CN103798256A - Bactericidal composition containing cyflufenamid and thifluzamide - Google Patents
Bactericidal composition containing cyflufenamid and thifluzamide Download PDFInfo
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- CN103798256A CN103798256A CN201410033864.3A CN201410033864A CN103798256A CN 103798256 A CN103798256 A CN 103798256A CN 201410033864 A CN201410033864 A CN 201410033864A CN 103798256 A CN103798256 A CN 103798256A
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- bacterium amine
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Abstract
The invention relates to a bactericidal composition containing cyflufenamid and thifluzamide. The bactericidal composition comprises active ingredients including the cyflufenamid and the thifluzamide in a binary compound way, and the balance of auxiliary components, wherein the mass ratio of the active ingredient cyflufenamid to the active ingredient thifluzamide in the pesticide composition is (1-50): (50-1); the preparation comprises the active ingredients including the cyflufenamid and the thifluzamide with the mass percent of 1-80%, and the balance of acceptable auxiliary components which are allowed to be used in pesticide. The pesticide composition can be prepared into different preparations such as missible oil, suspending agent, wettable powder, water dispersible granules, emulsion in water, microemulsion, granules, microcapsules or aqueous solution, is mainly used for controlling the powdery mildew of wheat, strawberries, grapes, apples and cucumbers, is capable of effectively controlling fungi such as rhizoctonia, puccinia, ustilago, tilletia, corticium and pyrenophora, and especially has special effect for diseases such as banded sclerotial blight and damping off caused by basidiomycotina fungus.
Description
Technical field
The present invention relates to agriculture chemical compounding technical field, particularly relate to a kind of bactericidal composition that contains epoxy bacterium amine and thifluzamide.
Background technology
Epoxy bacterium amine (ring fluorine benzyl acid amides), by suppressing formation and the growth of mitogenetic haustorium on mycelia in the Powdery Mildew history of life (being also pathogenic process), the growth of secondary hyphae and the formation of hapteron, prevent and treat powdery mildew for wheat class, strawberry, grape, apple, cucumber etc.
Thifluzamide belongs to thiazole amide bactericide, its chemistry 2' by name, the bromo-2-methyl-4'-of 6'-bis-trifluoromethoxy-4-Trifluoromethyl-1,3-thiadiazoles-5-hydroxyl anilide.Thifluzamide has strong interior conductivity and the long lasting effect of inhaling.Thifluzamide is succinate dehydrogenase inhibitor, thifluzamide all has activity to pathomycetes such as Rhizoctonia, Puccinia, Ustilago, Tilletia, corticium, nuclear cavity Pseudomonas, especially the fungus-caused disease of Basidiomycetes is had to special efficacy as banded sclerotial blight, damping off etc.
In the real process of agricultural production, using chemical agent is the most effectively means of control plant pest, but the problem the most easily producing by chemical control disease is the generation of disease drug resistance.In the chemical control of bacteriosis, years of researches are carried out both at home and abroad, although some antibacterium medicaments have started to enter practical stage, but the medicament of chemosynthesis has long, the shortcoming such as cost is high, toxicity is large, environmental pollution is serious of cycle, can not meet the requirement of agricultural sustainable development far away.And long-term use single pesticidal preparations continuously high dose, easily cause the problem such as residual, environmental pollution and resistance to pesticide resistance fungi development of medicament.And by contrast, exploitation is efficient with research, composite and the mixture of low toxicity, low-residual has small investment, the lead time is short and be subject to domestic and international attention, numerous and confused increasing develops dynamics.We filter out epoxy bacterium amine and thifluzamide and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And there is no at present people about the composite composition pesticide of epoxy bacterium amine and thifluzamide 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 composition pesticide, be mainly used in preventing and treating the powdery mildew on wheat class, strawberry, grape, apple, cucumber, the simultaneously effectively fungi such as control Rhizoctonia, Puccinia, Ustilago, Tilletia, corticium, nuclear cavity Pseudomonas, especially has special efficacy to the fungus-caused disease of Basidiomycetes as banded sclerotial blight, damping off etc.
Technical scheme of the present invention realizes by following measures:
A bactericidal composition that contains epoxy bacterium amine and thifluzamide, active ingredient epoxy bacterium amine and two yuan of the thifluzamides of this composition pesticide are composite, and all the other are auxiliary element.In wherein said composition pesticide, the mass ratio of active ingredient epoxy bacterium amine and thifluzamide is 1～50: 50～1, described composition pesticide of the present invention is through toxicity test experimental verification, the mass ratio of epoxy bacterium amine and thifluzamide is 1～10: 10～1 o'clock, synergistic effect optimum.
The formulations of pesticide that described composition pesticide of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations, aqua.Wherein active ingredient epoxy bacterium amine and the thifluzamide gross mass in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations, while wherein accounting for 1%～50%, and toxicity and residually reach good balance, cost is also lower.
The specific embodiments of the formulations of pesticide that composition pesticide of the present invention is mixed with is as follows:
Described bactericidal composition is cream preparation, and the mass fraction of component is: 1～50 part of epoxy bacterium amine; 1～50 part of thifluzamide; 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 is first active ingredient epoxy bacterium amine and thifluzamide to be added in solvent to the oily liquids that becomes transparent and homogeneous after adding again emulsifier, synergist to stir after dissolving completely, 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: 1～50 part of epoxy bacterium amine; 1～50 part of thifluzamide; 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 epoxy bacterium amine and thifluzamide, abrading-ball 2～3 hours in ball crusher, 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: 1～50 part of epoxy bacterium amine; 1～50 part of thifluzamide; 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 epoxy bacterium amine is mixed with thifluzamide and dispersant, wetting agent and filler, uniform stirring in stirred tank, after airslide disintegrating mill, mixing, 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: 1～50 part of epoxy bacterium amine; 1～50 part of thifluzamide; 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 epoxy bacterium amine is mixed with thifluzamide and dispersant, wetting agent, disintegrant and filler, pulverize with micro jet, through mediating, then add and in fluidized bed prilling dryer, carry out after granulation, dry, screening, through 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: 1～50 part of epoxy bacterium amine; 1～50 part of thifluzamide; 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: first epoxy bacterium amine and thifluzamide, 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 reactor high speed stirs, oil phase is added to water, slowly add water until reach 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: 1～50 part of epoxy bacterium amine, 1～50 part of thifluzamide, 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.Epoxy bacterium amine and thifluzamide are dissolved completely 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.
Described bactericidal composition is granule, and the mass fraction of component is: 1～50 part of epoxy bacterium amine, 1～50 part of thifluzamide, 1～10 part of wetting dispersing agent; 0.1～5 part of thickener; 0.1～5 part of defoamer; Castor oil, surplus is supplied.Each components such as active ingredient epoxy bacterium amine and thifluzamide, dispersant, stabilizing agent, defoamer and solvent are mixed in the ratio of formula, put into after the grinding of sand milling still, send in mixer for well-distribution and mix and get product.
Described bactericidal composition is microcapsule formulations, and the mass fraction of component is: 1～50 part of epoxy bacterium amine, 1～50 part of thifluzamide, 5～20 parts, urea; 5～20 parts, formaldehyde; 5～20 parts of emulsifying dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; Water, surplus.In the there-necked flask that agitating device is housed, add urea and formaldehyde (amount of substance ratio is about l:1.5～2.0), with the left and right, pH value to 8～9 of sodium hydroxide solution regulator solution, then be warming up to 70～80 ℃, reaction obtains stable urea resin prepolymer.Get a certain amount of epoxy bacterium amine and thifluzamide and be dissolved in cyclohexane, and add emulsifying dispersant in solution, follow vigorous stirring, be made into the O/W type stable emulsion take the aqueous solution containing emulsifying dispersant as water.Above-mentioned urea resin prepolymer is added in emulsion, regulate pH value, polymerization reaction take place under acid catalysis condition, is wrapped oil phase substance, forms microcapsule granule.Slowly heat up, solidify, temperature is controlled at 40～50 ℃, hardening time 1h.Selection adds appropriate auxiliary agent, the microcapsules that gets final product stablely.
Described bactericidal composition is aqua, and the mass fraction of component is: 1～50 part of epoxy bacterium amine, 1～50 part of thifluzamide, 0.1～30 part of wetting dispersing agent; 2～8 parts of antifreezing agents; 0.1～1 part of defoamer; 0.1～3 part of thickener; 5～15 parts of spreader-stickers; Water, surplus is supplied.Dissolve completely by active ingredient epoxy bacterium amine and thifluzamide, with cosolvent, then add other compositions such as dispersant, antifreezing agent, defoamer, evenly mix, finally add water, after fully stirring, get final product to obtain finished product.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, 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, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine-based vegetable oil code name is ND-45, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in water equal solvent are arbitrarily than the mixture of composition.
It is LG-3, GY-D1252, GY-D1256, SNWGF-01 that described dispersant is selected from polycarboxylate code name, lignosulfonates code name is 201107,201108, alkylphenol polyoxyethylene methyl ether condensate sulfate, alkylsulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, one or more in fatty acid glyceride APEO.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, moistening bleeding agent F, alkylbenzenesulfonate polyoxyethylene triphen phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in 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, the one 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
10-20saturated 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, take epoxy bacterium amine and thifluzamide as the composite bactericide of active ingredient has obvious synergistic effect, delays the drug-fast generation in key, and has reduced and become to produce cost and use cost.Be mainly used in preventing and treating the powdery mildew on wheat class, strawberry, grape, apple, cucumber, the simultaneously effectively fungi such as control Rhizoctonia, Puccinia, Ustilago, Tilletia, corticium, nuclear cavity Pseudomonas, especially has special efficacy to the fungus-caused disease of Basidiomycetes as banded sclerotial blight, damping off etc.
Embodiment
For making technical scheme of the present invention, object 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: epoxy bacterium amine proportioning co-toxicity experiments different from thifluzamide.
1.1 reagent agent
The former medicine of 95% epoxy bacterium amine, the former medicine of 95% thifluzamide, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test targets
Never executed epoxy bacterium amine and thifluzamide from Shouguang, Shandong and cucumber of the same type gathers and separates potted plantly, for 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 several different proportionings, then it is stand-by with acetone, each processing to be diluted to respectively to several concentration gradients.
Susceptible cucumber variety Chang Chun Mi Ci is cultivated in pot for growing seedlings, be placed in greenhouse and cultivate, 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 germ.
1.3.2 the cultivation of powdery mildew of cucumber germ and the preparation of spore suspension
Powdery mildew of cucumber germ adopts plants method to cultivate under 20 ℃, the condition of 12h alternation of light and darkness, and every 30 d turn culture 1 time.When 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 the leaf dish that diameter is 1.5cm, mix at random, be placed in respectively the series concentration liquid configuring and soak lh, 50 leaf dishes of each concentration, test is with the blank that is treated to of adding medicine not, after immersion finishes, leaf faces up and puts on the wetting blotting paper of identical liquor strength, liquid on leaf dish is blotted, the spore suspension l0L preparing is inoculated in to leaf dish central authorities, and room temperature is placed after 5 min, is placed under 20 ℃, the condition of 1 2h alternation of light and darkness and cultivates, after 10d, measure the onset area on leaf dish, calculate EC
50.
The percentage that accounts for leaf disc area according to lesion area is divided sick level
0 grade: anosis;
1 grade: sorus area accounts for below 5% of whole leaf area;
3 grades: sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: sorus area accounts for the 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%, does not proofread and correct, contrast lethality, between 5%-20%, is proofreaied and correct by formula 2, contrast lethality >20%, and test need be reformed.
Take the logarithm value of drug concentration (mg/L) as independent variable x, take the probability value of corrected mortality as dependent variable y, set up respectively virulence regression equation formula, adopt 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: (take epoxy bacterium amine as standard medicament, its toxicity index is 100):
The EC of toxicity index (TI)=epoxy bacterium amine of thifluzamide
50the EC of/thifluzamide
50× 100
The EC of true toxicity index (ATI)=epoxy bacterium amine of M
50the EC of/M
50× 100
TI × P thifluzamide of TI × P epoxy bacterium amine+thifluzamide of theoretical toxicity index (TTI)=epoxy bacterium amine of M
TTI × 100 of the ATI/M of co-toxicity coefficient (CTC)=M of M
In formula:
M is epoxy bacterium amine and the mixture of the different proportionings of thifluzamide
P epoxy bacterium amine is epoxy bacterium amine shared ratio in mixture
P thifluzamide is thifluzamide shared ratio in mixture.
2.1 toxicity test results
Table 1 epoxy bacterium amine and the toxicity test of thifluzamide 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 active ingredient ratio, wherein take epoxy bacterium amine: thifluzamide is synergistic effect the best as 1:10～10:1 time, suggestion is carried out further field control effectiveness test to suitable proportion 1:10～10:1 left and right mixture preparation, to evaluate its field practical application effect.
3, the experimental result of field trial control wheat powdery mildew, rice sheath blight disease
3.1 field trial control wheat powdery mildews
3.1.1 test method
Test site, in great Tong Qiao village, capital town, Fengyang County, is wheat for studying thing, and kind is short morning 781, broadcasts sowing, and growing way is better, and test is established every mu and established contrast totally 10 processing.Every processing repeats 4 times, and random district group is arranged, 30 square metres of community areas.
3.1.2 control time and number of times
Before dispenser, after the 1st medicine after 7 days and the 2nd dispenser 7 days, 14 days, every community adopted 5 samplings of diagonal, every some investigation 20 strains, before blooming, 2 leaves are got in every strain from upper end, after blooming, sword-like leave 2 leaves are got in every strain, by leaf classification investigation occurring degree, calculate disease and refer to and control efficiency.
Grade scale is as follows:
0 grade: anosis;
1 grade: lesion area accounts for below 5% of one-piece blade area;
3 grades: lesion area accounts for the 6%-15% of one-piece blade area;
5 grades: lesion area accounts for the 16%-25% of one-piece blade area;
7 grades: lesion area accounts for the 26%-50% of one-piece blade area;
9 grades: lesion area accounts for the more than 50% of one-piece blade area.
3.1.3 drug effect computational methods
The total number of sheets × 100 of sick leaf rate (%)=sick number of sheets/investigate
Disease index=∑ (the sick number of sheets × relative level numerical value at different levels)/(investigating the total number of sheets × 9) × 100
Control efficiency (%)=(disease index after the front disease index × treatment region medicine of 1-(blank district medicine)/(the front disease index of disease index × treatment region medicine after blank district medicine)) × 100.
3.1.4 poisoning investigation method
After dispenser, whether 14d range estimation medicament has poisoning to crop continuously.
3.1.5 result of the test and analysis
Each effect of processing control wheat powdery mildew.
As shown in Table 2 epoxy bacterium amine and thifluzamide composite bactericide for wheat powdery mildew control successful higher than epoxy bacterium amine and thifluzamide single dose, bactericidal effect increases progressively with the increase of dosage.According to field range estimation, within the scope of test dose, plant growth is normal, and the poisoning phenomenon to wheat does not all appear in each treatment agent, illustrates that it is safe to wheat.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
3.2 field trials are prevented and treated rice sheath blight disease
3.2.1 test method
Test is at Jimo Yi Feng town, Qingdao of Shandong province paddy base, and test kind is hybrid rice variety, and every processing repeats for 4 times, 5 points of every community double diagonal line investigation, and the whole blades of five strains when investigation, a situation arises for statistics disease.
Record occurring degree by staging, grade scale is as follows:
0 grade: anosis;
1 grade: scab heap area accounts for below 5% of whole leaf area;
3 grades: scab heap area accounts for below the 6%-10% of whole leaf area;
5 grades: scab heap area accounts for below the 11%-20% of whole leaf area;
7 grades: scab heap area accounts for below the 21%-50% of whole leaf area;
9 grades: scab heap area accounts for the more than 50% of whole leaf area.
3.2.2 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 for 15 days.
3.2.3 drug effect computational methods
The total number of sheets × 100 of sick leaf rate (%)=sick number of sheets/investigate
Disease index=∑ (the sick number of sheets × relative level numerical value at different levels)/(investigating the total number of sheets × 9) × 100
Control efficiency (%)=(disease index after the front disease index × treatment region medicine of 1-(blank district medicine)/(the front disease index of disease index × treatment region medicine after blank district medicine)) × 100.
3.2.4 poisoning investigation method
After dispenser, whether 15d range estimation medicament has poisoning to crop continuously.
3.2.5 result of the test and analysis
Table 3 different disposal is to rice sheath blight disease controlling measurement result
Show by above field experiment, epoxy bacterium amine and thifluzamide complex preparation are obviously better than single dose for the preventive effect of rice sheath blight disease, and bactericidal effect increases progressively with the increase of dosage.According to field range estimation, within the scope of test dose, plant growth is normal, occurs without poisoning situation, significant for agricultural produce, is worthy to be popularized.
In sum, the bactericidal composition that the present invention contains epoxy bacterium amine and thifluzamide, has good control efficiency to wheat powdery mildew, rice sheath blight disease, and it is to target crop safety.Complex preparation has not only improved preventive effect, and has expanded the control to bacterium, so this compounded combination tool in production practices is of great significance.
Claims (4)
1. a bactericidal composition that contains epoxy bacterium amine and thifluzamide, it is characterized in that: the active ingredient of this composition pesticide is epoxy bacterium amine and thifluzamide binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient epoxy bacterium amine and thifluzamide is 1～50: 50～1.
2. composition pesticide according to claim 1, is characterized in that: epoxy bacterium amine and the thifluzamide gross weight in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations.
3. composition pesticide according to claim 2, is characterized in that: epoxy bacterium amine and the thifluzamide gross weight in preparation accounts for 1%～50% of the whole quality of the pharmaceutical preparations.
4. according to the composition pesticide described in claim 1 or 2 or 3, it is characterized in that: the formulation of this composition pesticide is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, microcapsule formulations, granule, aqua.
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Application publication date: 20140521 |