CN103039459A - Sterilization composition containing pyraoxystrobin and JS399-19 - Google Patents

Sterilization composition containing pyraoxystrobin and JS399-19 Download PDF

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CN103039459A
CN103039459A CN 201210448920 CN201210448920A CN103039459A CN 103039459 A CN103039459 A CN 103039459A CN 201210448920 CN201210448920 CN 201210448920 CN 201210448920 A CN201210448920 A CN 201210448920A CN 103039459 A CN103039459 A CN 103039459A
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cyano
amino
azoles bacterium
bacterium ester
phenylancryic acetate
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葛大鹏
陈鹏
韩先正
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Hailir Pesticides and Chemicals Group Co Ltd
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Hailir Pesticides and Chemicals Group Co Ltd
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Abstract

The invention relates to a sterilization composition containing pyraoxystrobin and JS399-19. The effective ingredients, namely the pyraoxystrobin and the JS399-19, are compounded, wherein the mass ratio of the pyraoxystrobin to the JS399-19 is (1-80): (80-1); the total mass of the effective ingredients, namely the pyraoxystrobin and the JS399-19, is 1-80% of the total mass of the whole preparation, and the remnants are allowable and acceptable auxiliary components in pesticide. The sterilization composition can be prepared into following pesticide formulations: missible oil, suspending agents, wettable powder, water dispersible granule, emulsion in water and micro-emulsion, can be used for preventing and treating wheat scab, fusarium wilt of cotton, banana panama disease, rice bakanae disease and watermelon fusarium wilt, and has excellent control effects on cucumber downy mildew, grape downy mildew, tomato late blight, cucumber anthracnose and cucumber powdery mildew.

Description

A kind of bactericidal composition that contains azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate
Technical field
The present invention relates to the agriculture chemical compounding technical field, be specifically related to a kind of bactericidal composition that contains azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate.
Background technology
Azoles bacterium ester is the strobilurin fungicide that Shenyang Chemical Engineering Inst develops.Azoles bacterium ester fungicidal spectrum is wide, bactericidal activity is high, and relatively more outstanding stripped bactericidal activity is arranged, and cucumber downy mildew, downy mildew of garpe, tomato late blight, cucumber anthracnose, powdery mildew of cucumber are had excellent control efficiency.Azoles bacterium esterification formal name used at school is called (E)-2-(2-((3-(4-chlorphenyl)-1-methyl isophthalic acid H-pyrazoles-5-oxygen base) methyl) phenyl)-3-methoxy-methyl acrylate.
2-cyano-3-amino-3-phenylancryic acetate is the cyanoacrylate bactericide of a kind of novel structure, mode of action uniqueness, chemical name: 2-cyano group-3-aminoacrylic acid ethyl ester, 2-cyano-3-amino-3-phenylancryic acetate is effective to the disease that the reaping hook mushroom causes, has protective effect and therapeutic action.Can be used for preventing and treating wheat scab, cotton wilt, banana Panama disease, bakanae disease of rice, watermelon blight etc.
Using chemical agent is the most effectively means of controlling plant diseases.But long-term use single chemical bactericide continuously high dose, cause easily 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, prolong 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 the most one of the effective method that addresses 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 have 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 azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And about the composite bactericidal composition of azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate and use and there is no at present the people and 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 preventing and treating wheat scab, cotton wilt, banana Panama disease, bakanae disease of rice, watermelon blight, cucumber downy mildew, downy mildew of garpe, tomato late blight, cucumber anthracnose, powdery mildew of cucumber are also had excellent control efficiency.
Technical scheme of the present invention realizes by following measures:
A kind of bactericidal composition that contains azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate, active ingredient azoles bacterium ester and two yuan of the 2-cyano-3-amino-3-phenylancryic acetates of this bactericidal composition are composite, and all the other are auxiliary element.The mass ratio of active ingredient azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate is 1~80: 80~1 in the wherein said Pesticidal combination, described bactericidal composition of the present invention is through the toxicity test experimental verification, the mass ratio of azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate 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 azoles bacterium ester and the 2-cyano-3-amino-3-phenylancryic acetate gross mass in preparation accounts for 1%~80% of the whole quality of the pharmaceutical preparations, when wherein accounting for 5%-50%, and toxicity and the residual preferably balance 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: azoles bacterium ester 1~80; 1~80 part of 2-cyano-3-amino-3-phenylancryic acetate; 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 after dissolving fully in the solvent again for first active ingredient azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate being added, can namely can be made into the cream preparation of the present composition.
Described bactericidal composition is suspending agent, and the mass fraction of component is: 1~80 part of azoles bacterium ester; 1~80 part of 2-cyano-3-amino-3-phenylancryic acetate; 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 mixing other auxiliary agents first, mix through high speed shear, add active ingredient azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate, abrading-ball is 2~3 hours in ball crusher, make a diameter all below 5mm, namely 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: 1~80 part of azoles bacterium ester; 1~80 part of 2-cyano-3-amino-3-phenylancryic acetate; 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 prescription active ingredient azoles bacterium ester is mixed with 2-cyano-3-amino-3-phenylancryic acetate and dispersant, wetting agent and filler, uniform stirring in stirred tank, behind airslide disintegrating mill, mixing, namely 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: 1~80 part of azoles bacterium ester; 1~80 part of 2-cyano-3-amino-3-phenylancryic acetate; 3~10 parts of dispersants; 1~10 part of wetting agent; 1~5 part of disintegrant; The filler surplus.
The concrete production stage of this water dispersible granules is: by above-mentioned prescription active ingredient azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, then add and carry out granulation, drying, screening in the fluidized bed prilling dryer by sample analysis, namely 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: 1~80 part of azoles bacterium ester; 1~80 part of 2-cyano-3-amino-3-phenylancryic acetate; 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 azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate, solvent and emulsifier, cosolvent are added together, make and be dissolved into uniform oil phase; With part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear approximately half an hour, form the aqueous emulsion of oil-in-water type, namely can be made into the aqueous emulsion of the present composition.
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 the 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 that forms.
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 the sodium bicarbonate.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in the polyvinyl alcohol one or more.
Described stabilizing agent is selected from sodium citrate, a kind of in the resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, one or more in the 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 the precipitated calcium carbonate.
The composite bactericide of the present invention take azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate as active ingredient has obvious synergistic effect, delays the drug-fast generation in key, and reduced to become to produce cost and use cost, can be used for the improvement of resistance disease.Can be used for preventing and treating wheat scab, cotton wilt, banana Panama disease, bakanae disease of rice, watermelon blight, cucumber downy mildew, downy mildew of garpe, tomato late blight, cucumber anthracnose, powdery mildew of cucumber are also had excellent control efficiency.
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 all is ratio of quality and the number of copies.
Embodiment: the different proportioning co-toxicity experiments from 2-cyano-3-amino-3-phenylancryic acetate of azoles bacterium ester.
1.1 reagent agent
The former medicine of 95.5% azoles bacterium ester, the former medicine of 95% 2-cyano-3-amino-3-phenylancryic acetate, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 subjects
The tomato late blight germ, separation and purification gained from the Pingdu tomato plot incidence of leaf of Shandong is cultivated in 4 ℃ of refrigerators on the PDA inclined-plane and is preserved.
1.3 test method
The percentage mycelial inhibition assay method is adopted in test, and the medicine of different disposal is made into 5 variable concentrations gradients with sterile water, is respectively 7:37; 9:35; 11:33; 13:31; 15:29.
Drawing 1ml liquid (take clear water as contrast) with suction pipe on aseptic working platform joins in the 8cm culture dish, add the rear about 50-60PDA medium of 9ml fusing with syringe again, liquid is evenly mixed with medium, be cooled to room temperature, then the tomato late blight germ piece of inoculation diameter 5mm in the culture dish, in 25 ℃ of incubators, cultivate 5 ~ 7d, after culture dish is covered with in contrast, measure colony diameter with the right-angled intersection method.
If contrast lethality<5% is not proofreaied and correct, the contrast lethality by formula 2 is proofreaied and correct between 5%-20%, the contrast lethality〉20%, 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 the virulence regression equation formula, adopt DPS software to calculate the LC 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 azoles bacterium ester as the standard medicament, its toxicity index is 100):
The LC of the toxicity index of 2-cyano-3-amino-3-phenylancryic acetate (TI)=azoles bacterium ester 50The LC of/2-cyano-3-amino-3-phenylancryic acetate 50* 100
The LC of the true toxicity index (ATI) of M=azoles bacterium ester 50The LC of/M 50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=azoles bacterium ester * P azoles bacterium ester+2-cyano-3-amino-3-phenylancryic acetate * P 2-cyano-3-amino-3-phenylancryic acetate
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In the formula:
M is the mixture of azoles bacterium ester and the different proportionings of 2-cyano-3-amino-3-phenylancryic acetate
P azoles bacterium ester is azoles bacterium ester shared ratio in mixture
The P 2-cyano-3-amino-3-phenylancryic acetate is 2-cyano-3-amino-3-phenylancryic acetate shared ratio in mixture
2.1 toxicity test result
Table 1 different disposal is to tomato late blight Toxicity Determination result
Figure 866604DEST_PATH_IMAGE002
Measurement result shows, under different proportionings, all shows stronger synergistic effect, its co-toxicity coefficient is all greater than 120, show certain synergistic effect, wherein the mass ratio of azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate is that the synergistic effect of 11:33 is the most obvious, and co-toxicity coefficient is 175.98.Suggestion is carried out further field control effectiveness test to suitable proportion 11:33 left and right sides mixture preparation, to estimate its field practical application effect.
3 field trials are prevented and treated wheat scab, the experimental result of tomato late blight
3.1 field trial is prevented and treated wheat scab
3.1.1 test method
Test is adopted the diagonal sampling at Shandong Pingdu City wheat paddock, 5 points of every residential quarter investigation, and the sick spike number in 100 1 200 wheat heads of every some casual inspection, severity extent is divided into 5 grades with ocular estimate:
0 grade anosis;
The sick spikelet number of I level accounts for below 1/4 of whole small ears;
The sick spikelet number of II level accounts for 1/4~1/2 of whole small ears;
The sick spikelet number of III level accounts for 1/2~3/4 of whole small ears;
The sick spikelet number of IV level accounts for more than 3/4 of whole small ears.
3.1.2 control time and number of times
Test is investigated 4 times altogether, radix investigation before the medicine, for the first time behind the medicine 7 days, investigated in 15 days behind 7 days and the medicine behind the medicine for the second time.
3.1.3 drug effect computational methods
Disease tassel yield (%)=sick spike number/investigate total spike number * 100
Disease index=∑ (sick spike numbers at different levels * relative level numerical value)/(investigating total spike number * 4) * 100
Control efficiency (%)=(disease index behind disease index before the 1-(blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
3.1.4 poisoning investigation method
Whether continuous 7d range estimation medicament has poisoning to crop after the dispenser.
3.1.5 result of the test and analysis
Each processes the effect (table 2) of preventing and treating wheat scab
Each processes the effect of preventing and treating wheat scab table 2
Figure DEST_PATH_GDA0000283577851
The Mixed Pharmacy of different proportion is tested by different consumptions as can be seen from Table 2, and its control to wheat scab all is better than contrasting medicament and bactericidal effect and increases progressively with the increase of dosage behind the medicine.15 days preventive effect is the highest behind the medicine for the second time still can reach 90.68, and according to the field range estimation, in the test dose scope, 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.
4.1 field trial control tomato late blight
4.1.1 test method
Be full of and carry out in the water village Zhang Qingxiang booth in the test arrangement town of jumping in the Tengchong County, Yunnan Province, it is serious that tomato late blight experimental field occurs over the years, tomato grows fine, the uniformities such as the soil types of each experimental plot, cultivation condition and water and fertilizer management, and test the last fortnight was not executed the bactericidal agent for preventing and treating disease.
5 samplings are adopted in every residential quarter, investigate the 2-3 strain at every, investigate whole blades of every strain, come classification to record total number of sheets, the sick number of sheets at different levels with the number of the scab on the every leaf, calculate the blade incidence of disease, disease index, refer to comparison with the contrast disease, calculate relative control effect.
Severity Scaling standard (take 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, and 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 the medicine, behind the medicine 5 days for the first time, behind the medicine 5 days and investigated in 18 days behind the medicine for the third time for the second time.
4.1.3 drug effect computational methods
Sick leaf rate (the %)=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 behind disease index before the 1-(blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
4.1.4 poisoning investigation method
Whether continuous 7d range estimation medicament has poisoning to crop after the dispenser.
4.1.5 result of the test and analysis
Each processes the effect (table 3) of preventing and treating anthracnose of tomato
As can be seen from Table 3,44% azoles bacterium ester 2-cyano-3-amino-3-phenylancryic acetate is better than the preventive effect that azoles bacterium ester and two kinds of single doses of 2-cyano-3-amino-3-phenylancryic acetate are processed with isoconcentration with composite its control efficiency of anthracnose of tomato of preventing and treating of 11:33 ratio, has good quick-acting; 18 days preventive effect still can reach 90.62%, 44% azoles bacterium ester 2-cyano-3-amino-3-phenylancryic acetate and so that the 11:33 ratio is composite anthracnose of tomato had good lasting effect behind its 3rd medicine, can be good at controlling the generation of anthracnose.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to tomato does not all appear in each treatment agent, illustrates that it is safe to tomato.
In sum, the present invention is the bactericidal composition that contains azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate, wheat scab, anthracnose of tomato etc. all had preferably effect, and it is to the target crop safety, compare with single dose, bactericidal composition of the present invention has the advantage 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 are of great significance social tool.

Claims (5)

1. bactericidal composition that contains azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate, it is characterized in that: the active ingredient of this bactericidal composition is that azoles bacterium ester and two yuan of 2-cyano-3-amino-3-phenylancryic acetates are composite, and wherein the mass ratio of active ingredient azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate is 1~80: 80~1.
2. bactericidal composition according to claim 1, it is characterized in that: the quality optimization ratio of azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate is 1~40: 40~1.
3. bactericidal composition according to claim 1, it is characterized in that: azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate account for 1%~80% of the whole quality of the pharmaceutical preparations.
4. bactericidal composition according to claim 3, it is characterized in that: azoles bacterium ester and 2-cyano-3-amino-3-phenylancryic acetate account for 5%~50% of the whole quality of the pharmaceutical preparations.
5. according to claim 1 and 2 or 3 or 4 described bactericidal compositions, it is characterized in that: the formulations of pesticide that this bactericidal composition can be prepared into are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.
CN 201210448920 2012-11-10 2012-11-10 Sterilization composition containing pyraoxystrobin and JS399-19 Pending CN103039459A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106359418A (en) * 2016-08-25 2017-02-01 安徽美兰农业发展股份有限公司 JS399-19 and pyraclostrobin compound suspension agent and preparation method thereof
CN108849936A (en) * 2018-07-10 2018-11-23 江西正邦作物保护有限公司 A kind of bactericidal composition and its application containing tetramycin and pyraoxystrobin

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106359418A (en) * 2016-08-25 2017-02-01 安徽美兰农业发展股份有限公司 JS399-19 and pyraclostrobin compound suspension agent and preparation method thereof
CN108849936A (en) * 2018-07-10 2018-11-23 江西正邦作物保护有限公司 A kind of bactericidal composition and its application containing tetramycin and pyraoxystrobin

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Application publication date: 20130417