CN103719098B - A kind of bactericidal composition that contains bupirimate and Difenoconazole - Google Patents
A kind of bactericidal composition that contains bupirimate and Difenoconazole Download PDFInfo
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Abstract
The present invention relates to a kind of bactericidal composition that contains bupirimate and Difenoconazole, its active ingredient is bupirimate and Difenoconazole binary built, and all the other are auxiliary element. Wherein the mass ratio of active ingredient bupirimate and Difenoconazole is 1～80: 80～1, in preparation, the gross mass of active ingredient bupirimate and Difenoconazole accounts for 1%～80% of whole preparation gross mass, and the formulations of pesticide that bactericidal composition of the present invention can be made are missible oil, suspending agent, wettable powder, water dispersible granules, aqueous emulsion, microemulsion. Be mainly used in preventing and treating anthracnose, powdery mildew, scab, anthrachose of grape, white rot, spot defoliation, brown spot, rust, stripe rust, head blight etc. crop disease.
Description
Technical field
The present invention relates to agriculture chemical compounding technical field, particularly relate to one and contain bupirimate and DifenoconazoleBactericidal composition.
Background technology
Bupirimate belongs to miazines systemic fungicide, has protection and therapeutic action. Can by plant roots, stem,Leaf absorbs rapidly, and in plant, runs to each position, therefore resistance of rainwater washing against. Have that consumption is few, efficient, low toxicity, dialoguePowder disease has the advantages such as special efficacy, has therefore replaced the agricultural chemicals such as the phonetic phenol of second and dimethirimol. Being suitable for fruit tree, vegetables, flowers etc. views and admiresPlant, field crop. The various powdery mildews of controlling object, as apple, grape, cucumber, strawberry, rose, sweet Lay powdery mildew, to grassSome kind such as the certain kind of berries, apple, rose has poisoning. Bupirimate chemistry is by name: 5-butyl-2-ethylamino-6-methylpyrimidine-4-base dimethylamino sulfuric ester, its chemical structural formula is
Difenoconazole has protection, treatment and systemic activity, is sterol demethylation inhibitor, suppresses cell membrane steroidThe biosynthesis of alcohol, stops the growth of fungi. Difenoconazole is triazole bactericidal agent, and fungicidal spectrum is wide, foliar treatment or seedProcessing can improve output and the guaranteed quality of crop. Be widely used in the crop such as fruit tree, vegetables, effectively prevent and treat scab, hemorrhagic black smallpoxDisease, white rot, spot defoliation, powdery mildew, brown spot, rust, stripe rust, head blight etc., to bitter rot or anthracnose of grape, white rot effectFruit is also fine. Chemical name: suitable, the chloro-4-[4-methyl-2-1H-1 of trans-3-, 2,4-triazol-1-yl methyl)-1,3-bis-mute pentaAlkane-2-yl) phenyl 4-chlorphenyl ether, its chemical structural formula is
Using chemical agent is the most effectively means of controlling plant diseases. But use single long-term continuous high doseChemical bactericide, easily cause the problems such as residual, the environmental pollution of medicament and resistance to resistance to the action of a drug fungi development. Reasonably chemistryBactericide compounded or mixture has expansion fungicidal spectrum, improve prevention effect, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning,Reduce residual, delay the actively feature such as Antifungal resistance and drug-fast generation and development, bactericide compounded is to solve above-mentioned askingOne of effective method the most of topic. Develop new product bactericide price constantly soaring, and by contrast, develop and study efficiently,It is short and be subject to domestic and international attention that the composite and mixture of low toxicity, low-residual has small investment, lead time, and numerous and confused increasing developsDynamics. We on the basis of lab screening and field test, filter out bupirimate and Difenoconazole carry out composite,There is obvious synergistic effect. And composite bactericidal composition and application about bupirimate and Difenoconazole are currentThere is no people 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. Can be used for preventingControl anthracnose, powdery mildew, scab, anthrachose of grape, white rot, spot defoliation, brown spot, rust, stripe rust, head blight etc.Crop disease.
Technical scheme of the present invention realizes by following measures:
A bactericidal composition that contains bupirimate and Difenoconazole, the active ingredient second of this bactericidal compositionTwo yuan of phonetic sulfocarbolate and Difenoconazoles are composite, and all the other are auxiliary element. Active ingredient second in wherein said Pesticidal combinationThe mass ratio of phonetic sulfocarbolate and Difenoconazole is 1～80: 80～1, and described bactericidal composition of the present invention is through toxicity testExperimental verification, the mass ratio of bupirimate and Difenoconazole is 1～50: 50～1 o'clock, synergistic effect is better.
The formulations of pesticide that described bactericidal composition of the present invention can be prepared are missible oil, suspending agent, wettable powder, moistureShot agent, aqueous emulsion, microemulsion. Wherein active ingredient bupirimate and the Difenoconazole gross mass in preparation accounts for whole1%～80% of the individual quality of the pharmaceutical preparations, while wherein accounting for 5%-50%, toxicity and residually reach good balance, 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:
1～80 part of bupirimate
1～80 part of Difenoconazole
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 for first adding molten by active ingredient bupirimate and DifenoconazoleAfter adding again emulsifying agent, synergist to stir after dissolving completely in agent, become the oily liquids of transparent and homogeneous, filling, can be made intoThe cream preparation of the present composition.
Described bactericidal composition is suspending agent, and the mass fraction of component is:
1～80 part of bupirimate
1～80 part of Difenoconazole
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, for first other auxiliary agents being mixed, mixes through high speed shear, adds effectivelyComposition bupirimate and Difenoconazole, abrading-ball 2～3 hours in ball crusher, makes a diameter all below 5mm,Make the suspending agent preparation of the present composition.
Described bactericidal composition is wettable powder, and the mass fraction of component is:
1～80 part of bupirimate
1～80 part of Difenoconazole
3～10 parts of dispersants
1～5 part of wetting agent
Filler surplus.
The concrete production stage of this wettable powder is: by above-mentioned formula by active ingredient bupirimate and phenylate firstRing azoles and dispersant, wetting agent and filler mix, and uniform stirring in stirred tank is mixing after airslide disintegrating mill,Can be made into the wettable powder of the present composition.
Described bactericidal composition is water dispersible granules, and the mass fraction of component is:
1～80 part of bupirimate
1～80 part of Difenoconazole
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 by active ingredient bupirimate and phenylate firstRing azoles and dispersant, wetting agent, disintegrant and filler mix, and pulverize with micro jet, through mediating, then addEnter to carry out in fluid bed granulating and drying machine after granulation, dry, screening, through sample analysis, to can be made into the moisture of the present compositionShot agent.
Described bactericidal composition is aqueous emulsion, and the mass fraction of component is:
1～80 part of bupirimate
1～80 part of Difenoconazole
3～30 parts of emulsifying agents
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 by bupirimate and Difenoconazole, solvent and emulsifying agent,Cosolvent is added together, and makes to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobialMix into uniform water; When reactor high speed stirs, oil phase is added to water, slowly add water until reachTo phase inversion point, open cutter and carry out high speed shear, and add remaining water, shear about half an hour, form the water of oil-in-water typeEmulsion, can be made into the aqueous emulsion of the present composition.
Wherein above-described emulsifying agent is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkyl phenol polyoxyVinethene sulfosuccinate, styrylphenol polyoxyethylene ether, NPE, 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, turpentineOil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in water equal solvent are arbitrarily than the mixing of compositionThing.
Described dispersant is selected from polycarboxylate, lignosulfonates, APES methyl ether condensation product sulfuric acidSalt, alkylsulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, APES, polyoxyethylene carboxylate, fatAmine APEO, one or more in 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 phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in soapberry powder.
Described disintegrant is selected from bentonite, urea, and ammonium sulfate, aluminium chloride, citric acid, succinic acid, in sodium acid carbonateOne or more.
Described thickener is selected from xanthans, carboxymethyl cellulose, and carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate,In polyvinyl alcohol one or more.
Described stabilizing agent is selected from natrium citricum, 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, C10-20 saturated fat acid compounds, C8-10 fatOne or more of alcohol.
Described filler is selected from kaolin, diatomite, and bentonite, attapulgite, white carbon, starch, in precipitated calcium carbonateOne or more.
Bactericidal composition of the present invention has taking bupirimate and Difenoconazole as the composite bactericide of active ingredientSignificantly synergistic effect,, delay the drug-fast generation in key, and reduced to become to produce cost and use cost, can be used for resistance diseaseThe improvement of evil. Can be used for preventing and treating anthracnose, powdery mildew, scab, anthrachose of grape, white rot, spot defoliation, brown spot, rust,Stripe rust, head blight etc. crop disease.
Detailed description of the invention
For making technical scheme of the present invention, object and advantage are clearer, the following specific embodiment of the present inventionDescribe, but the present invention is not limited to these examples. Effect experiment of the present invention adopts indoor biometrics and field test phaseIn conjunction with mode, if no special instructions, the ratio of below mentioning is all ratio of quality and the number of copies.
Embodiment: bupirimate proportioning co-toxicity experiments different from Difenoconazole.
1.1 reagent agent
The former medicine of 95% bupirimate, 95% difenoconazole technical material, above-mentioned former medicine is limited by sea, Qingdao rel medicine companyResearch and development department of company provides.
1.2 test targets
Never executed bupirimate and Difenoconazole from Shouguang, Shandong and cucumber of the same type gathers potted plantlySeparate, for trying 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 5 different proportionings, then useIt is stand-by that each processing is diluted to respectively 5 concentration gradients by acetone, 5 30% bupirimate proportionings different from DifenoconazoleThe ratio of active ingredient is respectively 14:16; 17:13; 20:10; 23:7; 26:4. Be diluted to respectively 5 series concentration gradients stand-by.
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 leavesAfter date, 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
Powdery mildew of cucumber bacterium adopts plants method to cultivate under 20 DEG C, the condition of 12h alternation of light and darkness, and every 30d turns and is commissioned to trainSupport 1 time. When inoculation, with the conidium on sterilized water wash-out incidence of leaf, being mixed with spore concentration is l × 106Individual/mL'sSuspension.
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, randomMix, be placed in respectively the series concentration liquid configuring and soak lh, 50 leaf dishes of each concentration, test is with adding medicine notBe treated to blank, after immersion finishes, leaf faces up and puts on the wetting blotting paper of identical liquor strength, leaf dishOn liquid blot, the spore suspension l0L preparing is inoculated in to leaf dish central authorities, room temperature is placed after 5min, is placed in 20 DEG C, 1Under the condition of 2h alternation of light and darkness, cultivate, after 10d, measure the onset area on leaf dish, calculate EC50。
On the basis of pilot study, respectively single dose bupirimate and Difenoconazole are carried out to poison in order to upper methodPower is measured, the two EC50Value is respectively 4.76 ㎎/l and 18.34 ㎎/l
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 the contrast death rate < 5%, does not proofread and correct, the contrast death rate, between 5%-20%, is proofreaied and correct by formula 2, and contrast is deadThe rate of dying > 20%, test need be reformed.
Taking the logarithm value of drug concentration (mg/L) as independent variable x, taking the probability value of corrected mortality as dependent variable y, respectivelySet up virulence regression equation formula, adopt DPS software to calculate the LC of single dose and each proportioning mixture50Calculate poison altogether according to the abundant method of Sun YunCoefficient (CTC). Co-toxicity coefficient CTC, computing formula is as follows: (taking bupirimate as standard medicament, its toxicity index is100）：
The LC of toxicity index (the TI)=bupirimate of Difenoconazole50The LC of/Difenoconazole50×100
The LC of true toxicity index (ATI)=bupirimate of M50The LC of/M50×100
The TI of TI × P bupirimate+Difenoconazole of theoretical toxicity index (TTI)=bupirimate of M ×P Difenoconazole
TTI × 100 of the ATI/M of co-toxicity coefficient (CTC)=M of M
In formula:
M is bupirimate and the mixture of the different proportionings of Difenoconazole
P bupirimate is bupirimate shared ratio in mixture
P Difenoconazole is Difenoconazole shared ratio in mixture
2.1 toxicity test results
Table 1 bupirimate and the Difenoconazole toxicity test to powdery mildew of cucumber
| Process title | Proportioning | Virulence regression equation (Y=a+bX) | Correlation coefficient r value | LC50（mg/L） | Co-toxicity coefficient (CTC) |
| Bupirimate | _____ | Y=2.3784X+3.0291 | 0.9894 | 4.76 | _______ |
| Difenoconazole | _____ | Y=1.1348X+4.3217 | 0.9882 | 18.34 | _______ |
| Bupirimate: Difenoconazole | 14：16 | Y=2.4421X+3.8526 | 0.9892 | 5.77 | 136.23 |
| Bupirimate: Difenoconazole | 17：13 | Y=2.1356X+3.9388 | 0.9914 | 4.92 | 142.46 |
| Bupirimate: Difenoconazole | 20：10 | Y=2.7437X+3.7109 | 0.9891 | 4.05 | 156.04 |
| Bupirimate: Difenoconazole | 23：7 | Y=2.9133X+3.4479 | 0.9884 | 4.08 | 141.04 |
| Bupirimate: Difenoconazole | 26：4 | Y=2.7839X+3.4215 | 0.9901 | 3.92 | 134.82 |
As can be seen from the table, the result of the test of different proportion proportioning shows, is 14:16 in active ingredient ratio; 17:13; 20:10; 23:7; When 26:4 dilutes respectively, all show stronger synergistic effect, wherein with bupirimate and phenylateSynergistic effect the best when methyl cyclic-azole is 20:10, its co-toxicity coefficient is 156.04. Suggestion is mixed to suitable proportion 20:10 left and rightPreparaton carries out further field control effectiveness test, to evaluate its field practical application effect.
3 field tests are prevented and treated powdery mildew of cucumber, the experimental result of mango anthracnose
3.1 field tests are prevented and treated powdery mildew of cucumber
3.1.1 test method
Test is on Shandong Pingdu City cucumber ground, and 4 points of every community investigation, investigate 2 strains at every, by staging record morbidity journeyDegree, grade scale is as follows:
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;
3.1.2 control time and number of times
Test is investigated 4 times altogether, and radix investigation before medicine is investigated after 3 days, 7 days and medicine after medicine for 15 days.
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
Prevention effect (%)=(disease index after the front disease index × treatment region medicine of 1-(blank district medicine)/(blankThe front disease index of disease index × treatment region medicine after district's medicine)) × 100
3.1.4 poisoning investigation method
After dispenser, whether 7d range estimation medicament has poisoning to crop continuously.
3.1.5 result of the test and analysis
Each effect (table 2) of preventing and treating powdery mildew of cucumber of processing
The each effect of preventing and treating powdery mildew of cucumber of processing of table 2
30% bupirimate Difenoconazole ME(20:10 as shown in Table 2) composite bactericide for cucumber white powderSick controls successful higher than bupirimate and Difenoconazole single dose, and after medicine, the bactericidal effect of 15 days is respectively90.13,91.36,92.49. Bactericidal effect increases progressively with the increase of dosage. According to field range estimation, within the scope of test dose, doThing growth is normal, and the poisoning phenomenon to cucumber does not all appear in each treatment agent, illustrates that it is safe to cucumber. Suggestion and effectThe bactericide that mechanism is different mixes use to delay the drug-fast generation of germ.
4.1 field test control citrus anthracnoses
4.1.1 test method
Every community adopts 5 samplings, investigates 2-3 strain at every, investigates whole blades of every strain, with the scab on every leafNumber carry out classification and record total number of sheets, the sick number of sheets at different levels, calculate the blade incidence of disease, disease index, and contrast disease and refers to comparison, calculatingRelative control effect.
Severity Scaling standard (taking blade as unit)
0 grade: without scab;
1 grade: single blade has 3 of scabs;
3 grades: single blade has 4～6 of scabs;
5 grades: single blade has 7～10 of scabs;
7 grades: single blade has 11～20 of scabs, part is intensive in flakes;
9 grades: single blade has the intensive leaf area that accounts for of scab more than 1/4th.
4.1.2 control time and number of times
Test is investigated 4 times altogether, radix investigation before medicine, after medicine 5 days for the first time, after medicine 5 days and for the third time after medicine 18 for the second timeIt is investigated.
4.1.3 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
Prevention effect (%)=(disease index after the front disease index × treatment region medicine of 1-(blank district medicine)/(blankThe front disease index of disease index × treatment region medicine after district's medicine)) × 100
4.1.4 poisoning investigation method
After dispenser, whether 7d range estimation medicament has poisoning to crop continuously.
4.1.5 result of the test and analysis
Each effect of processing control citrus anthracnose
The each effect of processing control citrus anthracnose of table 3
As can be seen from Table 3,30% bupirimate Difenoconazole ME is with 20:10 mixture control citrus anthracnoseAfter its 1 medicine, the prevention effect of 5 days is better than bupirimate and two kinds of single doses of Difenoconazole preventive effect with isoconcentration processing,There is good quick-acting; After its 3 medicines, the preventive effect of 18 days can reach 81.78%-87.62%, 30% bupirimate phenylate firstThe combination of ring azoles mixture has good prevention effect to citrus anthracnose, can be good at controlling the generation of citrus anthracnose. RootAccording to field range estimation, within the scope of test dose, plant growth is normal, and the poisoning phenomenon to oranges and tangerines does not all appear in each treatment agent,Illustrate that it is safe to oranges and tangerines.
In sum, the present invention is the bactericidal composition that contains bupirimate and Difenoconazole, to cucumber white powderDisease, citrus anthracnose etc. all have good effect, and it is to target crop safety, compared with single dose, and Bactericidal composite of the present inventionThing has advantages of that quick-acting is good, the lasting period is long, is difficult for producing poisoning, so research and development of the present invention and popularization have societyVery important meaning.
Claims (1)
1. contain the bactericidal composition of bupirimate and Difenoconazole in the microemulsion of preparation control citrus anthracnosePurposes, it is characterized in that, the active ingredient of this bactericidal composition is bupirimate and Difenoconazole binary built, itsRemaining is auxiliary element, and wherein the mass ratio of active ingredient bupirimate and Difenoconazole is 20:10, wherein active ingredientGross mass account for 30% of whole microemulsion gross mass.
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