CN111838161A - Pyridachlorometyl and fluorobenzene ether amide-containing bactericidal composition and application thereof - Google Patents

Pyridachlorometyl and fluorobenzene ether amide-containing bactericidal composition and application thereof Download PDF

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CN111838161A
CN111838161A CN201910334672.9A CN201910334672A CN111838161A CN 111838161 A CN111838161 A CN 111838161A CN 201910334672 A CN201910334672 A CN 201910334672A CN 111838161 A CN111838161 A CN 111838161A
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pyridachlorometyl
composition
ether amide
fluorobenzene ether
amide
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李义涛
崔儒坤
梁任龙
刘新烁
张伟
陈锦昌
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Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd
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Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/581,2-Diazines; Hydrogenated 1,2-diazines

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  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
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Abstract

The invention relates to a bactericidal composition containing pyridachlorometyl and fluorobenzene ether amide, a preparation and application thereof, wherein the mass ratio of active ingredients pyridachlorometyl to fluorobenzene ether amide is 1-3: 5-1, the mass percentage content of pyridachlorometyl and fluorobenzene ether amide in the bactericidal composition/preparation is 20-80%, and the balance is auxiliary materials. The bactericidal composition/preparation of the invention has obvious synergistic effect on the prevention and treatment of cucumber powdery mildew. The sterilization composition and the preparation are suitable for preventing and treating powdery mildew of cucumber; and application in rice blast and sheath blight.

Description

Pyridachlorometyl and fluorobenzene ether amide-containing bactericidal composition and application thereof
Technical Field
The invention belongs to the technical field of pesticides, and relates to a bactericidal composition containing pyridachlorometyl and fluorobenzene ether amide.
Background
Cucumber powdery mildew is one of the main diseases in the current cucumber production. The cucumber powdery mildew is commonly called as 'white hair disease', the damage of leaves is the heaviest, then, the leaves and stems are the second, after the leaves and tender stems are infected by the powdery mildew, the symptoms are similar to those on the leaves, the scab is smaller, and the powder is less. Yellow spots begin to appear on the leaves, then the yellow spots expand and develop into round or oval spots, and white powdery mildew layers appear on the surfaces. Typically, there are more lower blades than upper blades, and more blades on the back than on the front. The mildew stains are independently dispersed at the early stage and then combined into a large mildew spot, even the large mildew spot can cover the whole leaves, the photosynthesis is seriously influenced, the normal metabolism is interfered, the premature senility is caused, and the cucumber yield is lost.
Pyridachlorometyl (development code: S-2190) is a pyridazine bactericide developed by Nippon Sumitomo chemical Co., Ltd., and is effective in preventing cucumber powdery mildew. CAS registry number 1358061-55-8, its structural formula is:
Figure BDA0002038783430000011
the fluorophenylene ether amide (development code: Y13149) is a succinate dehydrogenase inhibitor and has certain systemic conductivity. The fluophenylamide has excellent control effect on powdery mildew of cucumber and has excellent control effect on rice blast and banded sclerotial blight. The structural formula of the fluorophenylene ether amide is as follows:
Figure BDA0002038783430000012
however, the single bactericide cannot completely and effectively control the cucumber powdery mildew, and in the actual process of agricultural production, because the current pesticide is used in an irregular manner, the resistance of diseases to the pesticide is stronger and stronger, so that the using amount of the pesticide is increased year by year, and the environmental pollution is more and more serious.
Therefore, the development of a novel fungicide having a broad fungicide spectrum, a higher control effect and a reduced disease resistance is urgent.
Disclosure of Invention
The invention aims to provide a bactericidal composition, the effective components of the composition are pyridachlorometyl and fluorobenzene ether amide, the composition has obvious synergistic effect on cucumber powdery mildew, the using amount of the effective components can be reduced, the use cost can be reduced, and the generation of disease resistance can be delayed.
The technical scheme adopted for achieving the purpose of the invention is as follows:
in one aspect, the present invention provides a germicidal composition, wherein the active ingredients of the germicidal composition include pyridachlorometyl and fluorophenylether amide.
In some embodiments, the active ingredients of the germicidal composition of the present invention are pyridachlorometyl and fluorobenzene ether amide.
Further, the mass ratio of Pyridachlorometyl to fluorobenzene ether amide is 1-40: 40-1.
Further, the mass ratio of Pyridachlorometyl to fluorobenzene ether amide is 1-20: 20-1.
Furthermore, the mass ratio of Pyridachlorometyl to fluorobenzene ether amide is 1-10: 20-1.
Preferably, the mass ratio of Pyridachlorometyl to fluorobenzene ether amide is 1-5: 5-1.
Further preferably, the mass ratio of Pyridachlorometyl to fluorobenzene ether amide is 1-3: 1-5.
Furthermore, the mass percentage of Pyridachlorometyl and the fluorophenyletheramide in the bactericidal composition is 1-99%, and the balance is auxiliary materials.
Furthermore, the mass percentage of Pyridachlorometyl and the fluorophenyletheramide in the bactericidal composition is 10-90%, and the balance is auxiliary materials.
Preferably, the mass percentage of Pyridachlorometyl and the fluorophenyletheramide in the bactericidal composition is 20-80%, and the balance is auxiliary materials.
In another aspect, the invention provides the use of a fungicidal composition comprising pyridachlorometyl and fluorophenylether amide for the control of cucumber powdery mildew, rice blast and/or sheath blight.
On the other hand, the invention provides a bactericide which is prepared from the bactericidal composition and auxiliary materials acceptable in pesticide preparations.
On the other hand, the bactericide provided by the invention is in any one of missible oil, wettable powder, suspending agent, granules, water dispersible granules, microemulsion, emulsion in water or microcapsules.
In still another aspect, the present invention provides a method for controlling plant diseases, the method comprising applying an effective amount of a fungicidal composition comprising a fluorophenylether amide and pyridachlorometyl or a preparation comprising a fluorophenylether amide and pyridachlorometyl to the plant or plant part.
Detailed description of the invention
The invention provides a bactericidal composition or a preparation containing pyridachlorometyl and fluorobenzene ether amide, which can produce a synergistic effect, maintain good effect while reducing the application amount and improve the use safety.
In one aspect, the present invention provides a germicidal composition, wherein the active ingredients of the germicidal composition include pyridachlorometyl and fluorophenylether amide.
In some embodiments, the present invention provides a germicidal composition, wherein the effective components of the germicidal composition are pyridachlorometyl and fluorobenzene ether amide.
Furthermore, the mass ratio of Pyridachlorometyl to fluorobenzene ether amide in the bactericidal composition is 1-40: 40-1.
Furthermore, the mass ratio of Pyridachlorometyl to the fluorobenzene ether amide in the bactericidal composition is 1-20: 20-1.
Furthermore, the mass ratio of Pyridachlorometyl to fluorobenzene ether amide in the bactericidal composition is 1-10: 20-1.
Preferably, the mass ratio of pyridachlorometyl to fluorobenzene ether amide in the bactericidal composition is 1-5: 5-1.
More preferably, the mass ratio of Pyridachlorometyl to the fluorophenylether amide is 1-3: 5-1.
Specifically, the mass ratio of Pyridachlorometyl to fluorophenylether amide in the bactericidal composition is 1: 1, 1: 2, 1: 3, 1: 5, 1: 10, 1: 20, 1: 40, 2: 1, 3: 1, 5: 1, 10: 1, 20: 1 or 40: 1.
Furthermore, the mass percentage of Pyridachlorometyl and fluorobenzene ether amide in the sterilization composition is 1-99%, and the balance is auxiliary materials.
Furthermore, the mass percentage of the pyridachlorometyl and the fluorobenzene ether amide in the sterilization composition is 10-90%, and the balance is auxiliary materials.
Preferably, the mass percentage of the pyridachlorometyl and the fluorobenzene ether amide in the sterilization composition is 20-80%, and the balance is auxiliary materials.
Specifically, the content of pyridachlorometyl and fluorobenzene ether amide in the bactericidal composition is 8%, 20%, 36%, 40%, 50%, 60% or 80% by mass.
In another aspect, the invention provides the use of a fungicidal composition comprising pyridachlorometyl and fluorophenylether amide for the control of cucumber powdery mildew, rice blast and/or sheath blight.
On the other hand, the invention provides a bactericide which is prepared from the bactericidal composition and auxiliary materials acceptable in pesticide preparations.
On the other hand, the bactericide provided by the invention is in any one of missible oil, wettable powder, suspending agent, granules, water dispersible granules, microemulsion, emulsion in water or microcapsules.
In still another aspect, the present invention provides a method for controlling plant diseases, the method comprising applying an effective amount of a fungicidal composition comprising a fluorophenylether amide and pyridachlorometyl or a preparation comprising a fluorophenylether amide and pyridachlorometyl to the plant or plant part.
The term "comprising" is open-ended, i.e. includes the elements indicated in the present invention, but does not exclude other elements.
For the purposes of the present invention, the term "effective amount" means the total amount of the individual active ingredients in an amount sufficient to exhibit the desired control effect. This amount varies within wide limits depending on the fungus to be controlled, the plant species, the climatic conditions and the compounds contained in the composition according to the invention.
The invention can be processed into various suitable dosage forms according to actual agricultural use, including: water suspending agent, oil suspending agent, water dispersible granule, microemulsion, emulsion in water and the like. In the preparation, besides the active ingredients, the pesticide preparation also comprises auxiliary materials acceptable for pesticide preparations, wherein the auxiliary materials refer to wetting agents, dispersing agents, emulsifying agents, thickening agents, disintegrating agents, antifreezing agents, antifoaming agents, solvents, stabilizing agents, preservatives and the like. The composition may contain organic solvent or cosolvent, carrier (filler) or water and other diluents according to different formulations. If necessary, adding other functional additives such as an antifreeze agent, a thickening agent, a stabilizing agent, a defoaming agent, a disintegrating agent and the like.
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 and the like.
The dispersing agent is selected from one or more than two of naphthalenesulfonate polycondensate, 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, JR-P, TERSPERSE 2500, TERSPERSE 4894, Ethylan NS-500LQ 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, tristyrylphenol polyoxyethylene polyoxypropylene ether, alkyl naphthalene sulfonate, fatty acid polyoxyethylene ester, AEO series, nonionic hydroxy polyethylene oxide block copolymer, alkylphenol block polyether copolymer type emulsifier, castor oil polyoxyethylene ether, n-butyl alcohol and the like.
The thickening agent is one or more than two of white carbon black, kaolin, bentonite, xanthan gum, sodium carboxymethylcellulose, magnesium aluminum silicate and the like.
The disintegrating agent is one or more selected from urea, bentonite, aluminum chloride, ammonium sulfate, succinic acid, sodium bicarbonate, etc.
The antifreezing agent is one or more than two of glycerol, ethylene glycol, propylene glycol and the like.
The defoaming agent is selected from one or more of silicone defoaming agents, C8-10 fatty alcohol defoaming agents, silicone defoaming agents and the like.
The solvent is one or more of toluene, xylene, cyclohexanone, aromatic solvent, methanol, ethyl acetate, soybean oil, epoxy soybean oil, castor oil, AG-1705, n-butanol, etc.
The stabilizer is one or more than two 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, cason, WJB-20, etc.
The processing technology of various formulations of the bactericidal composition adopts known methods and equipment, and is a common method in the processing technology of pesticide preparations.
The bactericidal composition or the preparation of the invention is used for preventing and treating powdery mildew of cucumber and has the following beneficial effects: (1) the bactericidal composition shows good synergistic effect in a certain range, and the bactericidal effect is obviously improved compared with the simple addition of single agents; (2) the development of drug resistance of the single agent is delayed; (3) the dosage and the use cost are reduced; (4) is safe to crops and reduces the environmental pressure.
Detailed Description
The present invention is further illustrated by the following examples, it is to be understood that the preparation methods described in the examples are illustrative only and not limiting, and that simple modifications of the preparation methods of the present invention based on the concepts of the present invention are intended to be within the scope of the invention as claimed. In the formulation examples, the present invention introduces the detailed proportions of the compositions; in the bioactive examples, the invention details the outstanding bioactivity of the compositions. Pyridachlorometyl and fluorobenzene ether amide technical products are prepared by self, wherein the preparation method of the fluorophenylene ether amide refers to CN104557709A example 1, and the preparation method of the Pyridachlorometyl refers to CN103068238 and refers to preparation example 1; other reagents, adjuvants, formulations and the like used are commercially available.
In the following examples, all percentages are by weight unless otherwise indicated.
Indoor bioassay test
The method is characterized in that a potting method is adopted indoors, the inhibition effect of different agents on the growth of cucumber powdery mildew is measured, and the EC of each agent on pathogenic bacteria is calculated50The value is obtained.
Application of the medicine: selecting potted cucumber seedlings with consistent leaf length and vigor for experiments. The single dose or each composition (see Table 1) was dissolved in DMSO as a solvent, and then diluted with 0.1 wt% Tween 80 in water to 5mg/L, 2.5mg/L, 1.25mg/L, 0.625mg/L, 0.3125mg/L, and 0.15625 mg/L. Drying the test material in shade for 24h after spraying the stem leaves. The control group was spray treated with the same amount of solvent.
Inoculation: washing fresh spores on cucumber leaves with 0.1 wt% Tween 80 water solution, filtering with 2-4 layers of gauze to obtain a filtrate with a concentration of 6 × 105CFU/mL spore suspension, then using inoculation atomizer (pressure 0.1MPa) on cucumber seedlings evenly spray until the surface is wet. After spray inoculation, the seeds are moved into a climatic chamber, the relative humidity is 80 percent, the temperature is 25 ℃, the light intensity is 2000lx, and disease condition investigation is carried out after 7 days.
Grading standard:
level 0: no disease;
level 1: the area of the lesion spots accounts for less than 5% of the area of the whole leaf;
and 3, level: the area of the lesion spots accounts for 6 to 10 percent of the area of the whole leaf;
And 5, stage: the area of the lesion spots accounts for 11 to 20 percent of the area of the whole leaf;
and 7, stage: the area of the lesion spots accounts for 21 to 40 percent of the area of the whole leaf;
and 9, stage: the area of the lesion spots accounts for more than 40 percent of the area of the whole leaf.
And (3) calculating the drug effect:
Figure BDA0002038783430000051
Figure BDA0002038783430000052
corresponding regression analysis is carried out according to the concentration of each single agent and the composition and the corresponding control effect to obtain the EC of each single agent and the composition50The value is obtained.
The co-toxicity coefficient (CTC) of the mixture is calculated by adopting a co-toxicity coefficient calculation method introduced by Sun Yunpei, and the synergy of the mixture is determined.
Using a single dosage of the mixture as a standard medicament (EC is usually selected)50Lower), the calculation is performed:
single dose virulence index (standard dose EC)50A certain single agent EC50×100
Theoretical virulence index (TTI) ═ A virulence index of single agent, x proportion of single agent in mixed agent + B virulence index, x proportion of single agent in mixed agent
Measured virulence index (ATI) ═ EC for standard single dose50EC of value/blend50Value x 100
Co-toxicity coefficient (CTC) is measured virulence index/theoretical virulence index multiplied by 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 measurement results of various proportions of Pyridachlorometyl and fluorophenyletheramide for cucumber powdery mildew co-toxicity coefficient
Figure BDA0002038783430000053
Figure BDA0002038783430000061
As can be seen from Table 1, the bactericidal composition compounded by the pyritchlomeyl and the fluorophenylether amide has a high synergistic effect on cucumber powdery mildew pathogenic bacteria, the pyritchlomeyl and the fluorophenylether amide have a mass ratio of 10: 1-1: 20, the cotoxicity coefficients are both greater than 120, the bactericidal composition shows a synergistic effect, and the synergistic effect is more prominent when the mass ratio is 3: 1-1: 5. The bactericidal composition compounded by pyridachlorometyl and fluorobenzene ether amide can delay the generation of the drug resistance of diseases and reduce the production cost and the use cost.
Formulation example 1: 50% Pyridachlorometyl fluorobenzene ether amide suspension
1. Preparation of comminuted slurry
2g of phosphate dispersant (trade name: JR-P, Nanjing Jieron science and technology Limited), 1.5g of high molecular compound dispersant (trade name: TERSPERSE 2500, Huntsman) with a comb-shaped structure, 1.5g of nonionic hydroxy polyethylene oxide block copolymer (Ethyllan NS-500LQ, Nanjing Jieron science and technology Limited), 2g of wetting agent (GY-WS 10, Beijing Guangyuan Yinong), and 0.4g of high-efficiency organic silicon defoaming agent (ETXP-40, Hangzhou left soil new material Limited) are dispersed in 22.6g of water, 37.5g of Pyridachlorometyl raw material and 12.5g of fluorobenzene ether amide are dispersed in the water
Figure BDA0002038783430000062
The glass beads were subjected to wet pulverization for 2.0 hours using a sand mill (YS7142, Shenyang New micro electric machine Mill) to obtain 80g of a 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 pulverized slurry and 20g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, thereby obtaining a pyridachlorometyl/fluorophenylether amide suspension having an active ingredient mass content of 50%.
Formulation example 2: 20% Pyridachlorometyl fluorobenzene ether amide emulsion
10g of pyritchlomeyl technical raw material and 10g of fluorophenylether amide are added into a mixed solvent of 35g of cyclohexanone (an avadin reagent) and 35g of xylene (an avadin reagent), and then 5g of emulsifier agricultural emulsion 1601# (tristyrylphenol polyoxyethylene polyoxypropylene ether, chentai swallow chemical auxiliary agent limited company) and 5g of castor oil polyoxyethylene ether (trade name: EMULPON CO-360, Huntsman) are added and slowly stirred until the mixture is completely dissolved to prepare the pyritchlomeyl fluorophenylether amide emulsifiable concentrate with the active ingredient mass content of 20%.
Formulation example 3: 80% Pyridachlorometyl fluorobenzene ether amide water dispersible granule
13.33g of Pyridachlorometyl technical, 66.67g of fluorophenyletheramide, 2g of a comb-structured polymer dispersant (trade name: TERSPERSE 2500, Huntsman), 3g of lignin C (Congo chemical Co., Ltd., Guangzhou), 5g of ammonium sulfate (avastin reagent), and 0.4g of magnesium aluminum silicate (avastin 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, the mixture is pre-crushed and mixed uniformly, the mixture is crushed by air flow (model: SJM-100, Kunshan Yonke machine Co., Ltd.) to the required particle size (10-15 micrometers), and then a rotary granulator (model: ZLB1-80, Zongton drying engineering technology Co., Ltd.) is adopted for granulation to prepare the Pyridachlorometyl fluorobenzene amide water dispersible granule with the effective component mass content of 80%.
Formulation example 4: 60% Pyridachlorometyl fluorobenzene ether amide wettable powder
40g of pyritchlomeyl technical raw material, 20g of fluorophenylether amide, 5g of naphthalenesulfonate polycondensate (trade name: Morwet D-425, Acksonobel), 3g of lignin C (New left soil material Co., Ltd. in Hangzhou), 5g of ammonium sulfate (Alitin reagent), 0.5g of xanthan gum (Alitin reagent), 0.2g of organic silicone (OAM CORNING ANTIFC EMULSION, DOWCORNING) and 100g of kaolin (New left soil material Co., Ltd. in Hangzhou) are added, firstly pre-crushed and uniformly mixed, and then crushed by air flow (model: SJM-100, Yongnake machinery Co., Ltd. in Kunshan) to the required particle size (10-15 micrometers) to prepare the pyritchlomeyl fluorophenylether amide wettable powder with the mass content of 60 percent of the effective component.
Formulation example 5: 8% Pyridachlorometyl-fluorobenzene ether amide microemulsion
1. Preparation of the oil phase
2.67g of Pyridachlorometyl technical raw material and 5.33g of fluorobenzene ether amide are added into a mixed solvent of 8g of cyclohexanone (an avastin reagent) and 5g of AG-1705 (an environmentally friendly solvent, Huntsman), and then 10g of an emulsifier TERMUL 200 (an alkylphenol block polyether copolymer emulsifier, Huntsman) and 14g of an agricultural milk # (tristyrylphenol polyoxyethylene polyoxypropylene ether, Switzerland chemical auxiliary agent Co., Ltd., Schott) are added and slowly stirred until the mixture is completely dissolved.
2. Preparation of aqueous phase
4g of n-butanol (Allatin reagent), 0.2g of high-efficiency organic silicon defoamer (ETXP-40, New Material Ltd. left soil, Hangzhou) and 50.8g 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 the Pyridachlorometyl fluorobenzene ether amide microemulsion with the mass content of the active ingredient of 8%.
Formulation example 6: 36% Pyridachlorometyl fluorobenzene ether amide aqueous emulsion
1. Preparation of the oil phase
9g of Pyridachlorometyl technical raw material and 27g of fluorophenylether amide were added to a mixed solvent of 10g of cyclohexanone (an avadin reagent) and 10g of xylene (an avadin reagent), and then 1601# (tristyrylphenol polyoxyethylene polyoxypropylene ether, Switchen Chengxi chemical auxiliary Co., Ltd.) 5g of emulsifier agricultural milk and 3g 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 (Allatin reagent), 0.1g of xanthan gum (Allatin reagent), 0.4g of high-efficiency organic silicon defoamer (ETXP-40, New Material from Hangzhou left Earth Co., Ltd.) and 32.5g of water are uniformly stirred.
3. Blending of pesticide composition aqueous emulsion
Slowly adding the oil phase into the water phase, continuously stirring until the oil phase is completely added, and then performing high shear (8000 rpm) for 15 minutes in a high-speed disperser (trade name: TG25, Germany IKA) to obtain the Pyridachlorometyl-fluorophenylether amide aqueous emulsion with the mass content of the active ingredient of 36%.
Comparative example 1: 40% Pyridachlorometyl suspension
1. Preparation of comminuted slurry
2g of a non-alkylphenol 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 antifoaming agent (ETXP-40, New Material for left soil, Hangzhou Co., Ltd.) were dispersed in 32.7g of water, 40g of a Pyridachlorometyl base crude drug was dispersed therein, and 40g of the Pyridachlorometyl base crude drug was used
Figure BDA0002038783430000081
The glass beads were subjected to wet pulverization for 1.5 hours using a sand mill (YS7142, Shenyang New micro electric machine Mill) to obtain 80g of a 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 pulverized slurry (80 g) and a dispersion medium (20 g) were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, thereby obtaining a pyridachlorometyl suspension having an active ingredient mass content of 40%.
Comparative example 2: 50% fluorobenzene ether amide wettable powder
Adding 50g of fluorobenzene ether amide, 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 (Alisma reagent), 0.5g of xanthan gum (Alisma reagent), 0.2g of organic silicone (trade name: DOW CORNING ANTIFOAM C EMULSION, DOW CORNING) and 100g of kaolin (New left soil material Co., Ltd., Hangzhou) into 100g of fluorobenzene ether amide wettable powder, pre-crushing and uniformly mixing, and then crushing by air flow (model: SJM-100, Kunshanounck machinery Co., Ltd.) to the required particle size (10-15 micrometers) to obtain the fluorobenzene ether amide wettable powder with the effective component mass content of 50%.
Test of field drug effect
And (3) test treatment: three effective ingredient amounts were set for each of the test agents of formulation examples 1 to 3 and the single agents of comparative examples 1 to 2 according to the test design of the test agents in Table 2.
TABLE 2 test design of field drug effect of test agent
Figure BDA0002038783430000091
Setting a cell: each cell area is 66.7m2
The application method comprises the following steps: the medicament is applied at the early stage of powdery mildew of cucumber, and sprayed on the leaf surface, and the spraying amount is mainly no water drops;
the application times are as follows: 3 times, in windy days or in expected 1 hour, the rainfall was 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: the base number was investigated 1 day before the administration of the drug, and the index of disease was investigated 7 days, 14 days and 21 days after the administration of the drug.
The investigation method comprises the following steps: and (4) grading according to the damage symptom degree of the cucumber leaves, taking the cucumber leaves as a unit, sampling five points on the diagonal line of each cell, surveying and connecting 5 plants at each point for 25 plants in total, and recording the total number of plants, the number of diseased plants and the number of disease stages.
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. Grading standard:
level 0: no disease;
level 1: the area of the lesion spots accounts for less than 5% of the area of the whole leaf;
and 3, level: the area of the lesion spots accounts for 6 to 10 percent of the area of the whole leaf;
and 5, stage: the area of the lesion spots accounts for 11 to 20 percent of the area of the whole leaf;
and 7, stage: the area of the lesion spots accounts for 21 to 40 percent of the area of the whole leaf;
and 9, stage: the area of the lesion spots accounts for more than 40 percent of the area of the whole leaf.
And (3) calculating the drug effect:
Figure BDA0002038783430000092
Figure BDA0002038783430000101
in the formula: CK (CK)0-pre-drug disease index of the placebo zone; CK (CK)1-post-drug disease index in the placebo zone;
PT0-pre-drug disease index in the drug treatment area; PT1-post-drug disease index in the drug treatment area.
The results of the tests are detailed in table 3 below.
TABLE 3 preventive effect of different agents against powdery mildew of cucumber
Figure BDA0002038783430000102
As shown in Table 3, the bactericidal composition containing pyridachlorometyl and fluorophenyletheramide has good control effect on cucumber powdery mildew, and the control effect is still more than 89% 21 days after the bactericidal composition is applied, so that the bactericidal composition has a long lasting period. Compared with a single preparation, the bactericidal composition has quick acting performance and lasting effect superior to those of a control single preparation, and can show synergistic interaction after being compounded, so that the administration times can be reduced. In addition, no phytotoxicity of the pesticide composition on cucumbers is found in the application range, which shows that the bactericidal composition is good in safety to crops and can be popularized and applied.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. A germicidal composition, characterized by: the effective components of the bactericidal composition comprise pyridachlorometyl and fluorobenzene ether amide.
2. The germicidal composition of claim 1, wherein: the mass ratio of Pyridachlorometyl to fluorobenzene ether amide is 1-40: 40-1.
3. The germicidal composition of claim 2, wherein: the mass ratio of Pyridachlorometyl to fluorobenzene ether amide is 1-20: 20-1.
4. The germicidal composition of claim 3, wherein: the mass ratio of the pyridachlorometyl to the fluorobenzene ether amide is 1-10: 20-1; further preferably 1-3: 5-1.
5. The germicidal composition of claim 1, wherein: the mass percentage of the pyridachlorometyl and the fluorobenzene ether amide in the bactericidal composition is 1-99%, and the balance is auxiliary materials.
6. The germicidal composition of claim 5, wherein: the mass percentage of the pyridachlorometyl and the fluorobenzene ether amide in the bactericidal composition is 10-90%, and the balance is auxiliary materials.
7. The germicidal composition of claim 6, wherein: the mass percentage of the pyridachlorometyl and the fluorobenzene ether amide in the bactericidal composition is 20-80%, and the balance is auxiliary materials.
8. The use of the fungicidal composition of any one of claims 1 to 7 for the control of powdery mildew of cucumber, rice blast and/or sheath blight.
9. A fungicide, characterized by: comprising the fungicidal composition according to any one of claims 1 to 7.
10. The bactericide as claimed in claim 9, wherein: the bactericide is in the form of any one of missible oil, wettable powder, suspending agent, granules, water dispersible granules, microemulsion, emulsion in water or microcapsules.
CN201910334672.9A 2019-04-24 2019-04-24 Pyridachlorometyl and fluorobenzene ether amide-containing bactericidal composition and application thereof Pending CN111838161A (en)

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