CN103875695A - Sterilization composite containing propiconazole and thiophanate methyl - Google Patents
Sterilization composite containing propiconazole and thiophanate methyl Download PDFInfo
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- CN103875695A CN103875695A CN201210556159.2A CN201210556159A CN103875695A CN 103875695 A CN103875695 A CN 103875695A CN 201210556159 A CN201210556159 A CN 201210556159A CN 103875695 A CN103875695 A CN 103875695A
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- thiophanate
- propiconazole
- methyl
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Abstract
The invention relates to a sterilization composite having synergistic interaction effect, its effective active components are propiconazole and thiophanate methyl, wherein the weight ratio of propiconazole and thiophanate methyl is 1: 1-1: 10, an auxiliary agent and an excipient are added in the effective active component to prepare a suspoemulsion or microcapsule suspension-suspoemulsion, and the sterilization composite is used for preventing and treating the diseases due to Ascomycetes, Basidiomycetes and imperfect fungi pathogen.
Description
Technical field
The invention belongs to technical field of pesticide, relate to the application of a kind of bactericidal composition that contains propiconazole and thiophanate-methyl in crop pest.
Technical background
Propiconazole (propiconazol) is azoles fungicide.Molecular formula is C
15h
17o
2n
3cl
2, chemical name: 1-[2-(2,4-dichlorophenyl)-4-propyl group-DOX-Alpha-Methyl] and-1-hydrogen-1,2,4-triazole.
Propiconazole is a kind of have protection and interior absorption triazole bactericidal agent of therapeutic action, can be absorbed by root, stem, leaf portion, and can be very fast in plant body on conduct.It is sterol deoxidation methylation inhibitor.In antithetical phrase, due to the germ of Gammaproteobacteria, Basidiomycetes and Fungi Imperfecti, disease is effective, invalid to oomycetes.
Thiophanate-methyl (thiophanate～methyl) belongs to benzimidazole, and molecular formula is (C
12h
14n
4s
2o
4), chemical name: Thiophanate-Methyl.
Thiophanate-methyl is a kind of broad spectrum activity systemic fungicide, can prevent and treat various crop disease, has interior suction, preventive and therapeutic action.It is converted into carbendazim in plant corpus, disturbs the formation of spindle in germ mitosis, affects cell division.
No matter be propiconazole, thiophanate-methyl or other efficient germicides, long-term use separately, easily makes disease develop immunity to drugs, and causes the problem that dosage strengthens, preventive effect reduces, the lasting period shortens, and is unfavorable for environment sustainable development.The active ingredient of the different mechanisms of action is carried out composite, is to delay the disease conventional method that develops immunity to drugs, and according to the effect in production application, judge this composite be synergistic effect or antagonism.Complex role is significantly filled a prescription, and can obviously improve preventive effect, greatly reduces the dosage of agricultural chemicals, also can expand fungicidal spectrum, improves germicidal efficiency.Propiconazole is different from the thiophanate-methyl mechanism of action, and mutually composite have good synergistic effect within the specific limits.And about composite suspension emulsion or the microcapsule suspension-suspending agent made of propiconazole and thiophanate-methyl, there is not yet at present relevant report at home and abroad.
Summary of the invention
The object of the invention is to propose a kind of have synergistic function, use cost is low, preventive effect the is good bactericidal composition that contains propiconazole and thiophanate-methyl.
The present invention is achieved through the following technical solutions:
A kind of bactericidal composition containing propiconazole and thiophanate-methyl, the weight ratio that it is characterized in that bactericidal composition effective active composition propiconazole and thiophanate-methyl is 1:1 ~ 1 ︰ 10, the weight ratio that is preferably propiconazole and thiophanate-methyl is 1:2 ~ 1 ︰ 9, and more preferably the weight ratio of propiconazole and thiophanate-methyl is 1:3 ~ 1 ︰ 8.
The described bactericidal composition containing propiconazole and thiophanate-methyl, wherein effective active component content accounts for 1～50% of gross weight, is preferably 10～45%.
The described bactericidal composition containing propiconazole and thiophanate-methyl is made suspension emulsion or microcapsule suspension-suspending agent.
When making suspension emulsion, composition comprises following constituent content: propiconazole 1% ~ 50%, thiophanate-methyl 1% ~ 50%, dispersant 2% ~ 10%, defoamer 0.01% ~ 2%, solvent 1% ~ 15%, thickener 0 ~ 2%, emulsifier 2% ~ 12%, antifreeze 0 ~ 8%, deionized water add to 100%.
Dispersant, defoamer, thickener, antifreeze, stabilizing agent in above-mentioned formulation material are mixed through high speed shear, add thiophanate methyl raw pesticide, ball milling 2 ~ 3 hours in ball mill, make diameter of particle all below 5 μ m, make thiophanate-methyl suspending agent, then by propiconazole, emulsifier and various auxiliary agent with the direct emulsification of high speed agitator in suspending agent, make the suspension emulsion product of the present composition.
When making microcapsule suspension-suspending agent, composition comprises following constituent content: propiconazole 1% ~ 50%, thiophanate-methyl 1% ~ 50%, macromolecule cyst material 2% ~ 10%, dispersant 1% ~ 12%, wetting agent 1% ~ 8%, organic solvent 1% ~ 15%, emulsifier 1% ~ 6%, defoamer 0.01% ~ 2%, thickener 0 ~ 2%, pH adjusting agent 0.01% ~ 5%, deionized water add to 100%;
Adopt interfacial polymerization, to in above-mentioned formula, there be propiconazole, macromolecule cyst material, organic solvent to mix, make to be dissolved into even oil phase, oil phase is joined in the aqueous phase solution that contains emulsifier, pH adjusting agent, dispersant under shearing condition, bi-material reacts at oil-water interfaces, form macromolecule cyst wall around the drop that contains chemical substance, make propiconazole microcapsule suspending agent.Dispersant, wetting agent, defoamer, thickener, antifreeze are mixed through high speed shear, add thiophanate methyl raw pesticide, ball milling 2 ~ 3 hours in ball mill, make diameter of particle all below 5 μ m, make thiophanate-methyl suspending agent, then join in the aqueous phase solution of propiconazole microcapsule suspending agent being dissolved in thiophanate-methyl suspending agent stable in water, make the finely disseminated microcapsule suspension-suspending agent of present composition product.
Described dispersant is selected from alkylnaphthalene sulfonate, two (alkyl) naphthalenesulfonate formaldehyde condensation compound, naphthalene sulfonic acid-formaldehyde condensation product, aryl phenol polyoxyethylene succinate sulfonate, octylphenol polyethylene oxyethylene group ether sulfate, polycarboxylate, lignosulfonates, alkylaryl APEO, aliphatic alcohol polyethenoxy base ether, the phonetic formaldehyde condensation products sulphate of alkylphenol-polyethenoxy, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol-polyethenoxy is phonetic, aliphatic amine polyoxyethylene is phonetic, polyoxyethylene carboxylate, one or more during ester polyoxyethylene is phonetic.
Described wetting agent is selected from: lauryl sodium sulfate, neopelex, Nekal BX, wetting and penetrating agent F, spaonin powder, sldium lauryl sulfate, tea are withered, one or more in silkworm excrement, soapberry powder.
Described thickener is selected from: one or more in CMC, hydroxyethylcellulose, Magnesiumaluminumsilicate, gelatin, melon glue, gum Arabic, xanthans, sodium phosphate trimer, phenolic resins, sodium alginate, white dextrin, methylcellulose, PAA, polyvinylpyrrolidone, crospolyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol.
Described antifreeze is selected from: one or more in glycerine, ethylene glycol, propane diols, glycerine, diethylene glycol (DEG), triethylene glycol, polyethylene glycol.
Described defoamer is selected from: silicone, C
8 ~ 10aliphatic alcohols, C
10 ~ 20one or more in saturated fat acids (as capric acid) and acid amides, silicone oil, silicone compound.
Described emulsifier is selected from: agriculture breast 500#(alkyl benzene calcium sulfonate), OP series phosphate (polyoxyethylene nonylphenol ether phosphate), 600# phosphate (phenyl phenol polyoxy ethyl ether phosphate), styrene polyoxyethylene ether ammonium sulfate salt, alkyl biphenyl ether disulfonic acid magnesium salts, triethanolamine salt, agriculture breast 400#(benzyl dimethyl phenol polyoxy ethyl ether), agriculture breast 600#(phenyl phenol polyoxy ethyl ether), Nongru-700 #(alkylphenol-formaldehyde resin polyoxy ethyl ether), agriculture breast 36#(phenethyl fluosite polyoxy ethyl ether), agriculture breast 1600#(phenethyl phenol polyoxy ethyl polypropylene-base ether), ethylene oxide-propylene oxide block copolymer, OP series (polyoxyethylene nonylphenol ether), By series (castor oil polyoxyethylene ether), agriculture breast 33#(alkylaryl polyoxyethylene polyoxypropylene ether), agriculture breast 34#(alkylaryl polyoxyethylene poly-oxygen propylene aether), sapn series (sorbitan monostearate), tween series (sorbitan fatty acid ester APEO), one or more in AEO series (fatty alcohol-polyoxyethylene ether).
Described macromolecule cyst material is selected from one or more in urea, formaldehyde, PIC, polyfunctional group acyl halide polyamines, polyfunctional group acyl halide dihydroxylic alcohols, sodium alginate, polyvinyl alcohol, gelatin, gum Arabic, sucrose, modified starch, maltose, distortion milk protein, glycerine, calcium chloride, carboxymethyl cellulose, beta-schardinger dextrin-.
Described solvent is selected from pine slurry butyl ester, TOFA fatty acid ester, cocoa butter heptyl ester, tall oil fatty acid ester, white oil, petroleum hydrocarbon, fatty acid ester, linseed oil, methyl oleate, cocoa butter, palm oil, rapeseed oil, rape-seed oil methyl ester, vegetable oil carboxylate, triglyceride, mineral oil, vegetable oil, soybean oil, corn oil.
Suspension emulsion the key technical indexes of the present invention:
Microcapsule suspension-suspending agent the key technical indexes of the present invention:
Beneficial effect of the present invention: (1) present composition effective active composition propiconazole and thiophanate-methyl belong to the bactericide of two kinds of different mechanisms of action, and both mutual mixtures can not produce conflict; (2) present composition has good synergistic effect within the specific limits, and preventive effect is higher than single dose, and dosage is little; (3) the present invention not with an organic solvent, is difficult for producing poisoning, is convenient to transportation and storage; (4) present composition has special efficacy to powdery mildew, rust, banded sclerotial blight, leaf spot;
The advantage of microcapsule suspension-suspending agent of the present invention: after (1) dispenser, active ingredient discharges slowly, and the lasting period reaches more than 120 ~ 150 days, not only saves medicament but also save man-hour, and insect is also difficult for developing immunity to drugs.(2) improved the stability of active component.(3) active component is wrapped in cyst wall and has improved safety, has realized that high-toxic pesticide is low to be poisoned.(4) the present invention has reduced the stimulus to the sense organ of pyrethrin pesticide to human body, has covered the bad smell of former medicine.(5) reduced the poisoning to crop, be processed into after microcapsule suspending agent, active ingredient is wrapped in cyst material, and active component can directly not contact target biology, can alleviate poisoning, is beneficial to environmental protection.Consumption of organic solvent reduces, to person poultry safety, can avoid medicament to kind, the harm of seedling, without poisoning.
Of the present invention is also the environmental protection formulation of finding through inventor's lot of experiments by suspension emulsion, do not add any organic solvent, make preparation have good adhesivity and plate-out ability, easily adhere to wax or smooth blade face, preparation stability and anti-rain scouring capability strengthen, enter aqueous dispersion excellent, be cloud and disperse, stable in properties, there will not be layering and sedimentation problem in storage process, heat storage resolution ratio is low, and cost is low; Liquid is easily penetrated into target, and drug effect is high, without bad smell; Environmental protection, storing safety.And synergistic effect is remarkable, the lasting period is long, has the advantages such as the dosage of reduction.
Embodiment
Below in conjunction with embodiment, to further instruction of the present invention, the percentage in embodiment is all weight percentage, but the present invention is not limited thereto.
The embodiment of the present invention is the method that adopts Toxicity Determination and field trial to combine.
Implementation of an application example one the implementation of Formulation Example
Embodiment 1～8 suspension emulsion
Dispersant, defoamer, thickener (can add and can not add), antifreeze (can add and can not add) are mixed through high speed shear, add thiophanate-methyl, ball milling 2 ~ 3 hours in ball mill, make diameter of particle all below 5 μ m, make thiophanate-methyl suspending agent, then by propiconazole, solvent, emulsifier and various auxiliary agent with the direct emulsification of high speed agitator in suspending agent, surplus is supplied by deionized water, make suspension emulsion product of the present invention, specifically in table 1,2.
The each component of table 1 embodiment 1～4 and weight portion
The each component of table 2 embodiment 5～8 and weight portion
Embodiment 9～16 microcapsule suspensions-suspending agent
By propiconazole, macromolecule cyst material, solvent, make to be dissolved into even oil phase, oil phase is joined in the aqueous phase solution that contains emulsifier, pH adjusting agent under shearing condition, make finely disseminated microcapsule suspending agent.Dispersant, wetting agent, defoamer, thickener (can add and can not add) are mixed through high speed shear, add thiophanate-methyl, ball milling 2 ~ 3 hours in ball mill, make diameter of particle all below 5 μ m, make suspending agent, then suspending agent is joined in the aqueous phase solution of micro-capsule suspension, deionized water is supplied surplus, make the finely disseminated microcapsule suspension-suspending agent of present composition product, specifically in table 3,4.
The each component of table 3 embodiment 9-12 and weight portion
The each component of table 4 embodiment 13-16 and weight portion
Implementation of an application example two: propiconazole and thiophanate-methyl are composite to Rhizoctonia solani Kuhn Toxicity Determination
Test medicine provides by Shanxi Thompson Biological Technology Co., Ltd..
After the effective inhibition concentration scope of each medicament is determined in prerun, each medicament is established respectively 5 dosage processing by active constituent content, establishes clear water contrast.Carry out with reference to " farm-chemical indoor determination test rule bactericide ", adopt mycelial growth rate method to measure the virulence of medicament to Rhizoctonia solani Kuhn.After 72h, measure colony diameter by right-angled intersection method, calculate each processing net growth, mycelial growth inhibition rate.
Net growth (mm)=measurement colony diameter-5
Mycelial growth inhibition rate is converted into probit value (y), and liquor strength (μ g/mL) converts logarithm value to (x), tries to achieve virulence regression equation (y=a+bx) with method of least squares, and calculates thus the EC of every kind of medicament
50value.Calculate the different proportioning synergy ratios of two medicaments (SR) according to Wadley method, SR < 0.5 is antagonism simultaneously, and 0.5≤SR≤1.5 are summation action, and SR > 1.5 is synergistic effect.Computing formula is as follows:
Wherein: a, b are respectively propiconazole and thiophanate-methyl shared ratio in combination
A is propiconazole
B is thiophanate-methyl
Result of the test is as shown in table 5:
Table 5 propiconazole, thiophanate-methyl and the composite toxicity test analysis of results table to Rhizoctonia solani Kuhn thereof
As shown in Table 5, propiconazole, thiophanate-methyl are respectively 0.62mg/L and 5.34mg/L to the EC50 of Rhizoctonia solani Kuhn.The virulence of propiconazole is higher than the virulence of thiophanate-methyl.The synergy ratio of propiconazole and thiophanate-methyl proportioning 1:1,1:2,1:3,1:4,1:5,1:6,1:7,1:8,1:9,1:10 is respectively 1.71,1.94,2.19,2.33,2.24,2.19,2.07,1.95,1.86,1.79, illustrate that propiconazole and thiophanate-methyl mixture in 1 ︰ 1 to 1 ︰ 10 scopes all shows obvious synergistic effect, wherein synergy ratio SR maximum in the time that propiconazole and thiophanate-methyl weight ratio are 1 ︰ 4, synergistic effect is the most obvious.
Embodiment applies three propiconazoles and thiophanate-methyl and the composite rice sheath blight disease test of pesticide effectiveness of preventing and treating thereof
This experimental establishment is at Shaanxi Province's Hanzhong City, and test medicine is researched and developed, provided by Shanxi Thompson Biological Technology Co., Ltd., contrast medicament 25% propiconazole emulsifiable concentrate (commercial), 70% thiophanate-methyl water dispersible granules (commercial).
Investigation rice sheath blight disease disease index before medicine, in their early stage dispenser, once, dispenser 2 times altogether, investigates disease indexs and calculates preventive effect for after last dispenser 7 days, 15 days, 30 days in dispenser in every 7 days.Experimental result is as follows:
Table 6 propiconazole, thiophanate-methyl and the composite rice sheath blight disease test of pesticide effectiveness of preventing and treating thereof
As can be seen from Table 6, after propiconazole and thiophanate-methyl are composite, can effectively prevent and treat rice sheath blight disease, control efficiency is all better than contrasting medicament, and the lasting period is long.In test scope of medication, target crop is had no adverse effects.Implementation of an application example four propiconazoles and thiophanate-methyl and the composite control Rice Leaf rot test of pesticide effectiveness thereof
This experimental establishment is at Shaanxi Province's Hanzhong City, and test medicine is researched and developed, provided by Shanxi Thompson Biological Technology Co., Ltd., contrast medicament 25% propiconazole emulsifiable concentrate (commercial), 70% thiophanate-methyl water dispersible granules (commercial).
In the dispenser of Rice Leaf rot their early stage, once, dispenser 2 times altogether, investigates disease index before dispenser, within after the 2nd dispenser 10 days, 20 days, 30 days, investigate respectively disease index, and calculation correction preventive effect in dispenser in every 7 days, and result of the test is as follows:
Table 7 propiconazole and thiophanate-methyl and the composite control Rice Leaf rot test of pesticide effectiveness thereof
As can be seen from Table 7, propiconazole, thiophanate-methyl energy effectively preventing Rice Leaf rot, control efficiency is all better than contrasting medicament, dosage is little, test scope of medication in to target crop without harm.
Implementation of an application example five propiconazoles and thiophanate-methyl and composite wheat rust, the leaf spot test of pesticide effectiveness of preventing and treating thereof
This experimental establishment is in Sanyuan County, Xianyang, Shanxi province city, and test medicine is researched and developed, provided by Shanxi Thompson Biological Technology Co., Ltd., contrast medicament 25% propiconazole emulsifiable concentrate (commercial), 70% thiophanate-methyl water dispersible granules (commercial).
In wheat rust, the dispenser of leaf spot their early stage, once, dispenser 2 times altogether, investigates disease index before dispenser, within after the 2nd dispenser 10 days, 20 days, 30 days, investigate respectively disease index, and calculation correction preventive effect in dispenser in every 7 days, and result of the test is as follows:
Table 8 propiconazole and thiophanate-methyl and composite wheat rust, the leaf spot test of pesticide effectiveness of preventing and treating thereof
As can be seen from Table 8, propiconazole, thiophanate-methyl energy effectively preventing wheat rust, leaf spot, control efficiency is all better than contrasting medicament, dosage is little, test scope of medication in to target crop without harm.
Implementation of an application example six propiconazoles, thiophanate-methyl and the composite control wheat powdery mildew test of pesticide effectiveness thereof
This experimental establishment is in Chencang District, Baoji, Shaanxi province city, and test medicine is researched and developed, provided by Shanxi Thompson Biological Technology Co., Ltd., contrast medicament 25% propiconazole emulsifiable concentrate (commercial), 70% thiophanate-methyl water dispersible granules (commercial).
Investigation wheat powdery mildew state of an illness radix, total number of sheets, the sick number of sheets and sick leaf-size class number before medicine, in their early stage dispenser, once, dispenser 2 times, investigates respectively disease index and calculates preventive effect for after dispenser 10 days, 20 days, 30 days for the second time altogether in dispenser in every 7 days.Experimental result is as follows:
Table 9 propiconazole and thiophanate-methyl and the composite control wheat powdery mildew test of pesticide effectiveness thereof
As can be seen from Table 9, can effectively prevent and treat wheat powdery mildew and occur after propiconazole and thiophanate-methyl are composite, control efficiency is all better than contrasting medicament, in this test scope of medication, target crop is had no adverse effects.
Claims (8)
1. containing a bactericidal composition for propiconazole and thiophanate-methyl, the weight ratio that it is characterized in that bactericidal composition effective active composition propiconazole and thiophanate-methyl is 1:1 ~ 1 ︰ 10.
2. the bactericidal composition containing propiconazole and thiophanate-methyl according to claim 1, is characterized in that: wherein the weight ratio of propiconazole and thiophanate-methyl is 1:2 ~ 1 ︰ 9.
3. the bactericidal composition containing propiconazole and thiophanate-methyl according to claim 2, is characterized in that: wherein the weight ratio of propiconazole and thiophanate-methyl is 1:3 ~ 1 ︰ 8.
4. the bactericidal composition containing propiconazole and thiophanate-methyl according to claim 1, is characterized in that: bactericidal composition is made suspension emulsion or microcapsule suspension-suspending agent.
5. the bactericidal composition containing propiconazole and thiophanate-methyl according to claim 1, is characterized in that: wherein effective active component content accounts for 1～50% of gross weight.
6. the bactericidal composition containing propiconazole and thiophanate-methyl according to claim 5, is characterized in that: wherein effective active component content accounts for 10～45% of gross weight.
7. the bactericidal composition containing propiconazole and thiophanate-methyl according to claim 1 is for preventing and treating the application of corps diseases.
8. application according to claim 7, is characterized in that: described disease is powdery mildew, rust, banded sclerotial blight, leaf spot or leaf blight.
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|---|---|---|---|
| CN201210556159.2A CN103875695A (en) | 2012-12-19 | 2012-12-19 | Sterilization composite containing propiconazole and thiophanate methyl |
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|---|---|---|---|
| CN201210556159.2A CN103875695A (en) | 2012-12-19 | 2012-12-19 | Sterilization composite containing propiconazole and thiophanate methyl |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106472540A (en) * | 2016-08-31 | 2017-03-08 | 柳州市惠农化工有限公司 | A kind of composition pesticide disliking bacterium azoles and thiophanate-methyl containing dichloro |
| CN109832282A (en) * | 2019-03-22 | 2019-06-04 | 江苏禾本生化有限公司 | A kind of compound disinfectant and preparation method thereof containing propiconazole |
| CN115316395A (en) * | 2022-08-26 | 2022-11-11 | 浙江禾本科技股份有限公司 | Preparation method of azoxystrobin and propiconazole bactericidal composition suspending agent |
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| CN101822264A (en) * | 2010-02-03 | 2010-09-08 | 陕西美邦农资贸易有限公司 | Bactericidal composition with pyriproxyfen and thiophanate-methyl |
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| CN106472540A (en) * | 2016-08-31 | 2017-03-08 | 柳州市惠农化工有限公司 | A kind of composition pesticide disliking bacterium azoles and thiophanate-methyl containing dichloro |
| CN109832282A (en) * | 2019-03-22 | 2019-06-04 | 江苏禾本生化有限公司 | A kind of compound disinfectant and preparation method thereof containing propiconazole |
| CN115316395A (en) * | 2022-08-26 | 2022-11-11 | 浙江禾本科技股份有限公司 | Preparation method of azoxystrobin and propiconazole bactericidal composition suspending agent |
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Application publication date: 20140625 |