methanol, ethyl acetate, soybean oil, epoxidized soybean oil, castor oil and the like.
The stabilizer is selected from one or more of triphenyl phosphite, acetic anhydride, epichlorohydrin, resorcinol, sodium citrate and the like.
The preservative is selected from one or more of sodium benzoate, benzoic acid, potassium sorbate, kasong and the like.
The preparation method of various dosage forms of the bactericidal composition can adopt the known method and equipment, which are the common methods in the preparation method of pesticide preparations.
The bactericidal composition or the preparation is used for preventing and treating rice sheath blight disease.
In one or more embodiments, based on indoor toxicity measurement and field efficacy test, the application finds that the composition containing dichlobeniazox and fluorophenyletheramide has obvious synergistic effect, can improve the bactericidal effect, thereby reducing the application times and application amount, delaying the generation of drug resistance of germs, and is safe to crops and non-target organisms.
One or more embodiments of the present application provide a germicidal composition or formulation having one or more of the following advantages:
(1) the two effective component compositions have good synergistic effect;
(2) the generation of drug resistance is delayed;
(3) the production cost and the use cost are reduced;
(4) safe for crops and non-target organisms.
Detailed Description
The present application is further illustrated by the following examples, it should be understood that the preparation methods described in the examples are illustrative only and not limiting, and that simple modifications of the preparation methods described in the examples are intended to fall within the scope of the claims. The detailed proportions of the compositions are described in the formulation examples; the biological activity of the compositions is described in the biological activity examples.
In the following examples, all percentages are by weight unless otherwise indicated.
The technical product fluorobenzene ether amide is prepared by self, and the preparation method refers to CN104557709A example 1; dichlobentizox was purchased from hesu Henry Hengrong commercial Co., Ltd; other adjuvants, formulations, etc. used are commercially available.
Indoor bioassay test
measuring the growth inhibition effect of different agents on Rhizoctonia solani (Rhizoctonia solani Kuhn) by adopting a hypha growth rate method indoors, and calculating the EC of each agent on pathogenic bacteria50The value is obtained.
Activating strains:
selecting strains from test tubes (purchased from China agricultural microbial culture Collection center, ACCC36246), placing in the middle of potato glucose agar (PDA) culture medium, placing in 26 deg.C incubator for 2d, then selecting strains from cultured colonies, placing in the middle of new PDA culture medium, placing in 26 deg.C incubator for 2 d.
Weighing and preparing a sample:
a certain amount of sample (shown in Table 1) (single dose or a certain proportion of composition) is weighed, dissolved by using a solvent dimethyl sulfoxide, and then added with sterile aqueous solution containing 0.1% of Tween-80 to be released to 12.5mg/L, 25mg/L, 50mg/L, 100mg/L and 200mg/L for later use.
Plate addition method:
preparing a toxic plate by adopting the compound and a culture medium: in a clean bench, 5mL of sterilized compound solution was added to 45mL of PDA medium (cooled to 45-50 ℃ C.) (sterilization mode: UV sterilization), mixed well, poured onto a plate (diameter 90mm), cooled, and repeated for 3 plates. PDA medium with the addition of an equal amount of sterile water containing the same solvent emulsifier instead of compound solution served as blank.
The inoculated pellet (diameter 6mm) was picked and placed upside down in the center of the plate and incubated in an incubator at 26 ℃ for 2 days (incubation time should be determined according to growth conditions, typically when the diameter of the colony in the blank grows to 70-80 mm). The colony diameter was measured by the cross method.
Colony spread diameter (mm) ═ average diameter of colony (mm) -6(mm)
The biometric data values are obtained by looking up a table based on the relative inhibition rates. And (3) taking the concentration logarithm as an abscissa, and converting the inhibition percentage into a biological probability value according to a biological statistic probability value conversion table as an ordinate to draw a toxicity regression equation. The mass concentration when the value of the several degrees is 5 is obtained by the equation and is the EC50。
And (3) calculating the co-toxicity coefficient (CTC) of the mixture by adopting a Sun Yunpei co-toxicity coefficient calculation formula, and determining the synergy of the mixture.
Using a single dosage of the mixture as a standard medicament (EC is usually selected)50Lower), the calculation is performed:
single agent virulence index (EC of standard agent)50EC of a single dose50)×100
Theoretical virulence index (TTI) is the virulence index of A single agent multiplied by the proportion of A single agent in the mixture and the virulence index of B single agent multiplied by the proportion of B single agent in the mixture.
Measured virulence index (ATI) ═ EC for standard single dose50EC of value/blend50Value x 100
Co-toxicity coefficient (measured toxicity index/theoretical toxicity index) × 100
The mixture has synergistic effect when CTC is greater than 120, is antagonistic when CTC is less than 80, and has additive effect between 80 and 120.
Table 1. determination results of toxicity coefficient of Dichlorobentiazox and fluorophenyletheramide in different proportions on rice sheath blight disease
As can be seen from Table 1, the bactericidal composition containing Dichlorobentazox and fluorophenyletheramide has a high synergistic effect on pathogenic bacteria of rice sheath blight, the mass ratio of Dichlorobentazox to fluorophenyletheramide is 1:5-15:1, the co-toxicity coefficients are both greater than 120, the synergistic effect is shown, and the synergistic effect is more prominent when the mass ratio is 1:2-3: 1. The bactericidal composition containing dichlobeniazox and fluorophenyletheramide can delay the generation of disease resistance and reduce the production cost and the use cost.
Formulation example 1: 30% Dichlobenzazox-fluorophenyletheramide suspension
1. Preparation of comminuted slurry
2g of phosphate dispersant (trade name: JR-P, Nanjing Jieyun technology Co., Ltd.), 1g of high molecular compound dispersant with a comb-shaped structure (trade name: TERSPERSE 2500, Huntsman), 2g of nonionic hydroxy polyethylene oxide block copolymer (Ethylan NS-500LQ, Nanjing Jieyun technology Co., Ltd.), 2g of wetting agent (trade name: GY-WS10, Beijing Guangyuan Yinong) and high-efficiency organic silicon defoamer (Hangzhou left soil)NOVEL MATERIAL Co., Ltd.) 0.4g, 15g of dichlobenizox base drug and 15g of fluorophenyletheramide were dispersed therein, and usedGlass beads (Zhejiang golden jade zirconium industries, Ltd.) were subjected to wet pulverization for 2.0 hours using a sand mill (Shenyang new micro-electric machine factory) to obtain 80g of pulverized slurry.
2. Preparation of Dispersion Medium
0.3g of xanthan gum (an avadin reagent), 0.4g of white carbon black (an avadin reagent), 5g of ethylene glycol (an avadin reagent) and 0.5g of sodium benzoate (an avadin reagent) were dispersed in 13.8g of water to obtain 20g of a dispersion medium.
3. Preparation of aqueous suspension pesticide composition
80g of the above-mentioned pulverized slurry was mixed with 20g of a dispersion medium to obtain 100g of an aqueous suspension-type agricultural chemical composition, thereby obtaining a suspension containing 30% by mass of active ingredients (Dichlobentiazox and fluorophenyletheramide).
Formulation example 2: 33% Dichlobenzazox fluorobenzene ether amide aqueous emulsion
1. Preparation of the oil phase
11g of Dichlorobentiazox technical material and 22g of fluorophenylether amide were added to a mixed solvent of 10g of cyclohexanone (an avadin reagent) and 20g of xylene (an avadin reagent), and then 1601# (tristyrylphenol polyoxyethylene polyoxypropylene ether, Switzerland chemical assistants, Inc. of Chaste) 3g of emulsifier, 5g of castor oil polyoxyethylene ether (trade name: EMULPON CO-360, Huntsman) were added and slowly stirred until completely dissolved.
2. Preparation of aqueous phase
3g of ethylene glycol (avadin reagent), 0.1g of xanthan gum (avadin reagent), 0.4g of high-efficiency organic silicon defoamer (New Material Co., Ltd., left Hangzhou China) and 25.5g of water are uniformly stirred.
3. Blending of pesticide composition aqueous emulsion
The oil phase was slowly added to the aqueous phase, and stirred until completely added, and then an aqueous emulsion having an active ingredient (Dichlobentiazox and fluorophenyletheramide) content of 33% by mass was obtained under high shear (8000 rpm) for 15 minutes in a high speed disperser (trade name: TG25, IKA, germany).
Formulation example 3: 60% dichlobenizox fluorobenzene ether amide water dispersible granule
50g of Dichlorobentazox raw medicine, 10g of fluorophenyletheramide, 2g of a high molecular compound dispersing agent with a comb-shaped structure (trade name: TERSPERSE 2500, Huntsman), 3g of lignin C (Guangzhou bush laugh chemical industry Co., Ltd.), 5g of ammonium sulfate (latin reagent), 0.4g of magnesium aluminum silicate (latin reagent), 0.3g of white carbon black (Hangzhou left soil new material Co., Ltd.), 0.2g of WJB-20 (Shanghai Wanjin Co., Ltd.), and 100g of kaolin (Hangzhou left soil new material Co., Ltd.) are added, pre-crushed and uniformly mixed, and then crushed by air flow (Kunshan Yongke machinery Co., Ltd.) to a required particle size (0-5 micrometers), and granulated by a rotary granulator to prepare the water dispersible granule with the mass content of the effective components (Dichlorobentazox and fluorophenyletheramide) of 60%.
Formulation example 4: 64% Dichlobenzazox fluorobenzene ether amide wettable powder
60g of Dichlobentiazox technical material, 4g of fluorophenyletheramide, 5g of naphthalene sulfonate polycondensate (trade name: Morwet D-425, Acksonobel), 3g of lignin C (New left soil material Co., Ltd. Hangzhou), 5g of ammonium sulfate (Oratin reagent), 0.5g of xanthan gum (Oratin reagent), 0.2g of organic silicone (trade name: DOW CORNING ANTIFOAM C EMULSION, DOW CORNING), and adding 100g of kaolin (New left soil material Co., Ltd. Hangzhou) to obtain wettable powder with the mass content of effective components (Dichlobentiazox and fluorophenyletheramide) of 64 percent by pre-crushing, uniformly mixing, and then carrying out air flow crushing (Kunshanounake machinery Co., Ltd.) to obtain the required particle size (0-5 microns).
Formulation example 5: 16% dichlobenizox-fluorophenyletheramide microemulsion
1. Preparation of the oil phase
4g of Dichlorobentiazox technical material and 12g of fluorophenylether amide are added into a mixed solvent of 10g of cyclohexanone (an latin reagent) and 15g of AG-1705 (an environmentally friendly solvent, Huntsman), and then 10g of TERMUL 200 (an alkylphenol block polyether copolymer emulsifier, Huntsman) and 14g of Nongru 1601# (tristyrylphenol polyoxyethylene polyoxypropylene ether, Switzerland chemical assistants, Inc., from Schott) are added and slowly stirred until completely dissolved.
2. Preparation of aqueous phase
4g of n-butanol (an latin reagent), 0.2g of high-efficiency organic silicon defoamer (Hangzhou left soil new material Co., Ltd.), and 30.8g of deionized water are uniformly stirred.
3. Compounding of composition in water emulsion
Slowly adding the oil phase into the water phase, and continuously stirring until the oil phase is transparent to obtain microemulsion with the mass content of the effective components (Dichlorobentazox and fluorobenzene ether amide) of 16%.
Formulation example 6: 3.2% Dichlobenzazox fluorobenzene ether amide oil suspending agent
Adding 0.2g of Dichlobetiazox technical and 3g of fluorophenyletheramide into a mixed solvent of 40g of methyl oleate (an avastin reagent) and 34.4g of soybean oil (the avastin reagent), then 5g of macromolecular compound dispersant (trade name: TERSPERSE 2500, Huntsman) with a comb-shaped structure, 7g of nonionic hydroxy polyethylene oxide block copolymer (Ethylan NS-500LQ, Nanjing Jieron science and technology Limited) and 8g of emulsifier (calcium dodecylbenzene sulfonate, trade name: Nongru 500#, Swedish Cork chemical auxiliary agent of Schedle and Taiwan) are added into the system for shearing by a homogenizer, then adding 0.2g of high-efficiency organic silicon defoamer (Hangzhou left soil new material Co., Ltd.), 2g of thickener bentonite (Hangzhou left soil new material Co., Ltd.), and 0.2g of WIB-20 (Shanghai Wanjin) to mix, sanding for 1.5h, and finally stirring for 20min by a high-speed shearing machine to obtain the suspending agent with the active ingredients (Dichlorobentazox and fluorophenyletheramide) of which the mass content is 32%.
Comparative example 1: 30% Dichlobeniazox suspension
1. Preparation of comminuted slurry
2g of a non-alkylphenol type high-efficiency dispersant (trade name: TERSPERSE 4894, Huntsman), 2g of a comb-structured polymer dispersant (trade name: TERSPERSE 2500, Huntsman), 3g of a wetting agent (trade name: GY-WS10, Guangyuan Yinong Beijing) and 0.3g of a high-efficiency silicone defoamer (silicone defoamer, ETXP-40, left earth new material Co., Ltd. of Hangzhou) were dispersed in 42.7g of water, 30g of a Dichlorobentazox base drug was dispersed therein, and the water was usedGlass beads (Zhejiang golden jade zirconium industries, Ltd.) were subjected to wet pulverization for 1.5 hours using a sand mill (Shenyang new micro-electric machine factory) to obtain 80g of pulverized slurry.
2. Preparation of Dispersion Medium
In 15.2g of water were dispersed 0.2g of xanthan gum (avadin reagent), 0.5g of magnesium aluminum silicate (avadin reagent), 4g of ethylene glycol (avadin reagent) and 0.1g of sodium benzoate (avadin reagent) to obtain 20g of a dispersion medium.
3. Preparation of aqueous suspension pesticide composition
The above pulverized slurry (80 g) and a dispersion medium (20 g) were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and a suspension concentrate containing an active ingredient (dichlobeniazox) in an amount of 30% by mass was obtained.
Comparative example 2: 64% fluorobenzene ether amide wettable powder
The wettable powder with the mass content of the active ingredient (fluorobenzene ether amide) of 64g is prepared by adding 64g of fluorobenzene ether amide, 5g of naphthalenesulfonate polycondensate (trade name: Morwet D-425, Acksonobel), 3g of lignin C (New left soil material Co., Ltd., Hangzhou), 5g of ammonium sulfate (Alisma reagent), 0.5g of xanthan gum (Alisma reagent), 0.2g of organic silicone (trade name: DOW CORNING ANTIFOAM C EMULSION, DOW CORNING) to 100g of kaolin (New left soil material Co., Ltd., Hangzhou) to the mixture, pre-crushing and uniformly mixing the mixture, and then crushing the mixture by air flow (Younganc mechanical Co., Ltd., Hangzhou) to the required particle size (0-5 micrometers).
Test of field drug effect
And (3) test treatment: the test agents of examples 1 to 3 were each set with two effective ingredient amounts according to the test design of the test agents in Table 2. The control agents are 30% dichlobeniazox suspending agent and 64% fluorophenyletheramide wettable powder and blank clear water in the control example respectively.
TABLE 2 test design of field drug effect of test agent
Setting a cell: each cell area is 66.7m2;
The application method comprises the following steps: applying a medicament at the early stage of rice sheath blight disease, and carrying out leaf surface spraying treatment, wherein the spraying amount is mainly no water drops;
the application times are as follows: and 3 times, if the rainfall is expected to be in strong wind weather or within 1 hour, the pesticide is not applied. The disease condition base is investigated before the first application, the subsequent application is carried out for 1 time every 7 days, and the control effect is investigated 7 days after the 3 rd application.
Investigation time and number of times: base number was investigated 1 day after administration, and disease index was investigated 7 days and 14 days after administration.
The investigation method comprises the following steps: and (4) grading according to the damage symptom degrees of the rice leaf sheaths and the rice leaves, taking the plants as a unit, sampling five points on the diagonal line of each cell, surveying 5 connected clusters at each point for 25 clusters, and recording the total plant number, the diseased plant number and the disease grade number.
The method for investigating before pesticide application and checking the pesticide effect after prevention and treatment comprises the following steps: randomly sampling 5 points in the test treatment area, and recording the total leaf number, the diseased leaf number and the diseased stage number. The standard method of classification is as follows:
level 0: the whole plant is disease-free;
level 1: the fourth leaf and the leaf sheaths below the fourth leaf, wherein the leaf is diseased (the sword leaf is taken as the first leaf);
and 3, level: the third leaf and the leaf sheaths below the third leaf cause diseases;
and 5, stage: the second leaf and the leaf sheaths below the second leaf cause diseases;
and 7, stage: the scabies of the sword leaf and the leaf sheaths below the sword leaf are attacked;
and 9, stage: the whole plant is attacked and withered in advance.
And (3) calculating the drug effect:
the results of the tests are detailed in table 3 below.
TABLE 3 field test results of the test agents
As shown in Table 3, the bactericidal composition containing Dichlorobentazox and fluorophenyletheramide has good control effect on rice sheath blight, and the control effect is more than 85% in 21 days after the application. Compared with a single preparation, the bactericidal composition has the advantages that the quick-acting property and the lasting effect are better than those of a control single preparation, the bactericidal composition and the control single preparation can show a synergistic effect after being combined, and the administration times can be reduced. In addition, no toxicity of the pesticide composition to rice is found in the application range, and the bactericidal composition is good in safety to crops and can be popularized and applied.
The preferred embodiments of the present application have been described in detail above, but the present application is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present application within the technical idea of the present application, and these simple modifications all belong to the protection scope of the present application.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described in the present application.
In addition, any combination of the various embodiments of the present application is also possible, and the same should be considered as disclosed in the present application as long as it does not depart from the idea of the present application.
Claims (10)
1. A germicidal composition comprising dichlobeniazox and fluorophenyletheramide.
2. The bactericidal composition according to claim 1, wherein the mass ratio of dichlobeniazox to fluorophenyletheramide is 1:15 to 15:1, preferably 1:5 to 15:1, 1:1 to 15:1, 1:2 to 3:1, more preferably 1:1 to 5: 1.
3. The fungicidal composition according to claim 1, wherein the total content of dichlobeniazox and fluorophenyletheramide in the fungicidal composition is 1 to 90% by mass, preferably 10 to 60% by mass, more preferably 15 to 60% by mass.
4. A formulation prepared from the germicidal composition of any of claims 1-3.
5. The formulation of claim 4, wherein the formulation is in the form of a suspension, an aqueous emulsion, a wettable powder, a water dispersible granule, a microemulsion, or an oil suspension.
6. Use of the fungicidal composition according to any one of claims 1 to 3 for controlling powdery mildew, banded sclerotial blight, gibberellic disease, blight, leaf spot, late blight, rust disease, sclerotinia disease, rice blast, or anthracnose or leaf spot of melon, fruit and vegetable crops.
7. Use of the formulation according to claim 4 or 5 for controlling powdery mildew, banded sclerotial blight, head blight, leaf spot, late blight, rust, sclerotinia, rice blast, or anthracnose or leaf spot of melon, fruit and vegetable crops.
8. A method for controlling powdery mildew, banded sclerotial blight, gibberellic disease, fusarium wilt, leaf spot, late blight, rust disease, sclerotinia disease, rice blast, or anthracnose or leaf spot of melon, fruit and vegetable crops of cereal crops, which comprises applying the fungicidal composition of any one of claims 1 to 3 and/or the formulation of claim 4 or 5 to the cereal crops or melon, fruit and vegetable crops.
9. A process for the preparation of a fungicidal composition according to any of claims 1 to 3, which process comprises combining dichlobeniazox with a fluorophenylether amide, preferably in a mass ratio of dichlobeniazox to fluorophenylether amide of from 1:15 to 15:1, preferably from 1:5 to 15:1, from 1:1 to 15:1, from 1:2 to 3:1, more preferably from 1:1 to 5: 1.
10. A method of preparing a formulation according to claim 4 or 5, the method comprising combining a fungicidal composition according to any one of claims 1 to 3 with one or more carriers, adjuvants and/or excipients, preferably wherein the total content of dichlobeniazox and flufenide in the formulation is from 1 to 90 mass%, preferably from 10 to 60 mass%, more preferably from 15 to 60 mass%, preferably the formulation is prepared as a suspension, an aqueous emulsion, a wettable powder, a water dispersible granule, a microemulsion or an oil suspension.
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