CN102007929B - Thifluzamide-containing bactericidal composition - Google Patents
Thifluzamide-containing bactericidal composition Download PDFInfo
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- CN102007929B CN102007929B CN 201010583221 CN201010583221A CN102007929B CN 102007929 B CN102007929 B CN 102007929B CN 201010583221 CN201010583221 CN 201010583221 CN 201010583221 A CN201010583221 A CN 201010583221A CN 102007929 B CN102007929 B CN 102007929B
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- thifluzamide
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Abstract
The invention relates to a bactericidal composition in the field of pesticide compounding. The composition comprises the active ingredients of compounded thifluzamide and thiophanate methyl, wherein the weight percentage ratio of the two active ingredients is 50:1 to 1:80, preferably 20:1 to 1:30; the active ingredients account for 1 to 85 percent of the total weight of the bactericidal composition, preferably 1 to 35 percent; and the balance is auxiliary components which are permitted to be used and are acceptable in pesticides. Wettable powder, suspending agents, powder, microemulsion, emulsion in water and water dispersible granules can be prepared by known methods. The bactericidal composition is mainly used for preventing and controlling fungal and bacterial diseases on cereals, vegetables and fruit trees, particularly for preventing and controlling rice sheath blight and false smut.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, be specifically related to a kind of thifluzamide and composite bactericidal composition of thiophanate-methyl of containing.
Background technology
Thifluzamide, English name thifluzamie, chemical name: 2 ', 6 '-two bromo-2-methyl-4 '-three furan methoxyl group-4-three furan methyl isophthalic acids, 3-thiadiazoles-5-hydroxyl anilide; The thiophene methuroxam, chemical structural formula:
Thifluzamide; belong to the thifluzamide series bactericidal agent and have strong interior conductivity and the long lasting effect of inhaling; it is the succinate dehydrogenase inhibitor; by suppressing mitochondrial succinate ester dehydrase; hinder tricarbonic acid cycle; make amino acid; sugar lacks energy to be reduced; the division of interference cell and growth; disease there is neural activity, suppresses spore germination; the bacterium pipe extends; mycelial growth and spore mother cell form the Main Stage of conk and breeding, and bactericidal action is directly caused by the parent active substance; there is not corresponding metabolic activity; have protection and therapeutic action, absorb the back and in plant, shift the distribution leaf by the blade face infiltration; flower; really.Be mainly used in the control of rice sheath blight disease at present.This compound effects mode is single, uses pesticide resistance risk height separately.
Thiophanate-methyl (thiophanate-methyl), two (3-methoxycarbonyl-2-the ghiourea group)-benzene of chemical name: 1,2-, belong to benzimidazole germicide, be a kind of broad spectrum activity systemic fungicide, can prevent and treat the various crop disease, have interior suction, preventive and therapeutic action.It is converted into carbendazim in plant corpus, the formation of spindle influences cell division in the mitosis of interference bacterium.Multiple diseases on cereal class, greengrocery, the fruit tree there is the better prevention effect.As vegetable disease, prevent and treat powdery mildew of cucumber, anthracnose, gray mold, anthracnose, stalk breaks such as eggplant, onion, celery, tomato, Kidney bean, fruit tree kind disease such as pear tree ring spot, anthracnose; The brown spot of grape, strawberry, anthracnose, gray mold, peach brown rot etc., the mould in the citrus storage, green mould; Stinking smut, head blight, powdery mildew, rice blast, banded sclerotial blight etc.
No matter be thifluzamide, thiophanate-methyl or other efficient germicides, long-term use separately makes disease develop immunity to drugs easily, 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 method commonly used that develops immunity to drugs, and according to the effect in the production application, judge this composite be synergistic effect or antagonism.Complex role is more significantly filled a prescription, and can obviously improve preventive effect, reduces the dosage of agricultural chemicals greatly, also can enlarge fungicidal spectrum, improves germicidal efficiency.Thifluzamide is different with the thiophanate-methyl mechanism of action, and mutually composite have good synergistic effect within the specific limits.And composite about thifluzamide and thiophanate-methyl do not see relevant report at present at home and abroad as yet.
Summary of the invention
Based on above situation, the objective of the invention is to rationally be mixed by thifluzamide and thiophanate-methyl, obtain a kind of bactericidal composition, be used for preventing and treating the disease on the agricultural, in particular for preventing and treating rice sheath blight disease, false smut, fruit tree, vegetables, other crop fungies of cereal class, bacteriosis, delay the drug-fast generation of germ, enlarge fungicidal spectrum and reduce drug cost, improve actual preventive effect.
The present invention for a kind of be the composite bactericidal composition that forms of active ingredient with thifluzamide and thiophanate-methyl, the objective of the invention is to realize by following measure:
Composition pesticide of the present invention is characterized in that with thifluzamide (A) and thiophanate-methyl (B) be that active ingredient is mixed, and the mass ratio of effective constituents A and B is 50: 1～1: 80.
As a kind of improvement of the present invention, preferred 20: 1～1: 30 of the mass ratio of effective constituents A and B.
Composition pesticide of the present invention can be prepared into wetting powder, suspending agent, pulvis, microemulsion, aqueous emulsion and water dispersible granules with known method, the quality percentage composition of active ingredient is 1%～85% in the preparation, be preferably 1%～35%, all the other are usual auxiliaries in the agricultural chemicals.
Specific embodiments of the present invention is as follows:
One of technical scheme of the present invention, described bactericidal composition are wetting powder, and the percentage by weight of component is:
Thifluzamide 1～50%
Thiophanate-methyl 1～80%
Dispersant 3～20%
Wetting agent 3～10%
Filler 10～70%
The concrete procedure of processing of this bactericidal composition wetting powder is: press above-mentioned prescription with thifluzamide and thiophanate-methyl and dispersant, wetting agent and filler mixing, in stirred tank, evenly stir, behind airslide disintegrating mill, mixing, namely can be made into the wetting powder of the present composition.
Two of technical scheme of the present invention, described bactericidal composition are suspending agent, and the percentage by weight of component is:
Thifluzamide 1～50%
Thiophanate-methyl 1～80%
Dispersant 5～20%
Antifreezing agent 1～5%
Thickener 0.1～2%
Defoamer 0.1～0.8%
Water surplus
The concrete production stage of this suspending agent is earlier other auxiliary agents to be mixed, mix through high speed shear, add thifluzamide and thiophanate-methyl, abrading-ball is 2～3 hours in ball crusher, make a diameter all below 5mm, make the suspending agent preparation that contains the bactericidal composition of thifluzamide and thiophanate-methyl of the present invention.
Three of technical scheme of the present invention, described bactericidal composition are aqueous emulsion, and the percentage by weight of component is:
Thifluzamide 1～50%
Thiophanate-methyl 1～80%
Emulsifier 3～30%
Solvent 5～15%
Stabilizing agent 2～15%
Antifreezing agent 1～5%
Defoamer 0.1～8%
Thickener 0.2～2%
Water surplus
The concrete production stage of this aqueous emulsion is: at first former medicine thifluzamide and thiophanate-methyl, solvent and emulsifier, cosolvent are added together, make and be dissolved into uniform oil phase; With part water, antifreeze, other insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water until reaching the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear half an hour approximately, form the aqueous emulsion of oil-in-water type.Namely make the aqueous emulsion of the bactericidal composition that contains thifluzamide and thiophanate-methyl.
Four of technical scheme of the present invention, described bactericidal composition are water dispersible granules, and the percentage by weight of component is:
Thifluzamide 1～50%
Thiophanate-methyl 1～80%
Dispersant 3～20%
Wetting agent 3～10%
Disintegrant 2～5%
Filler 10～70%
The concrete procedure of processing of this bactericidal composition water dispersible granules is: by above-mentioned prescription thifluzamide, thiophanate-methyl and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, add then and carry out granulation, drying, screening in the fluidized bed prilling dryer by sample analysis, make the water dispersible granules that contains the bactericidal composition of thifluzamide and thiophanate-methyl of the present invention.
Described emulsifier is selected from any one or more mixtures formed with arbitrary proportion in calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkylphenol polyoxyethylene sulfosuccinate, styryl phenol APEO, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, the polyoxyethylene aliphatic alcohol ether.
Described solvent is any one or more mixed solvents formed with arbitrary proportion in dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), the water equal solvent.
Described dispersant is selected from one or more in polycarboxylate, lignosulfonates, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, aliphatic amine polyoxyethylene ether, polyoxyethylene carboxylate, the fatty acid glyceride APEO.
Described wetting agent is selected from: lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX., among the wetting and penetrating agent F, alkylnaphthalene sulfonate, polyoxyethylene triphenylethylene phosphenylic acid salt, spaonin powder, silkworm excrement, soapberry powder one or more.
Described disintegrant is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, the sodium bicarbonate.
Described thickener is selected from: one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose, Magnesiumaluminumsilicate, the polyvinyl alcohol.
Described stabilizing agent is selected from: a kind of in sodium citrate, the resorcinol.
Described antifreezing agent is selected from: one or more in ethylene glycol, propane diols, the glycerine.
Described defoamer is selected from: silicone oil, silicone compound, C
10-20Saturated fat acid compounds, C
8-10In the aliphatic alcohols compound one or more.
Described filler is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, the precipitated calcium carbonate.
Composition pesticide of the present invention can be used for preventing and treating the disease on the various plants such as vegetables, fruit tree, cereal, ornamental plants, for example prevents and treats early blight and late blight, alternaria leaf spot of apple, downy mildew of garpe, pear scab, wheat rust, melon anthracnose and downy mildew, rice sheath blight disease and the rice blast etc. of the early blight of tomato and late blight, potato.Wherein the control efficiency to rice sheath blight disease and rice blast is remarkable.
Embodiment:
In order to make purpose of the present invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention only limits to these examples absolutely not.The method that the present invention adopts indoor bioassay and field trial to combine.If no special instructions, the ratio of below mentioning (comprising percentage) all is percentage by weight.
The synergy test that thifluzamide and thiophanate-methyl are composite.It is tested object that Rhizoctonia solani Kuhn is adopted in test.
Concrete grammar is:
(1) test medicine
The former medicine of 96% thifluzamide is produced by The Dow Agrosciences, LLC.; The former medicine of 95% thiophanate-methyl, Guangxin, Anhui farmingization limited company produces;
Thifluzamide and thiophanate-methyl dissolve with proper amount of acetone, are made into the mother liquor of 10000 μ g/ml, preserve in 4 ℃ of following low temperature, and be stand-by, is diluted to a series of concentration with sterile water before the test.
(2) subjects
The Rhizoctonia solani Kuhn germ, separation and purification gained from the incidence of leaf of Hunan paddy field is cultivated in 4 ℃ of refrigerators on the PDA inclined-plane and is preserved.
PDA medium: potato 200g, glucose 20g, agar 20g, water 1000ml
AEA medium: dusty yeast 5g/L, glycerine 20mL/L, Mg SO
40.25g/L, Na NO
36g/L, KCL0.5g/L, KH
2PO
41.5g/L, agar powder 20g/L, deionized water 1L
(3) test method
Rhizoctonia solani Kuhn after pre-cultivation the on the AEA medium, is inoculated in the bacterium dish of diameter 5mm respectively on the AEA flat board that contains the variable concentrations gradient, under 25 ℃ of dark conditions, cultivates.Every processing repeats 3 times.When control strain colony diameter length is above to 6.5c m, adopt " right-angled intersection method " to measure.According to the linear regression analysis between the logarithm value of the probit value of inhibiting rate and medicine series concentration, obtain the EC that two kinds of single agent suppress mycelial growths
50Value, correlation coefficient and virulence regression equation.
On the basis of preliminary experiment, respectively single agent thifluzamide and thiophanate-methyl are carried out toxicity test in order to last method, the two EC
50Value is respectively 0.5mg/L and 6.2mg/L.
Test was respectively 1: 5,1: 3,1: 1,3: 1,5: 1 i.e. 2.5%+12.5%, 3.75%+11.25%, 7.5%+7.5%, 11.25%+3.75%, 12.5%+2.5% totally 5 combinations that are mixed with 15% thifluzamide thiophanate-methyl mass ratio.
(4) data statistics and analysis
Carry out the toxicity test of mixture according to mixed ratio with single agent toxicity test method.
EC that each that will measure according to the abundant method of Sun Yun handled
50Value is converted into the actual toxicity index (ATI) of using with; According to the proportioning of mixture, obtain theory and use toxicity index (TTI) with, calculate the co-toxicity coefficient (CTC) of mixture by following formula.
Single agent toxicity index=(standard medicament EC
50/ reagent agent EC
50) * 100
ATI=(standard medicament EC
50/ reagent agent (using with) EC
50) * 100
The content (%) of toxicity index XB in using with of content (the %)+B of the toxicity index x A of TI I=A in using with
CTC＝(ATI/TTI)*100
If co-toxicity coefficient is big by 120, showing has synergistic effect; If be starkly lower than 100 (below 80), be indicated as antagonism; Between 100～120, be indicated as summation action.Data see Table 1,2.
(5) toxicity test result and analysis
The composite virulence to Rhizoctonia solani Kuhn of table 1 thifluzamide and thiophanate-methyl
The composite co-toxicity to Rhizoctonia solani Kuhn of table 2 acid amides and thiophanate-methyl
According to bactericide joint toxicity measuring result, thifluzamide and thiophanate-methyl mass ratio are that the co-toxicity coefficient when being 2.5%+12.5% at 1: 5 is 136.9, obviously big by 120, show as synergistic effect, think that thifluzamide and thiophanate-methyl mass ratio are that 1: 5 o'clock synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 1: 5 left and right sides scope of suitable proportion, to estimate its field practical application effect.
Test example 1: field trial is measured the rice sheath blight disease controlling effect
(1) test method
Test dispenser twice altogether, check plot spray equivalent clear water.When making up a prescription, after with low amounts of water medicament fully being dissolved earlier, add suitable quantity of water again and carry out complete stool spraying processing, even spraying.All adopting power driven sprayer, operating pressure during the spray medicine is 2.0～2.3kg/cm
2, shower nozzle aperture 1.2mm.The residential quarter spouting liquid is used by 675 liters/hectare, and soup is sprayed application to the crop complete stool uniformly.
(2) investigation method
Experimental field be located at the Hunan, publish the medium rice field of course of disease degree for experimental field, soil fertility is medium, and irrigation and drainage are convenient.Adopt the bilinear sampling method, 5 points are got in every residential quarter, look into 5 caves at every, and 2 blades in the fixing middle part of every strain fix a point to check during investigation.
Come classification according to the rice sheath blight disease grade scale, record total strain number, diseased plant number, degree of being in a bad way, calculate diseased plant rate, disease index and preventive effect.
The rice sheath blight disease grade scale is
0 grade: complete stool is anosis;
1 grade: the 4th blade and following each leaf sheath thereof, blade morbidity (be 1st slice leaf with sword-like leave);
3 grades: the 3rd blade and following each leaf sheath thereof, blade morbidity;
5 grades: the 2nd blade and following each leaf sheath thereof, blade morbidity;
7 grades: sword-like leave blade and following each leaf sheath thereof, blade morbidity;
9 grades: the complete stool morbidity, withered ahead of time.
Test is investigated 4 times altogether, i.e. disease index investigation before the medicine, preventive effect investigation in 10 days behind the 1st medicine, 10 days and preventive effect investigation in 20 days behind 2 medicines.
(3) poisoning investigation
Whether continuous 7d range estimation medicament has poisoning to crop after the dispenser.
(4) 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 (%)=(1-(disease index behind disease index before the blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
Each is handled the effect of preventing and treating rice sheath blight disease and sees Table 3
(5) field control effectiveness test result of the test
Each handles the effect of preventing and treating rice sheath blight disease table 3
As shown in Table 3, to prevent and treat the effect of rice sheath blight disease more remarkable in the combination that is mixed of 15% thifluzamide thiophanate-methyl 1: 5.The effect of complex preparation significantly is better than two kinds of single agent, has not only significantly improved the effect for sheath blight fungus, and has further prolonged its lasting period.Simultaneously, under same dosage, 24% thifluzamide list agent significantly is better than 70% thiophanate-methyl list agent for the effect of banded sclerotial blight.
Test example 2: field trial is measured the control efficiency to rice green smut
(1) test method
Test dispenser twice altogether, check plot spray equivalent clear water.When making up a prescription, after with low amounts of water medicament fully being dissolved earlier, add suitable quantity of water again and carry out complete stool spraying processing, even spraying.All adopting power driven sprayer, operating pressure during the spray medicine is 2.0～2.3kg/cm
2, shower nozzle aperture 1.2mm.The residential quarter spouting liquid is used by 675 liters/hectare, and soup is sprayed application to whole rice uniformly.
(2) control time and method
20 clumps of the parallel great-jump-forward investigation in every residential quarter are recorded every clump of sick spike number, sick spike number at different levels and total spike number and are calculated disease tassel yield and disease index.Investigation grade scale following (be unit with the fringe).
0 grade: no infected seed;
1 grade: 1 curve of every fringe;
3 grades: 2 curves of every fringe;
5 grades: 3～5 curves of every fringe;
7 grades: every fringe 6-9 curve;
9 grades: 10 of every fringes are more than the curve;
(3) poisoning investigation
Whether continuous 7d range estimation medicament has poisoning to crop after the dispenser.
(4) drug effect computational methods
Test is investigated 4 times altogether, i.e. disease index investigation before the medicine, preventive effect investigation in 7 days behind the 1st medicine, 7 days and preventive effect investigation in 15 days behind 2 medicines.
Diseased plant rate (%)=sick spike number/investigate total spike number * 100
Disease index=∑ (sick spike numbers at different levels * relative level numerical value)/(investigating total spike number * 9) * 100
Control efficiency (%)=(1-(disease index behind disease index before the blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
Each effect of handling the control rice green smut sees Table 4
(5) field control effectiveness test result of the test
Each handles the effect of control rice green smut table 4
Can be known that by table 4 effect of 1: 5 the combination control rice green smut that is mixed of 15% thifluzamide thiophanate-methyl is very remarkable.Under same 12 milliliters every mu consumption, the effect of complex preparation significantly is better than two kinds of single agent, and its quick-acting and lasting effect are all relatively good, and is the most outstanding with lasting effect especially.Complex preparation significantly is better than effect under the low concentration consumption in control efficiency under the consumption of high concentration.20 days preventive effects reach 85.09% after 10 days control efficiency behind the 1st, 2 medicine reaches 68.08% and 77.64%, the 2 medicine respectively.And single agent 24% thifluzamide SC, 20 days preventive effects are 80.97% after 10 days control efficiency behind the 1st, 2 medicine is respectively 63.70% and 73.42%, the 2 medicine, significantly are better than single agent 70% thiophanate-methyl.
In sum, this complex preparation has remarkable prevention effect to rice sheath blight disease and false smut simultaneously, can effectively suppress further developing of disease, and simultaneously to crop safety, suggestion is promoted the use of.
Claims (2)
1. bactericidal composition that contains thifluzamide, it is characterized in that: the active ingredient of this bactericidal composition is thifluzamide and thiophanate-methyl binary built, wherein total active ingredient is that 15% thifluzamide and the mass ratio of thiophanate-methyl are 1:5.
2. bactericidal composition according to claim 1, it is characterized in that: the formulation of this bactericidal composition is suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.
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| CN102919222A (en) * | 2012-11-20 | 2013-02-13 | 河北三农农用化工有限公司 | Thifluzamide water dispersible granule |
| CN103314954A (en) * | 2013-07-04 | 2013-09-25 | 江苏省绿盾植保农药实验有限公司 | Seed coating agent for preventing rice sheath blight diseases, preparing method and application method thereof |
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