CN103168780A - Bactericidal composition containing fluopicolide and metrafenone - Google Patents
Bactericidal composition containing fluopicolide and metrafenone Download PDFInfo
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- CN103168780A CN103168780A CN2013100872744A CN201310087274A CN103168780A CN 103168780 A CN103168780 A CN 103168780A CN 2013100872744 A CN2013100872744 A CN 2013100872744A CN 201310087274 A CN201310087274 A CN 201310087274A CN 103168780 A CN103168780 A CN 103168780A
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- acid amides
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Abstract
The invention relates to a bactericidal composition containing fluopicolide and metrafenone. The active ingredients fluopicolide and metrafenone are compounded with each other, wherein the mass ratio of fluopicolide to metrafenone is (1-40): (40-1); the mass fraction of the active ingredients fluopicolide and metrafenone in the preparation is 1-80%, and the other ingredients of the preparation are auxiliaries allowed to be used and accepted in pesticides. The form of the bactericidal composition provided by the invention is missible oil, suspending agent, wettable powder, water dispersible granule, emulsion in water and microemulsion; and the bactericidal composition is mainly used for preventing and controlling grape downy mildew, late blight and various powdery mildews.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of bactericidal composition that contains fluorine pyridine bacterium acid amides and metrafenone.
Background technology
Fluopicolide is a kind of novel amide-type systemic fungicide of Beyer Co., Ltd's exploitation; Be mainly used in preventing and treating the microbial disease of Oomycete cause of disease as downy mildew of garpe and late blight etc.Fluopicolide not only has unique mode of action, with other series bactericidal agent, without cross resistance, and has good lasting effect.The chemistry of fluopicolide is called the chloro-5-of the chloro-N-{[3-of 2,6-bis-(trifluoromethyl)-2-pyridine] methyl } benzamide, its chemical structural formula is
.
Metrafenone is the new type bactericide of a Benzophenones of BASF AG's exploitation, and all kinds of powdery mildews are had to good control efficiency.The chemical name of metrafenone: (the bromo-6-methoxyl group of 3--2-aminomethyl phenyl)-(2,3,4-trimethoxy-6-aminomethyl phenyl) ketone, its blossom fall structural formula is
.
Using chemical agent is the most effectively means of controlling plant diseases.But long-term use single chemical bactericide continuously high dose, easily cause the problems such as residual, the environmental pollution of medicament and anti-pesticide resistance fungi development.Reasonably chemical bactericide is composite or be mixed and have the expansion fungicidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay Antifungal resistance and the positive characteristics such as drug-fast generation and development, bactericide compounded is one of the effective method the most addressed the above problem.Exploitation new product bactericide price is constantly soaring, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite be mixed there is small investment, the lead time is short and be subject to domestic and international attention, the numerous and confused dynamics that develops that strengthens.We filter out fluorine pyridine bacterium acid amides and metrafenone and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And there is no at present the people about the composite bactericidal composition of fluorine pyridine bacterium acid amides and metrafenone and application reported.
Summary of the invention
Based on above situation, the object of the invention is to provide a kind of new and effective pesticide sterilizing composite.Be mainly used in preventing and treating downy mildew of garpe, late blight and all kinds of powdery mildew.
Technical scheme of the present invention realizes by following measures:
A kind of fluorine pyridine bacterium acid amides and metrafenone bactericidal composition of containing, active ingredient fluorine pyridine bacterium acid amides and two yuan of the metrafenones of this bactericidal composition are composite, and all the other are auxiliary element.In wherein said Pesticidal combination, the mass ratio of active ingredient fluorine pyridine bacterium acid amides and metrafenone is 1～40: 40～1, described bactericidal composition of the present invention is through the toxicity test experimental verification, the mass ratio of fluorine pyridine bacterium acid amides and metrafenone is 1～40: 40～1 o'clock, and synergistic effect is better.
The formulations of pesticide that described bactericidal composition of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.Wherein active ingredient fluorine pyridine bacterium acid amides and the gross mass of metrafenone in preparation account for 1%～80% of the whole quality of the pharmaceutical preparations, while wherein accounting for 15%～50%, and toxicity and the residual balance preferably that reaches, cost is also lower.
The specific embodiments of the formulations of pesticide that bactericidal composition of the present invention is mixed with is as follows:
Described bactericidal composition is cream preparation, and the mass fraction of component is: 1～40 part of fluorine pyridine bacterium acid amides; 1～40 part of metrafenone; 10～30 parts of conventional emulsifiers; 20～50 parts of conventional solvents; 1～5 part of conventional synergist.The concrete production stage of this cream preparation adds emulsifier, the synergist rear oily liquids that becomes transparent and homogeneous that stirs again for first active ingredient fluorine pyridine bacterium acid amides and metrafenone being added in solvent after dissolving fully, filling, can be made into the cream preparation of the present composition.
Described bactericidal composition is suspending agent, and the mass fraction of component is: 1～40 part of fluorine pyridine bacterium acid amides; 1～40 part of metrafenone; 5～20 parts of dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; 0～10 part of penetrating agent; 0.1～5 part of pH value conditioning agent; Water, surplus.The concrete production stage of this suspending agent is for first mixing other auxiliary agents, mix through high speed shear, add active ingredient fluorine pyridine bacterium acid amides and metrafenone, in ball crusher, abrading-ball is 2～3 hours, make a diameter all below 5mm, can be made into the suspending agent preparation of the present composition.
Described bactericidal composition is wetting powder, and the mass fraction of component is: 1～40 part of fluorine pyridine bacterium acid amides; 1～40 part of metrafenone; 3～10 parts of dispersants; 1～5 part of wetting agent; Filler, surplus.The concrete production stage of this wetting powder is: by above-mentioned formula, active ingredient fluorine pyridine bacterium acid amides is mixed with metrafenone and dispersant, wetting agent and filler, uniform stirring in stirred tank, mixing after airslide disintegrating mill, can be made into the wetting powder of the present composition.
Described bactericidal composition is water dispersible granules, and the mass fraction of component is: 1～40 part of fluorine pyridine bacterium acid amides; 1～40 part of metrafenone; 3～10 parts of dispersants; 1～10 part of wetting agent; 1～5 part of disintegrant; Filler, surplus.The concrete production stage of this water dispersible granules is: by above-mentioned formula, active ingredient fluorine pyridine bacterium acid amides is mixed with metrafenone and dispersant, wetting agent, disintegrant and filler, with micro jet, pulverize, through mediating, then add in the fluidized bed prilling dryer and carry out granulation, drying, screening by sample analysis, can be made into the water dispersible granules of the present composition.
Described bactericidal composition is aqueous emulsion, and the mass fraction of component is: 1～40 part of fluorine pyridine bacterium acid amides; 1～40 part of metrafenone; 3～30 parts of emulsifier; 5～15 parts of solvents; 2～15 parts of stabilizing agents; 1～5 part of antifreezing agent; 0.1～8 part of defoamer; 0.2～2 part of thickener; Water, surplus.The concrete production stage of this aqueous emulsion is: at first fluorine pyridine bacterium acid amides and metrafenone, solvent and emulsifier, cosolvent are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added to water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type, can be made into the aqueous emulsion of the present composition.
Described bactericidal composition is microemulsion, and the mass fraction of component is: 1～40 part of fluorine pyridine bacterium acid amides; 1～40 part of metrafenone; 10～30 parts of emulsifier, 1～8 part of antifreezing agent, 0.5～10 part of stabilizing agent, 20～50 parts of conventional solvent cosolvents.Fluorine pyridine bacterium acid amides and metrafenone are dissolved fully with cosolvent, then add other compositions such as emulsifier, antifreezing agent stabilizing agent, evenly mix, finally add water, after fully stirring, can be made into microemulsion.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, the alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any or more than one any mixtures than forming in polyoxyethylene aliphatic alcohol ether.
Described solvent is dimethylbenzene or biodiesel, toluene, and diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in the water equal solvent are arbitrarily than the mixture formed.
Described dispersant is selected from polycarboxylate, lignosulfonates, alkylphenol polyoxyethylene methyl ether condensate sulfate, the alkylsulfonate calcium salt, the naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, one or more in the fatty acid glyceride APEO.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, and Nekal BX, moistening bleeding agent F, alkylbenzenesulfonate polyoxyethylene triphen is phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in the soapberry powder.
Described disintegrant is selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, one or more in sodium bicarbonate.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in polyvinyl alcohol one or more.
Described stabilizing agent is selected from sodium citrate, a kind of in resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, one or more in glycerine.
Described defoamer is selected from silicone oil, silicone compound, C
10-20the saturated fat acid compounds, C
8-10one or more of fatty alcohol.
Described filler is selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, one or more in precipitated calcium carbonate.
The present invention be take the composite bactericide that fluorine pyridine bacterium acid amides and metrafenone be active ingredient and is had obvious synergistic effect, delays the drug-fast generation in key, and has reduced to become to produce cost and use cost, can be used for the improvement of resistance disease.Be mainly used in preventing and treating downy mildew of garpe, late blight and all kinds of powdery mildew.
Embodiment
For making technical scheme of the present invention, purpose and advantage are clearer, and the present invention describes with following specific embodiment, but the present invention is not limited to these examples.The mode that effect experiment of the present invention adopts indoor biometrics and field trial to combine, if no special instructions, the ratio of below mentioning is all ratio of quality and the number of copies.
Embodiment: fluorine pyridine bacterium acid amides proportioning co-toxicity experiments different from metrafenone.
1.1 reagent agent
The former medicine of 96% tiadinil, the former medicine of 95% alkene oxime amine, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Never executed fluorine pyridine bacterium acid amides and metrafenone from Shouguang, Shandong and cucumber of the same type gathers and separates potted plantly, for the examination cucumber variety: Chang Chun Mi Ci.
1.3 test method
1.3.1 medicament preparation
First use the former medicine of acetone solution, according to the result of preliminary experiment, two appropriate former medicines are made into to different proportionings, then it is stand-by with acetone, each processing to be diluted to respectively to some concentration gradients.
Susceptible cucumber variety Chang Chun Mi Ci cultivation, in pot for growing seedlings, is placed in to greenhouse and cultivates, and plant grows to three to four leaf after dates, gathers the blade of identical leaf age, for cultivation and the mensuration of powdery mildew of cucumber bacterium.
1.3.2 the cultivation of powdery mildew of cucumber bacterium and the preparation of spore suspension
The powdery mildew of cucumber bacterium adopts the plants method to cultivate under 20 ℃, the condition of 12h alternation of light and darkness, and every 30 d turn culture 1 time.During inoculation, with the conidium on sterile water wash-out incidence of leaf, being mixed with spore concentration is l * 10
6the suspension of individual/mL.
1.3.3 strains tested sensitivity testing
Adopt leaf dish moisturizing method to carry out toxicity test.First the blade of collection is prepared into to the leaf dish that diameter is 1.5cm, mix at random, be placed in respectively the series concentration liquid configured and soak lh, 50 leaf dishes of each concentration, test is with the blank that is treated to of adding medicine not, after soaking end, leaf faces up and puts on the blotting paper wetting in identical liquor strength, liquid on the leaf dish is blotted, the spore suspension l0L prepared is inoculated in to leaf dish central authorities, after room temperature is placed 5 min, is placed under 20 ℃, the condition of 1 2h alternation of light and darkness and cultivates, measure the onset area on the leaf dish after 10d, calculate EC
50.
On the basis of preliminary experiment, respectively single dose fluorine pyridine bacterium acid amides and metrafenone are carried out to toxicity test in order to upper method, the two EC
50value is respectively 8.69 ㎎/l and 8.26 ㎎/l.
The percentage that accounts for the leaf disc area according to lesion area is divided sick level
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area.
1.3.4 mixture toxicity test and interpretation of result
Carry out the toxicity test of mixture according to mixed ratio by single dose toxicity test method.
If contrast lethality<5%, do not proofread and correct, the contrast lethality, between 5%-20%, is proofreaied and correct by formula 2, the contrast lethality > 20%, test need be reformed.
The logarithm value of drug concentration (mg/L) of take is independent variable x, and the probability value of corrected mortality of take is dependent variable y, sets up respectively the virulence regression equation formula, adopts DPS software to calculate the EC of single dose and each proportioning mixture
50calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.Co-toxicity coefficient CTC, computing formula is as follows: (the fluorine pyridine bacterium acid amides of take is the standard medicament, and its toxicity index is 100):
The EC of the toxicity index of metrafenone (TI)=fluorine pyridine bacterium acid amides
50the EC of/metrafenone
50* 100
The EC of the true toxicity index (ATI) of M=fluorine pyridine bacterium acid amides
50the EC of/M
50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=fluorine pyridine bacterium acid amides * P fluorine pyridine bacterium acid amides+metrafenone * P metrafenone
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In formula:
M is fluorine pyridine bacterium acid amides and the mixture of the different proportionings of metrafenone
P fluorine pyridine bacterium acid amides is fluorine pyridine bacterium acid amides shared ratio in mixture
The P metrafenone is metrafenone shared ratio in mixture.
2.1 toxicity test result
Table 1 fluorine pyridine bacterium acid amides and the metrafenone toxicity test to powdery mildew of cucumber
As can be seen from the table, the result of the test of different proportion proportioning shows, dilute respectively and all show stronger synergistic effect in the active ingredient ratio, wherein take fluorine pyridine bacterium acid amides: metrafenone as 1:20～20:1 the time the good suggestion of synergistic effect suitable proportion 1:20～20:1 left and right mixture preparation is carried out to further field control effectiveness test, to estimate its field practical application effect.
3 field trials are prevented and treated powdery mildew of cucumber, the experimental result of downy mildew of garpe
3.1 field trial is prevented and treated powdery mildew of cucumber
3.1.1 test method
Test is at 4 points of Pingdu City cucumber Di，Mei community, Shandong investigation, and every some investigation 2 strains, put down in writing occurring degree by staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area.
3.1.2 control time and number of times
Test is investigated 4 times altogether, and radix investigation before medicine is investigated after 7 days, 7 days for the second time and medicine after medicine for the first time in 15 days.
3.1.3 drug effect computational methods
Sick leaf rate (%)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(disease index after disease index before 1-(blank district medicine * treatment region medicine)/(disease index before disease index after blank district medicine * treatment region medicine)) * 100.
3.1.4 poisoning investigation method
After dispenser, whether continuous 15d range estimation medicament has poisoning to crop.
3.1.5 result of the test and analysis
Each processes the effect of preventing and treating powdery mildew of cucumber.(table 2)
Each processes the effect of preventing and treating powdery mildew of cucumber table 2
48% fluorine pyridine bacterium acid amides as shown in Table 2: metrafenone with 24:24 ratio composite bactericide for powdery mildew of cucumber control successful higher than fluopicolide and metrafenone single dose, bactericidal effect increases progressively with the increase of dosage.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to cucumber does not all appear in each treatment agent, illustrates that it is safe to cucumber.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
4.1 field trial is prevented and treated downy mildew of garpe
4.1.1 test method
Test is at 4 points of Pingdu City wine-growing Di，Mei community, Shandong investigation, and every some investigation 2 strains, put down in writing occurring degree by staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area.
4.1.2 control time and number of times
Test is investigated 4 times altogether, radix investigation before medicine, for the first time after medicine 14 days, after 14 days and medicine, within 21 days, investigated after medicine for the second time.
4.1.3 drug effect computational methods
Sick leaf rate (%)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(disease index after disease index before 1-(blank district medicine * treatment region medicine)/(disease index before disease index after blank district medicine * treatment region medicine)) * 100.
4.1.4 poisoning investigation method
After dispenser, whether continuous 14d range estimation medicament has poisoning to crop.
4.1.5 result of the test and analysis
Each processes the effect (table 3) of control cucumber downy mildew
Each processes the effect of control cucumber downy mildew table 3
The Mixed Pharmacy of different proportion, tested by different consumptions as can be seen from Table 3, and after medicine, its control to downy mildew of garpe all is better than contrasting medicament, and bactericidal effect increases progressively with the increase of dosage.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to grape does not all appear in each treatment agent, illustrates that it is safe to grape.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
In sum, the bactericidal composition that the present invention contains fluopicolide and metrafenone, powdery mildew of cucumber and downy mildew of garpe are had to good control efficiency, and it is to the target crop safety.Complex preparation has not only improved preventive effect, and has enlarged fungicidal spectrum, so this compounded combination tool in production practices is of great significance.
Claims (4)
1. a bactericidal composition that contains fluorine pyridine bacterium acid amides and metrafenone, it is characterized in that: the active ingredient of this bactericidal composition is fluorine pyridine bacterium acid amides and metrafenone binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient fluorine pyridine bacterium acid amides and metrafenone is 1～40: 40～1.
2. bactericidal composition according to claim 1, it is characterized in that: fluorine pyridine bacterium acid amides and the gross weight of metrafenone in preparation account for 1%～80% of the whole quality of the pharmaceutical preparations.
3. bactericidal composition according to claim 2, it is characterized in that: fluorine pyridine bacterium acid amides and the gross weight of metrafenone in preparation account for 5%～50% of the whole quality of the pharmaceutical preparations.
4. according to claim 1 or 2 or 3 described bactericidal compositions, it is characterized in that: the formulation of this bactericidal composition is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion
.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104068019A (en) * | 2014-07-18 | 2014-10-01 | 陕西上格之路生物科学有限公司 | Sterilization composition containing cyflufenamid and metrafenone |
| CN105831122A (en) * | 2016-05-26 | 2016-08-10 | 南京华洲药业有限公司 | Sterilization composition containing fluoride ether bacteria amide and metrafenone and application thereof |
| CN106665583A (en) * | 2016-11-14 | 2017-05-17 | 湖南化工研究院有限公司 | Bactericidal composition and application thereof |
| CN111587879A (en) * | 2020-06-30 | 2020-08-28 | 青岛润农化工有限公司 | Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof |
| CN111685117A (en) * | 2020-06-30 | 2020-09-22 | 青岛润农化工有限公司 | Bactericidal composition containing metrafenone and flutolanil and application thereof |
-
2013
- 2013-03-19 CN CN2013100872744A patent/CN103168780A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 杨吉春 等: "吡啶类农药的研究新进展及合成", 《农药》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104068019A (en) * | 2014-07-18 | 2014-10-01 | 陕西上格之路生物科学有限公司 | Sterilization composition containing cyflufenamid and metrafenone |
| CN104068019B (en) * | 2014-07-18 | 2015-11-18 | 陕西上格之路生物科学有限公司 | A kind of bactericidal composition containing cyflufenamid and metrafenone |
| CN105831122A (en) * | 2016-05-26 | 2016-08-10 | 南京华洲药业有限公司 | Sterilization composition containing fluoride ether bacteria amide and metrafenone and application thereof |
| CN106665583A (en) * | 2016-11-14 | 2017-05-17 | 湖南化工研究院有限公司 | Bactericidal composition and application thereof |
| CN111587879A (en) * | 2020-06-30 | 2020-08-28 | 青岛润农化工有限公司 | Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof |
| CN111685117A (en) * | 2020-06-30 | 2020-09-22 | 青岛润农化工有限公司 | Bactericidal composition containing metrafenone and flutolanil and application thereof |
| CN111685117B (en) * | 2020-06-30 | 2021-09-14 | 青岛润农化工有限公司 | Bactericidal composition containing metrafenone and flutolanil and application thereof |
| CN111587879B (en) * | 2020-06-30 | 2021-09-21 | 青岛润农化工有限公司 | Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof |
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