CN107347893A - A kind of bactericidal composition containing propiconazole Yu fluorobenzene ether amide - Google Patents

A kind of bactericidal composition containing propiconazole Yu fluorobenzene ether amide Download PDF

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Publication number
CN107347893A
CN107347893A CN201610308421.XA CN201610308421A CN107347893A CN 107347893 A CN107347893 A CN 107347893A CN 201610308421 A CN201610308421 A CN 201610308421A CN 107347893 A CN107347893 A CN 107347893A
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China
Prior art keywords
propiconazole
ether amide
fluorobenzene ether
bactericidal composition
fluorobenzene
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CN201610308421.XA
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Chinese (zh)
Inventor
葛尧伦
白复芹
司国栋
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Hailir Pesticides and Chemicals Group Co Ltd
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Hailir Pesticides and Chemicals Group Co Ltd
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Priority to CN201610308421.XA priority Critical patent/CN107347893A/en
Publication of CN107347893A publication Critical patent/CN107347893A/en
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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
    • A01N43/64Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647Triazoles; Hydrogenated triazoles
    • A01N43/6531,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
    • 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

Abstract

The present invention relates to a kind of bactericidal composition containing propiconazole Yu fluorobenzene ether amide, its active ingredient is propiconazole and fluorobenzene ether amide binary built.The mass ratio of wherein propiconazole and fluorobenzene ether amide is 1~40: 40~1, active ingredient propiconazole and the quality parts ratio 1%~80% of fluorobenzene ether amide in preparation, remaining is the auxiliary element for allowing to use and receiving in agricultural chemicals, the formulation of bactericidal composition of the present invention is missible oil, suspending agent, wettable powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations, effectively preventing and treating late blight, downy mildew, scab, anthrachose of grape, white rot, spot defoliation, powdery mildew, brown spot, rust, stripe rust, head blight etc., to bitter rot or anthracnose of grape, white rot effect is also fine.

Description

A kind of bactericidal composition containing propiconazole Yu fluorobenzene ether amide
Technical field
The present invention relates to technical field of pesticide combination, more particularly to a kind of sterilization group containing propiconazole Yu fluorobenzene ether amide Compound.
Background technology
Fluorobenzene ether amide (exploitation code name:Y13149 it is) new succinate dehydrogenase inhibitors (SDHI), to rice sheath blight disease With remarkable preventive effect, while have efficient sterilizing active to powdery mildew, the late blight of potato.Fluorobenzene ether amide has Uptake and translocation Property, and there is resistance to rainwater shower, dosage is low, cost is low.
Propiconazole, the entitled propiconazole of English, chemical name is 1- [2- (2,4- dichlorophenyl) -4- propyl group -1,3- bis- Butyl oxide link -2- methyl] -1,2,4 triazole of -1 hydrogen.It is a kind of three series bactericidal agents of absorbability with treatment and protective effect, It can be absorbed by the root, stem, leaf portion of crop, and upward conduction quickly, preventing and treating sac fungus, load can be put forward in crop Disease caused by bacterium and Fungi Imperfecti.Propiconazole is the triazole bactericidal agent belonged in sterol inhibitor, and its mechanism of action is shadow The biosynthesis of sterol is rung, the cell membrane function of pathogen is destroyed, ultimately results in cell death, killed so as to play Bacterium, diseases prevention and the effect of cure the disease.The characteristics of propiconazole has the lasting period long, the longevity of residure was up to one month as long as.
The content of the invention
Corresponding resistance is easily produced in order to avoid fluorobenzene ether amide or propiconazole single dose use, and expands the fungicidal spectrum of medicament, Preferably protection is provided crop.It is an object of the invention to propose a kind of to have good bactericidal effect concurrently with synergistic effect Novel built composition, active ingredient fluorobenzene ether amide are to belong to new benzamides series bactericidal agent, and active ingredient propiconazole is three Azoles fungicide.Fluorobenzene ether amide and the weight of propiconazole ratio are 1~100:1~100, it is more high quality than being 1~80:1~80, most High quality ratio 10~50:10~80, for need to add in the bactericidal composition different surfactants and carrier and by thickener, disappear The auxiliary agent of the compositions such as infusion, sticker, stabilizer, antifreeze, according to the existing processing method of the art be prepared into missible oil, The bactericidal composition of the formulations such as suspending agent, aqueous emulsion, wettable powder.
One of technical scheme, described bactericidal composition are cream preparation, and the percentage by weight of component is:
The specific production stage of the cream preparation is first to add fluorobenzene ether amide and propiconazole in solvent after being completely dissolved to add breast Agent, synergist stir after into homogeneous transparent oily liquids, it is filling, that is, be made and of the present invention contain fluorobenzene ether acyl The cream preparation of the bactericidal composition of amine and propiconazole.
The two of technical scheme, described antimicrobial combination are aqueous emulsion, and the percentage by weight of component is:
The specific production stage of the aqueous emulsion is:Active compound fluorobenzene ether amide and propiconazole, solvent, emulsifying agent, cosolvent are added first Together, make to be dissolved into uniform oil phase;Other auxiliary agents such as part water, antifreeze, antimicrobial are mixed into equal Even aqueous phase;In a kettle while high-speed stirred, oil phase is added into aqueous phase, slowly adds water to phase inversion point, opens cutter High speed shear is carried out, and adds remaining water, shearing about half an hour, the aqueous emulsion of oil-in-water type is formed, is made and contains fluorobenzene ether The water and milk agent formulation of the bactericidal composition of acid amides and propiconazole.
Technical scheme three, described bactericidal composition are suspending agent, and the percentage by weight of component is:
The specific production stage of the suspending agent is first to mix other auxiliary agents, be well mixed through high speed shear, adds active ingredient fluorine Phenylate acid amides and propiconazole, ball milling 2~3 hours in ball mill, make a diameter below 5 μm, be made of the present invention The aqueous suspension formulations of bactericidal composition containing fluorobenzene ether amide and propiconazole.
The four of technical scheme, described bactericidal composition are wettable powders, and the percentage by weight of component is:
The specific production stage of the wettable powder is:By above-mentioned formula by fluorobenzene ether amide, propiconazole and dispersant, wetting agent Mixed with filler, the uniform stirring in stirred tank, be well mixed after airslide disintegrating mill crushes, the present composition can be made Wettable powder.
Described emulsifying agent is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, APES sulfosuccinic acid Ester, styrylphenol polyoxyethylene ether, NPE, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base The mixture of one or more of arbitrary proportions composition in ester, polyoxyethylene aliphatic alcohol ether.
The solvent is dimethylbenzene or biodiesel, toluene, diesel oil, methanol, ethanol, n-butanol, isopropanol, turpentine oil, molten The mixed solvent of one or more arbitrary proportions composition in agent oil, dimethylformamide, dimethyl sulfoxide (DMSO), water equal solvent.
The synergist refers to there is enhancing medicament penetration, gos deep into extended capability, knocks down insect speed, provides the resistance to rainwater of agricultural chemicals Scouring force, so as to improve a kind of safe and environment-friendly, nontoxic, noresidue New-type adjuvant of agricultural insecticide, mite killing, bactericidal effect, It may be selected from organic silicon pesticide synergist ZC-650 or organic silicon pesticide bleeding agent extended pattern Agrowet810c, agricultural organic silicon pesticide Any one in synergist Silwet408, azone.
Described dispersant is selected from polycarboxylate, lignosulfonates, APES formaldehyde condensation products sulfat, alkyl Benzene sulfonic acid calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sulfate, APES, aliphatic amine polyoxyethylene ether, fatty acid polyglycol One or more in oxygen vinyl acetate, glycerine fatty acid ester APEO.
The wetting agent stated is selected from:Lauryl sodium sulfate, DBSA, Nekal BX, moistening bleeding agent F, alkylnaphthalene One or more in sulfonate, polyoxyethylene tri-styryl phosphenylic acid salt, spaonin powder, silkworm excrement, spaonin powder.
The thickener is selected from:Xanthans, hydroxymethyl cellulose, hydroxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, poly- second One or more in enol.
Described antifreeze is selected from:One or more in ethylene glycol, propane diols, glycerine.
Described filler is selected from:In kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate It is one or more.
Described bactericidal composition is mainly used in preventing and treating the various diseases caused by sac fungus, basidiomycetes etc., such as:The downy mildew of vegetables The disease such as disease, powdery mildew, anthracnose, wheat scab, powdery mildew.
The present invention has following features:
1st, double action mechanism, it is not likely to produce drug resistance;
2nd, fungicidal spectrum is expanded, propiconazole has splendid absorbability, and prevention effect increases;
3rd, the lasting period is grown, and the longevity of residure can reach one month or so;
4th, environment friendly agricultural is belonged to, fluorobenzene ether amide and propiconazole belong to the agricultural chemicals to person poultry safety in use range, and it is compounded Preparation high-efficiency low-toxicity, to crop and Environmental security, be advantageous to the sustainable development of agricultural production.
Embodiment:
1 materials and methods
1.1 test material
1.1.1 reagent agent
96% fluorobenzene ether amide active compound, is produced by Jiangsu Heyi Chemical Industry Co., Ltd.;95% propiconazole, Jiangsu bumper harvest agricultural chemicals have Limit company produces;
1.1.2 for examination pathogen
Cucumber powdery mildew's pathogen, separation was not gathered with not applying the cucumber cultivation of fluopicolide and propiconazole and similar medicament from Shandong Shouguang.
1.1.3 for examination cucumber variety
Chang Chun Mi Ci
1.2 test method and Tests of Synergistic Actions
1.2.1 the drug solution preparing of single dose toxicity test
Fluorobenzene ether amide and propiconazole are that solvent dissolves with acetone, are made into 10000 μ g/ml mother liquors, stand-by in 4 DEG C of preservations.
1.2.2 test plant
By the cultivation of susceptible cucumber variety Chang Chun Mi Ci in pot for growing seedlings, it is placed in greenhouse and cultivates, plant grows to three to after four leaf stage, The blade of identical leaf age is gathered, culture and measure for cucumber powdery mildew's pathogen.
1.2.3 the culture of cucumber powdery mildew's pathogen and the preparation of spore suspension
Cucumber powdery mildew's pathogen is cultivated using plants method under conditions of 20 DEG C, 12h alternation of light and darkness, turns to be commissioned to train foster 1 per 30d It is secondary.With the conidium on sterile water elution incidence of leaf during inoculation, it is l × 10 to be configured to spore concentration6Individual/mL suspension.
1.2.4 strains tested sensitivity testing
Toxicity test is carried out using leaf dish moisturizing method.The blade of collection is first prepared into a diameter of 1.5cm leaf dish, it is random mixed It is even, it is respectively placed in the series concentration decoction configured and soaks lh, each 50 leaf dishes of concentration, tests with the place of not adding medicine Manage as blank control, after immersion terminates, leaf is face-up placed on the blotting paper of identical liquor strength wetting, in leaf dish Decoction blot, by the spore suspension l0L prepared be inoculated in leaf dish center, room temperature place 5min after, be placed in 20 DEG C, Cultivated under conditions of 12h alternation of light and darkness, the onset area in leaf dish is measured after 10d, calculates EC50
On the basis of pilot study, toxicity test is carried out to single dose fluorobenzene ether amide and propiconazole respectively with above method, the two EC50Value is respectively 0.9 ㎎/l and 2.8 ㎎/l.
The percentage that leaf dish area is accounted for according to lesion area divides sick level:
0 grade:Scab
1 grade:Lesion area accounts for the 1%~20% of leaf dish area
2 grades:Lesion area accounts for the 21%~50% of leaf dish area
3 grades:Lesion area accounts for more than the 50% of leaf dish area
1.2.2 mixture combination settings
60% fluorobenzene ether amide propiconazole mass ratio is respectively that 5%+55%, 6%+54%, 10%+50%, 15%+45% and 30%+30% are total to 5 mixture combinations.
1.2.3 mixture toxicity test
The toxicity test of mixture is carried out according to mixed ratio with single dose toxicity test method.
According to the abundant methods of Sun Yun by the EC of each processing of measure50Value is converted into actual mixed toxicity index (ATI);According to the proportioning of mixture, Theoretical mixed toxicity index (TTI) is obtained, the co-toxicity coefficient (CTC) of mixture is calculated by following equation.
Single dose toxicity index=(standard agent EC50/ reagent agent EC50)*100
ATI=(standard agent EC50/ reagent agent (mixed) EC50)*100
Toxicity index X B contents (%) in mixed of the TI I=A toxicity index X A in content (%)+B in mixed
CTC=(ATI/TTI) * 100
If co-toxicity coefficient is big by 120, show there is synergistic effect;If being significantly lower than 100 (less than 80), antagonism is shown to be;100~120 Between, it is shown to be summation action
Data are shown in Table 1,2
The virulence of the different ratio fluorobenzene ether amide of table 1 and propiconazole mixture to cucumber powdery mildew's pathogen
The co-toxicity of the fluorobenzene ether amide of table 2 and propiconazole compound to cucumber powdery mildew's pathogen
Test medicine Mass ratio Actual measurement poison refers to Theoretical poison refers to Co-toxicity coefficient Conclusion
Fluorobenzene ether amide (A) 1:0 100 100 / /
Propiconazole (B) 0:1 32.14 32.14 / /
A+B 1:11 25.17 22.68 111.0 It is added
A+B 1:9 27.89 23.36 119.4 It is added
A+B 1:5 36.21 26.07 138.9 Synergy
A+B 1:3 33.76 29.46 114.6 It is added
A+B 1:1 40.36 39.64 101.8 It is added
2 results and analysis
According to bactericide joint toxicity measuring result, fluorobenzene ether amide propiconazole mass ratio is 1:Co-toxicity coefficient when 5 is 138.9, More than 120, synergistic effect is shown as, other are more than 100, show as summation action, it is believed that 1:5 be optimum proportioning.
3 field tests are determined to powdery mildew of cucumber and the prevention effect of Pumpkin powdery mildew
3.1 field tests determine the prevention effect to powdery mildew of cucumber
3.1.1 application method
3.1.2 investigation method
With being experimental field located at the cucumber in Yangling district of Shaanxi Province Li Tai townshiies, investigate per cell at 5 points, investigate 2 plants, is remembered with staging at every Occurring degree is carried, grade scale is as follows:
0 grade:Disease-free spot;
1 grade:Lesion area accounts for less than the 5% of whole leaf area;
3 grades:Lesion area accounts for whole leaf area 6%~10%;
5 grades:Lesion area accounts for the 11%~25% of whole leaf area;
7 grades:Lesion area accounts for the 26%~50% of whole leaf area;
9 grades:Lesion area accounts for more than the 50% of whole leaf area.
3.1.3 control time and number
Experiment is investigated 4 times altogether, i.e., disease index is investigated before medicine, preventive effect investigation in 7 days after the 1st medicine, 7 days and 15 after 2 medicines Its preventive effect is investigated.
3.1.4 drug effect computational methods
Sick leaf rate (the %)=sick number of sheets/investigation total number of sheets × 100
Disease index=∑ (the sick numbers of sheets at different levels × relative value of series)/(investigation total number of sheets × 9) × 100
Prevention effect (%)=(1- (disease index after disease index × treatment region medicine before blank district medicine)/(after blank district medicine Disease index before disease index × treatment region medicine)) × 100
3.1.5 poisoning investigation method
Whether continuous 7d range estimations medicament has poisoning to crop after dispenser.
3.1.6 result of the test and analysis
Table 3 respectively handles the effect of preventing and treating powdery mildew of cucumber
Interpretation of result:
As can be seen from Table 3,60% fluorobenzene ether amide propiconazole SC 1:The effect of 5 mixture combination preventing and treating powdery mildew of cucumber shows Write.Under same 10 grams every mu dosage, the significant effect of complex preparation is better than two kinds of single doses, and its quick-acting and lasting effect all compare Preferably, it is especially the most prominent with lasting effect.Complex preparation prevention effect under the dosage of high concentration is significantly better than under low concentration dosage Effect.The prevention effect of 7 days respectively reaches 72.46% and 77.69% after the 1st, 2 medicine, the holding effect of 15 days after the 2nd medicine Property is more notable, reaches 83.49%.Experiment results proved, 41.7% fluorobenzene ether amide SC single doses positive effect are better than 25% propiconazole EC single doses.15 days after 2nd medicine, the highest preventive effect of 41.7% fluorobenzene ether amide SC single doses is 80.80%, 25% propiconazole EC The highest preventive effect of single dose is 79.08%.Estimated according to field, in the range of test dose, plant growth is normal, each treatment agent Do not occur the poisoning phenomenon to cucumber, it is safe to cucumber to illustrate it.Prevent at the initial stage of a disease or in advance, it is desirable more Preferable prevention effect.
3.2 field tests determine the prevention effect to Pumpkin powdery mildew
3.2.1 application method
3.2.2 investigation method
Experimental field be located in the cucurbita pepo greenhouse in Yangling district of Shaanxi Province Li Tai townshiies, per cell investigate 5 points, every investigate 2 plants, with point Level method records occurring degree, and grade scale is as follows:
0 grade:Disease-free spot;
1 grade:Lesion area accounts for less than the 5% of whole leaf area;
3 grades:Lesion area accounts for whole leaf area 6%~10%;
5 grades:Lesion area accounts for the 11%~25% of whole leaf area;
7 grades:Lesion area accounts for the 26%~50% of whole leaf area;
9 grades:Lesion area accounts for more than the 50% of whole leaf area.
3.2.3 control time and number
Experiment is investigated 4 times altogether, i.e., disease index is investigated before medicine, preventive effect investigation in 7 days after the 1st medicine, 7 days and 14 after 2 medicines Its preventive effect is investigated.
3.2.4 drug effect computational methods
Diseased plant leaf (the %)=sick number of sheets/investigation total number of sheets × 100
Disease index=∑ (the sick numbers of sheets at different levels × relative value of series)/(investigation total number of sheets × 9) × 100
Prevention effect (%)=(1- (disease index after disease index × treatment region medicine before blank district medicine)/(after blank district medicine Disease index before disease index × treatment region medicine)) × 100
3.2.5 poisoning investigation method
Whether continuous 7d range estimations medicament has poisoning to crop after dispenser.
3.2.6 result of the test and analysis
Table 4 respectively handles the effect of preventing and treating Pumpkin powdery mildew
Interpretation of result:
As can be seen from Table 4,60% fluorobenzene ether amide propiconazole SC 1:The effect of 5 mixture combination preventing and treating Pumpkin powdery mildew Significantly.Under same 10 grams every mu dosage, the significant effect of complex preparation is better than two kinds of single doses, and its quick-acting and lasting effect are all It is relatively good, it is especially the most prominent with lasting effect.Complex preparation prevention effect under the dosage of high concentration is significantly better than under low concentration dosage Effect.The prevention effect of 7 days respectively reaches 73.76% and 78.86% after the 1st, 2 medicine, holds within 15 days after the 2nd medicine Effect property is more notable, reaches 83.71%.Experiment results proved, 41.7% fluorobenzene ether amide SC single doses positive effect is better than the 25% the third rings Azoles EC single doses.15 days after 2nd medicine, the highest preventive effect of 41.7% fluorobenzene ether amide SC single doses is 78.07%, 25% propiconazole The highest preventive effect of EC single doses is 72.53%.Estimated according to field, in the range of test dose, plant growth is normal, respectively handles medicine Agent does not occur the poisoning phenomenon to cucurbita pepo, and it is safe to cucurbita pepo to illustrate it.Prevent at the initial stage of a disease or in advance, can use More preferably prevention effect.
In summary, the Bactericidal composite of the invention containing fluorobenzene ether amide and propiconazole, to powdery mildew of cucumber and Pumpkin powdery mildew Have a good prevention effect, and it is to Target crops safety, compared with single dose, bactericidal composition of the present invention have quick-acting it is good, The advantages of lasting period is long, it is not likely to produce poisoning.So research and development and popularization of the invention are of great significance to society's tool.

Claims (4)

  1. A kind of 1. bactericidal composition containing propiconazole Yu fluorobenzene ether amide, it is characterised in that:The active ingredient of the bactericidal composition is Propiconazole and fluorobenzene ether amide binary built, remaining is auxiliary element, wherein active ingredient propiconazole and the matter of fluorobenzene ether amide Amount is than being 1~40: 40~1.
  2. 2. bactericidal composition according to claim 1, it is characterised in that:Propiconazole and the gross weight of fluorobenzene ether amide in the formulation Amount accounts for the 1%~80% of the whole quality of the pharmaceutical preparations.
  3. 3. bactericidal composition according to claim 2, it is characterised in that:Propiconazole and the gross weight of fluorobenzene ether amide in the formulation Amount accounts for the 5%~50% of the whole quality of the pharmaceutical preparations.
  4. 4. according to the bactericidal composition described in claim 1 or 2 or 3, it is characterised in that:The formulation of the bactericidal composition be missible oil, Suspending agent, wettable powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.
CN201610308421.XA 2016-05-10 2016-05-10 A kind of bactericidal composition containing propiconazole Yu fluorobenzene ether amide Pending CN107347893A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113180037A (en) * 2020-01-14 2021-07-30 东莞市东阳光菌阳氢专利农药有限公司 Environment-friendly type fluophenyl ether amide missible oil preparation and preparation method and application thereof
CN114097795A (en) * 2020-08-26 2022-03-01 山东省联合农药工业有限公司 Bactericidal composition containing pyrazole amide compounds and triazole bactericide

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113180037A (en) * 2020-01-14 2021-07-30 东莞市东阳光菌阳氢专利农药有限公司 Environment-friendly type fluophenyl ether amide missible oil preparation and preparation method and application thereof
CN113180037B (en) * 2020-01-14 2024-02-02 东莞市东阳光菌阳氢专利农药有限公司 Environment-friendly fluorophenylether amide emulsifiable concentrate preparation as well as preparation method and application thereof
CN114097795A (en) * 2020-08-26 2022-03-01 山东省联合农药工业有限公司 Bactericidal composition containing pyrazole amide compounds and triazole bactericide

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