CN107467022A - A kind of bactericidal composition containing bromothalonil Yu fluorine azoles bacterium aniline - Google Patents

A kind of bactericidal composition containing bromothalonil Yu fluorine azoles bacterium aniline Download PDF

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Publication number
CN107467022A
CN107467022A CN201710700351.7A CN201710700351A CN107467022A CN 107467022 A CN107467022 A CN 107467022A CN 201710700351 A CN201710700351 A CN 201710700351A CN 107467022 A CN107467022 A CN 107467022A
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China
Prior art keywords
bromothalonil
azoles bacterium
fluorine azoles
bacterium aniline
bactericidal composition
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CN201710700351.7A
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Inventor
葛家成
葛尧伦
李晓静
王金凤
孙晓培
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Qingdao Audis Bio & Tech Co Ltd
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Qingdao Audis Bio & Tech Co Ltd
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Priority to CN201710700351.7A priority Critical patent/CN107467022A/en
Publication of CN107467022A publication Critical patent/CN107467022A/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
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/34Nitriles
    • 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

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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The present invention relates to a kind of bactericidal composition containing bromothalonil Yu fluorine azoles bacterium aniline, its active ingredient is bromothalonil and fluorine azoles bacterium aniline binary built.The mass ratio of wherein bromothalonil and fluorine azoles bacterium aniline is 1~25: 25~1, the quality parts ratio 1%~80% of active ingredient bromothalonil and fluorine azoles bacterium aniline in preparation, remaining is the auxiliary element for allowing to use and receiving in agricultural chemicals, and the formulation of bactericidal composition of the present invention is missible oil, suspending agent, wettable powder, aqua, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.It is mainly used in preventing and treating the diseases such as cucumber, downy mildew of garpe, gray mold.

Description

A kind of bactericidal composition containing bromothalonil Yu fluorine azoles bacterium aniline
Technical field
The present invention relates to technical field of pesticide combination, more particularly to a kind of sterilization containing bromothalonil Yu fluorine azoles bacterium aniline Composition.
Background technology
Bromothalonil is a kind of wide spectrum, bactericide efficiently, less toxic, can suppress and root out fungi, the growth of bacterium, algae, There is preferable prevention effect to corps diseases, have special efficacy to anthracnose.It is widely used in fruit tree, grape, vegetables, cotton, flower The various crops such as life, watermelon, tobacco, tea tree, flowers, preventing and treating anthracnose, scab, shot hole, powdery mildew, rust, damping-off, A variety of fungoids such as samping off, rhizome maize ear rot, canker, bacterial wilt, angular leaf spot, bacteroidal disease.Application mode is flexible, leaf Face spraying, seed treatment and soil pouring root, all show preferable preventive effect.
Fluorine azoles bacterium aniline (penflufen) is succinate dehydrogenase inhibitors (SDHI) series bactericidal agent, has interior suction, prevention concurrently And therapeutic action, lasting period length.It is mainly used as sterile seeds inorganic agent, and after seed treatment, medicament is through penetrating into germination Seed, conducted by the xylem of shoot to whole plant, so as to protect the seedling of growth at high level.Under the product low dosage Disease caused by the pathogens such as basidiomycetes and sac fungus can be prevented and treated extensively.
It is the maximally efficient means of controlling plant diseases using chemical agent.But apply single long-term continuous high dose Chemical bactericide, easily cause the problems such as residual of medicament, environmental pollution and resistance to resistance to the action of a drug fungi are developed.Rational chemistry Bactericide compounded or mixture have expand fungicidal spectrum, improve prevention effect, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, Reduce residual, delay the positive feature such as Antifungal resistance and drug-fast generation and development, bactericide compounded is to solve above-mentioned ask One of maximally efficient method of topic.Develop new product bactericide price is constantly soaring, and by contrast, exploitation with research efficiently, Low toxicity, the compounding of low-residual with mixture has small investment, the lead time is short and is paid attention to both at home and abroad, one after another increasing develop Dynamics.We screen and on the basis of field test, filter out bromothalonil and compounded with fluorine azoles bacterium aniline indoors, have bright Aobvious synergistic effect.And people there is no to report at present on bromothalonil and the bactericidal composition of the compounding of fluorine azoles bacterium aniline and application Cross.
The content of the invention
Based on case above, present invention aims at provide a kind of new and effective pesticide sterilizing composite.It is mainly used in Prevent and treat the diseases such as cucumber, downy mildew of garpe, gray mold.
Technical scheme of the present invention is realized by following measures:
A kind of bactericidal composition containing bromothalonil Yu fluorine azoles bacterium aniline, the active ingredient bromothalonil of the bactericidal composition with Fluorine azoles bacterium aniline two-spot compounds, and remaining is auxiliary element.Active ingredient bromothalonil and fluorine azoles bacterium in wherein described bactericidal composition The mass ratio of aniline is 1~25: 25~1, and described bactericidal composition of the present invention is through toxicity test experimental verification, bromothalonil and fluorine When the mass ratio of azoles bacterium aniline is 1~10: 10~1, synergistic effect is preferable.
The formulations of pesticide that described bactericidal composition of the present invention can be prepared are missible oil, suspending agent, wettable powder, water Agent, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.Wherein active ingredient bromothalonil exists with fluorine azoles bacterium aniline Gross mass in preparation accounts for the 1%~80% of the whole quality of the pharmaceutical preparations, wherein when accounting for 10%~60%, toxicity and residual reach preferable Balance, cost is relatively low.
The specific embodiment for the formulations of pesticide that bactericidal composition of the present invention is configured to is as follows:
Described bactericidal composition is cream preparation, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium aniline 1 ~25 parts;10~30 parts of conventional emulsifier;20~50 parts of Conventional solvents;Conventional 1~5 part of synergist.The cream preparation it is specific Production stage is first by active ingredient bromothalonil with adding emulsifying agent, synergy after being completely dissolved in fluorine azoles bacterium aniline addition solvent Agent stir after into transparent and homogeneous oily liquids, it is filling, you can the cream preparation of the present composition is made.
Described bactericidal composition is suspending agent, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium aniline 1~ 25 parts;5~20 parts of dispersant;1~5 part of antifreezing agent;0.1~2 part of thickener;0.1~0.8 part of defoamer;Penetrating agent 0~10 Part;0.1~5 part of pH value regulator;Water, surplus.The specific production stage of the suspending agent is first mixes other auxiliary agents, through at a high speed Shear-mixed is uniform, adds active ingredient bromothalonil and fluorine azoles bacterium aniline, abrading-ball 2~3 hours in ball crusher, makes a diameter equal In below 5mm, you can the aqueous suspension formulations of the present composition are made.
Described bactericidal composition is wettable powder, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium benzene 1~25 part of amine;3~10 parts of dispersant;1~5 part of wetting agent;Filler, surplus.The specific production stage of the wettable powder is: Active ingredient bromothalonil is mixed with fluorine azoles bacterium aniline and dispersant, wetting agent and filler by above-mentioned formula, in stirred tank Uniform stirring, remixed after airslide disintegrating mill uniformly, you can the wettable powder of the present composition is made.
Described bactericidal composition is water dispersible granules, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium benzene 1~25 part of amine;3~10 parts of dispersant;1~10 part of wetting agent;1~5 part of disintegrant;Filler, surplus.The tool of the water dispersible granules Body production stage is:By above-mentioned formula by active ingredient bromothalonil and fluorine azoles bacterium aniline and dispersant, wetting agent, disintegrant and Filler is well mixed, and is crushed with micro jet, through mediating, be then granulated in addition fluidized-bed granulation dryer, Through sampling analysis after dry, screening, you can the water dispersible granules of the present composition are made.
Described bactericidal composition is aqueous emulsion, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium aniline 1~ 25 parts;3~30 parts of emulsifying agent;5~15 parts of solvent;2~15 parts of stabilizer;1~5 part of antifreezing agent;0.1~8 part of defoamer;Thickening 0.2~2 part of agent;Water, surplus.The specific production stage of the aqueous emulsion is:First by bromothalonil and fluorine azoles bacterium aniline, solvent and breast Agent, cosolvent are added together, and make to be dissolved into uniform oil phase;By other agricultural chemicals such as part water, antifreeze, antimicrobial Auxiliary agent mixes into uniform aqueous phase;Oil phase is added into aqueous phase while high-speed stirred in a kettle, slowly plus water is straight To phase inversion point is reached, open cutter and carry out high speed shear, and add remaining water, shearing about half an hour, form oil-in-water type Aqueous emulsion, you can the aqueous emulsion of the present composition is made.
Described bactericidal composition is microemulsion, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium aniline 1~ 25 parts;10~30 parts of emulsifying agent, 1~8 part of antifreezing agent, 0.5~10 part of stabilizer, 20~50 parts of Conventional solvents cosolvent.By bromine Bacterium nitrile is completely dissolved with fluorine azoles bacterium aniline with cosolvent, adds the other compositions such as emulsifying agent, antifreezing agent, stabilizer, uniformly mixed Close, be eventually adding water, microemulsion can be made into after being sufficiently stirred.
Described bactericidal composition is granule, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium aniline 1~ 25 parts;1~10 part of wetting dispersing agent;0.1~5 part of thickener;0.1~5 part of defoamer;Castor oil, surplus are supplied.Will effectively into Divide each component such as bromothalonil and fluorine azoles bacterium aniline, dispersant, stabilizer, defoamer and solvent to be mixed in the ratio of formula, be put into After being ground in sand milling kettle, it is sent into mixing in mixer for well-distribution and gets product.
Described bactericidal composition is aqua, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium aniline 1~25 Part;0.1~30 part of wetting dispersing agent;2~8 parts of antifreezing agent;0.1~1 part of defoamer;0.1~3 part of thickener;Spreader-sticker 5~15 Part;Water, surplus are supplied.Active ingredient bromothalonil is completely dissolved with fluorine azoles bacterium aniline, with cosolvent, dispersant is added, prevents Freeze the other compositions such as agent, defoamer, uniformly mixing, is eventually adding water, after being sufficiently stirred, you can obtain finished product.
Described bactericidal composition is microcapsule formulations, and the mass fraction of component is:1~25 part of bromothalonil;Fluorine azoles bacterium aniline 1 ~25 parts;5~20 parts of urea;5~20 parts of formaldehyde;5~20 parts of emulsifying dispersant;1~5 part of antifreezing agent;0.1~2 part of thickener; 0.1~0.8 part of defoamer;Water, surplus.Urea and formaldehyde (the amount ratio of material are added in the three-necked flask equipped with agitating device About l:1.5~2.0) pH value for, adjusting solution with sodium hydroxide solution then heats to 70~80 DEG C, instead to 8~9 or so The urea resin prepolymer that should be stablized.A certain amount of bromothalonil is taken to be dissolved in fluorine azoles bacterium aniline in hexamethylene, and in solution Middle addition emulsifying dispersant, with being stirred vigorously, it is made into using the aqueous solution containing emulsifying dispersant as the stable breast of the O/W types of aqueous phase Liquid.Above-mentioned urea resin prepolymer is added in emulsion, pH value is adjusted, polymerisation occurs under acid catalysed conditions, makes oil Phase material is wrapped, and forms microcapsule granule.Slowly heating, solidification, temperature control is at 40~50 DEG C, hardening time 1h. Selection adds appropriate auxiliary agent, you can the microcapsules that must stablize.
Wherein above-described emulsifying agent is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkyl phenol polyoxy Ethene ether sulfosuccinates, styrylphenol polyoxyethylene ether, NPE, castor oil polyoxyethylene ether, Any one of aliphatic acid polyethenoxy base ester, polyoxyethylene aliphatic alcohol ether or more than one any mixtures than composition.
Described solvent is dimethylbenzene or biodiesel, toluene, diesel oil, methanol, ethanol, n-butanol, isopropanol, rosin-based Vegetable oil code name is ND-45, solvent naphtha, dimethylformamide, dimethyl sulfoxide (DMSO), and the one or more in water equal solvent are appointed Anticipate than the mixture of composition.
Described dispersant is LG-3, GY-D1252, GY-D1256, SNWGF-01 selected from polycarboxylate code name, lignin Sulfonate code name is 201107,201108, APES methyl ether condensate sulfate, alkylsulfonate calcium salt, naphthalene Sulfonic formaldehyde condensation compound sodium salt, APES, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, glyceride One or more of fat acid ester polyoxyethylene ether.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, moistens bleeding agent F, Alkylbenzenesulfonate polyoxyethylene triphen phosphenylic acid salt dimly, spaonin powder, silkworm excrement, the one or more in spaonin powder.
Described disintegrant is selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, in sodium acid carbonate It is one or more.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, It is one or more in polyvinyl alcohol.
Described stabilizer is selected from sodium citrate, one kind in resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, the one or more in glycerine.
Described defoamer is selected from silicone oil, silicone compound, C10-20Saturated fat acids compound, C8-10Fatty alcohol It is one or more.
Described filler is selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, in precipitated calcium carbonate One or more.
The present invention has obvious synergistic effect using bromothalonil and composite bactericide of the fluorine azoles bacterium aniline as active ingredient, prolongs The slow drug-fast generation in key, and production cost and use cost are reduced into, it is mainly used in preventing and treating cucumber, downy mildew of garpe, ash The diseases such as mildew.
Embodiment
To make technical scheme, purpose and advantage are more clearly understood, present invention specific examples below Illustrate, but the present invention is not limited to these examples.The effect experiment of the present invention uses indoor biometricses and field test phase With reference to mode, unless otherwise instructed, ratio mentioned below is all quality parts ratio.
Embodiment:Bromothalonil is tested with fluorine azoles bacterium aniline different ratio co-toxicity.
1.1 reagent agent
85% fluorine azoles bacterium aniline active compound, 90% bromothalonil active compound, above-mentioned active compound is by extra large rel medicine company limited company Research and development department provides.
1.2 experiment targets
From Shandong Shouguang never applied bromothalonil and the cucumber of fluorine azoles bacterium aniline and same type it is potted plant gather and separate, supply Try cucumber variety:Chang Chun Mi Ci.
1.3 test method
1.3.1 medicament is prepared
Acetone solution active compound is first used, two appropriate active compounds are made into by several different ratios according to the result of preliminary experiment, It is stand-by that each processing is diluted to several concentration gradients respectively with acetone again.
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 four leaves After phase, the blade of identical leaf age is gathered, culture and measure for gray mold of cucumber germ.
1.3.2 the culture of gray mold of cucumber germ and the preparation of spore suspension
Gray mold of cucumber germ is cultivated using plants method under conditions of 20 DEG C, 12h alternation of light and darkness, turns generation per 30d Culture 1 time.With the conidium on sterile water elution incidence of leaf during inoculation, it is l × 10 to be configured to spore concentration6Individual/mL's Suspension.
1.3.3 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, at random Mix, be respectively placed in the series concentration decoction configured and soak lh, each 25 leaf dishes of concentration, test 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, 12h Cultivated under conditions of alternation of light and darkness, the onset area in leaf dish is measured after 10d, calculates EC50
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 mixture Proportioning, obtain theoretical mixed toxicity index (TTI), the co-toxicity coefficient (CTC) of mixture 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; Between 100~120, summation action is shown to be.
2.1 toxicity test results
Toxicity test of the fluorine azoles bacterium aniline of table 1 with bromothalonil to gray mold of cucumber
As can be seen from the table, the result of the test of different proportion proportioning shows, dilutes equal table respectively in active ingredient ratio Reveal stronger synergistic effect, wherein using bromothalonil and fluorine azoles bacterium aniline as 1:10~10:Synergistic effect good suggestion pair when 1 Suitable proportion 1:10~10:1 or so mixture preparation carries out further field control effectiveness test, to evaluate its field practical application effect Fruit.
3. field test prevents and treats cucumber downy mildew
3.1 test method
Twice, equivalent clear water is sprayed in check plot for dispenser altogether for experiment.When making up a prescription, after first medicament is fully dissolved with a small amount of water, then Add suitable quantity of water and carry out complete stool spraying treatment, even spraying.Using power driven sprayer during spray, operating pressure is 0.3~ 0.4MPa, shower nozzle aperture 1.3mm.Cell spouting liquid is 40~50kg/667m2, continuous dispenser twice, 10 days intervals, by medicine Liquid uniformly sprays application to crop complete stool.
3.2 investigation method
Shandong Shouguang is experimental field located at, the plastic tent cucumber for selecting natural occurrence is experimental field, and soil fertility is medium, irrigation and drainage side Just.Using bilinear sampling method, take per cell at 5 points, look into 5 caves, and 2 blades in every plant of fixed middle part carry out fixed point inspection during investigation at every Look into.
It is classified according to cucumber downy mildew grade scale, record total strain number, diseased plant number, severity, calculating diseased plant rate, Disease index and preventive effect.
Cucumber downy mildew grade scale is
0 grade:Blade disease-free spot;
1 grade:Lesion area accounts for less than the 5% of whole leaf area;
3 grades:Lesion area accounts for the 6%~10% of whole leaf area;
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.
Experiment is investigated 3 times altogether, i.e., disease index is investigated before medicine, preventive effect investigation in 10 days after the 1st medicine, after 2 medicines 10 days and Preventive effect investigation in 20 days.
3.3 poisoning are investigated
Whether continuous 7d range estimations medicament has poisoning to crop after dispenser.
3.4 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)/(blank pair According to disease index before disease index after area's medicine × treatment region medicine)) × 100.
3.4 field control effectiveness test result of the tests
2 each test medicine of table prevents and treats the experiment effect of cucumber downy mildew
As shown in Table 2, bromothalonil combines the effect for preventing and treating cucumber downy mildew with fluorine azoles bacterium aniline mixture than more significant, compounding The significant effect of preparation is better than two kinds of single doses, not only significantly improves the prevention effect for downy mildew, and further extend Its lasting period, and produced under the poisoning observation of continuous 7 days without poisoning.
Interpretation of result:
In summary, the bactericidal composition of the invention containing bromothalonil Yu fluorine azoles bacterium aniline, to cucumber downy mildew, gray mold There is good prevention effect, and it is safe to Target crops.Complex preparation not only increases preventive effect, and expands fungicidal spectrum, Use range is widened, reduces cost, multiple diseases are played a part of with a medicine is simultaneous to be controlled, mitigates manpower and materials, improves productivity effect. So the invention of this complex preparation is of great significance with promoting to society's tool.

Claims (4)

  1. A kind of 1. bactericidal composition containing bromothalonil Yu fluorine azoles bacterium aniline, it is characterised in that:The bactericidal composition it is effective into It is divided into bromothalonil and fluorine azoles bacterium aniline binary built, remaining is auxiliary element, wherein active ingredient bromothalonil and fluorine azoles bacterium aniline Mass ratio be 1~25: 25~1.
  2. 2. bactericidal composition according to claim 1, it is characterised in that:Bromothalonil and fluorine azoles bacterium aniline in the formulation total Weight 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:Bromothalonil and fluorine azoles bacterium aniline in the formulation total Weight accounts for the 5%~60% 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 is breast Oil, suspending agent, aqua, wettable powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.
CN201710700351.7A 2017-08-16 2017-08-16 A kind of bactericidal composition containing bromothalonil Yu fluorine azoles bacterium aniline Pending CN107467022A (en)

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Application publication date: 20171215