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CN103168785A - Ternary compound sterilizing composition containing trifloxystrobin and application of sterilizing composition - Google Patents

Ternary compound sterilizing composition containing trifloxystrobin and application of sterilizing composition Download PDF

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Publication number
CN103168785A
CN103168785A CN2013100951731A CN201310095173A CN103168785A CN 103168785 A CN103168785 A CN 103168785A CN 2013100951731 A CN2013100951731 A CN 2013100951731A CN 201310095173 A CN201310095173 A CN 201310095173A CN 103168785 A CN103168785 A CN 103168785A
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bactericidal composition
agent
carbendazim
active component
prothioconazoles
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鞠晓东
周彬
钱海宾
许永进
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Jiangsu Sevencontinent Green Chemical Co Ltd
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Jiangsu Sevencontinent Green Chemical Co Ltd
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Abstract

The invention relates to a ternary compound sterilizing composition containing trifloxystrobin and application of the sterilizing composition. The ternary compound sterilizing composition comprises an active component, and auxiliary components of pesticide preparations, wherein the active component is compounded by the trifloxystrobin, prothioconazole and carbendazim according to the weight ratio of (0.1-1): (0.1-1):1. The ternary compound sterilizing composition has the advantages that since the trifloxystrobin, the prothioconazole and the carbendazim are compounded according to the specific proportion, an obvious synergistic interaction effect is obtained; and compared with a sterilizing composition subjected to two-component compounding, the ternary compound sterilizing composition has an expanded bacteriocidal spectrum and has the special effect for diseases such as leaf spot disease, downy mildew, scab and anthracnose of fruit trees, vegetables and cereal crops. In addition, proved by many experiments, the toxicity to mammals is not increased after compounding. An applicant further discovers that the compounding effect of the active component can be further enhanced by means of specific wetting dispersants and dispersing wetting agents, and the synergistic action can be played at the most extent.

Description

A kind of ternary built bactericidal composition and application thereof that contains oxime bacterium ester
Technical field
The invention belongs to pesticide field, particularly a kind of ternary built bactericidal composition and application thereof that contains oxime bacterium ester.
Background technology
Prothioconazoles, English name: prothioconazole, molecular formula: C 14H 15C 12N 3OS, chemical name: (RS)-2-[2-(1-chlorine cyclopropyl)-3-(2-chlorphenyl)-2-hydroxypropyl]-2,4-dihydro-1,2,4-triazole-3-thioketones is a kind of New-type wide-spectrum triazolinthione series bactericidal agent of Beyer Co., Ltd's development.Former medicine is white crystal, has toxicity low, without teratogenesis, and without the mutagenesis type, to embryo's avirulence, the advantage such as safe for human and animal and environment.The mechanism of action of prothioconazoles is the demethylation effect of precursor-lanosterol on methylene lanostenol l4-or 24-position of sterol in Antifungi, i.e. demethylation inhibitor (DMIs).Prothioconazoles not only has good systemic activity, excellent protection, treats and root out activity, and the lasting period is long.By a large amount of field control effectiveness tests, result shows that prothioconazoles not only has good safety to crop, and preventing disease theraping effect is good, and volume increase is obvious, compares with triazole bactericidal agent, and prothioconazoles has the more bactericidal activity of wide spectrum.It is mainly used in preventing and treating cereal crop such as numerous diseases such as wheat, barley, rape, peanut, paddy rice and legume crop.Almost all wheat class diseases there is good control efficiency, as the powdery mildew of Wheat and barley, banded sclerotial blight, fusarium wilt, leaf spot, rust, stalk break, net blotch, moire disease etc.Can also prevent and treat the soil-borne disease of oily Lay and peanut, as stalk break, and main foliage disease, as gray mold, black spot, brown spot, balck shank, stalk break and rust etc.But single dose usage amount and cost are higher, and long-term use can make plant produce resistance, and is also limited to the control efficiency of special crop and different diseases.
At present, have some and carry out composite bibliographical information about prothioconazoles and other bactericide.for example Chinese invention patent application 201110238819.8 discloses a kind of prothioconazoles and triazole bactericidal agent of containing according to the bactericidal composition of the weight ratio composition of proportions of 1: 80~80: 1, wherein active components A is selected from prothioconazoles, active component B is selected from epoxiconazole, a kind of in own azoles alcohol, said composition is used for preventing and treating powdery mildew, banded sclerotial blight, false smut, leaf spot, rust, stalk break, spot defoliation, gray mold, helminthosporium leaf spot, scab, black spot, brown spot, the diseases such as black rot, has dosage little, resistance of rainwater washing against, synergy significantly acts on.Chinese invention patent application 201110237522.X discloses a kind of bactericidal composition that contains prothioconazoles, the active components A of said composition is selected from prothioconazoles, active component B is selected from thiophanate-methyl, carbendazim, a kind of in Prochloraz, wherein the weight ratio of active components A and active component B is 1: 80~80: 1, be used for preventing and treating powdery mildew, banded sclerotial blight, fusarium wilt, leaf spot, rust, stalk break, virus disease, anthracnose, gray mold, ring spot, bakanae disease, rice blast, early blight, green mould, blossom-end rot, penicilliosis, helminthosporium leaf spot, scab, the diseases such as damping off, has dosage little, resistance of rainwater washing against, the obvious characteristics of synergy.also has in addition Chinese invention patent 201110252217.8, 201110247843.8, 201110245251.2, 201110260045.9 and 201110237204.3, 201110247597.6 disclose respectively prothioconazoles and the glyoxalin of performance synergistic effect, penconazole, Triadimenol, bitertanol, Cyproconazole, Flusilazole, Flutriafol, triazolone, propiconazole, tetraconazole, alkene azoles alcohol, nitrile bacterium azoles, cyprodinil, mancozeb, Propineb, the bactericidal composition of zineb and Carbatene.
Oxime bacterium ester, chemical name: methyl (E)-methoxyl group imido grpup-(E)-ɑ-[1-(α, α-three fluoro-m-tolyl)-ethylidene amido oxygen base]-o-tolyl } ethyl acetate, english common name: trifloxystrobin, molecular formula: C 20H 19F 3N 2O 4, molecular weight: 408.3, No. CA: 141517-21-7, white solid, fusing point: 72.9 ℃, boiling point: 312 ℃, be soluble in multiple organic solvent.Oxime bacterium ester belongs to oxime bacterium ester class wide-spectrum bactericide; it is the new fungicides of a class of successfully developing as the bactericide lead compound from natural products strobilurins; characteristics such as having efficient, wide spectrum, protection, treat, root out, infiltration, systemic activity, resistance of rainwater washing against, lasting period are long, with at present existing bactericide without cross resistance.Nearly all Mycophytes (Ascomycetes, Basidiomycetes, Oomycete and Fungi Imperfecti) disease such as powdery mildew, rust, Ying's rot, net blotch, downy mildew, rice blast etc. all there is good activity.Powdery mildew, leaf spot are had outside special efficacy, rust, downy mildew, damping off, apple apple scab are had good activity.To crop safety, capable of being fast degraded in soil, water because of it, therefore environmentally safe.But when alone the sterilization duration short, protection effect is not quite desirable.
Known again, carbendazim (carbendazim), chemical molecular formula are C 9H 9N 3O 2Chemical name: the N-(2-benzimidazolyl)-methyl carbamate; belong to benzimidazole high-efficiency low-toxicity systemic fungicide; interior suction treatment and protective effect are arranged; it can be absorbed by the seed of plant, root and leaf, and transporting within plant tissue is more stable to heat; chance is sour, alkali is unstable, dissolves in inorganic acid or organic acid and forms corresponding salt.Carbendazim affects cell division by disturbing the formation of spindle in pathogen mitosis, plays bactericidal action.Can prevent and treat cucurbits powdery mildew, epidemic disease, tomato early blight, beans anthracnose, epidemic disease, sclerotinia rot of colza, control vegetable sprout term damping off, damping off, long-term single use carbendazim easily makes germ develop immunity to drugs.Therefore, normal with other bactericide rotations uses or mix use.At present, the composite report about carbendazim and other bactericide is very many.For example, Chinese invention patent application 200510042119.6 discloses a kind of propiconazole and the composite bactericidal composition of carbendazim; Chinese invention patent application 200610147118.2 discloses a kind of Tebuconazole and the composite bactericidal composition of carbendazim.
Above, carry out the composite example of obtaining synergy although have in prior art about above-mentioned each bactericide and some bactericide, substantially all be confined to binary built, carry out composite report and have no about above-mentioned three kinds of bactericide.In addition, existing agriculture chemical compounding patent is mainly all only considered the composite synergistic effect that brings, yet, although synergistic effect is more obvious better, be not but to use unique factor of considering as agricultural chemicals, what also need especially to consider is, toxicity and the problem of environmental pollution of the composition after composite.For example, although some active component uses problem little separately, after composite use, bad chemical reaction may occur and cause problem of environmental pollution in the intermediate product that produces in their degradation process.Therefore, provide truly have synergistic effect and composite toxicity not to have to increase and bactericidal composition that problem of environmental pollution is less significant.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of new bactericidal composition, and it can expect to have better control efficiency, lower resistance, higher safety and lower use cost.
For solving above technical problem, the technical solution adopted in the present invention is as follows:
A kind of ternary built bactericidal composition, it is comprised of active component and pesticidal preparations auxiliary element, and particularly, active component is formed by weight 0.1~1:0.1~1:1 is composite by oxime bacterium ester, prothioconazoles and carbendazim.
Preferably, described active component is formed by weight 0.2~0.5:0.2~0.5:1 is composite by oxime bacterium ester, prothioconazoles and carbendazim.More preferably, particularly 0.33:0.33:1 is composite forms by weight 0.3~0.35:0.3~0.35:1 by oxime bacterium ester, prothioconazoles and carbendazim for active component.When three kinds of compositions are composite according to this ratio, not only reached the most significant synergistic effect, and minimum to the toxicity of people and animals and environment.
According to the present invention, bactericidal composition can be made acceptable formulation on any agricultural, and preferred green pesticide form is as water dispersible granules, suspending agent, effervescent tablet.
According to a concrete aspect of the present invention, the formulation of described ternary built bactericidal composition is water dispersible granules, in weight percentage, it is composed as follows: active component 5%~90%, dispersion moisture agent 1%~15%, disintegrant 2%~15%, binding agent 1%~15% and filler surplus.
When bactericidal composition was water dispersible granules, the weight content that active component preferably accounts for described bactericidal composition was 15%~80%.
In water dispersible granules, dispersion moisture agent preferably is comprised of by weight 1:1~10 lignosulfonates and dodecane sulfonate.
In water dispersible granules, disintegrant can be for being selected from one or several in alkyl phenol polyether, carboxymethyl cellulose, crospolyvinylpyrrolidone, crosslinked carboxymethyl fecula sodium, low-substituted hydroxypropyl cellulose, Ac-Di-Sol, ammonium sulfate, magnesium chloride, aluminium chloride, urea, anhydrous sodium sulfate, polyethyl acrylate and calcium chloride.
In water dispersible granules, the selection of binding agent and filler is not particularly limited, and can be commonly used those in this area.For example, binding agent can be starch, dextrin, gum Arabic, soybean protein, sodium silicate, gypsum, polyvinyl alcohol, polyvinyl acetate, ethene-vinyl acetate copolymer resins etc.Filler can be calcite, clay, kaolin, talcum, quicklime, diatomite, atlapulgite, mineral salt, diatomite, bentonite, white carbon, silica gel etc.
A preparation process of water dispersible granules is as follows: first with oxime bacterium ester, carbendazim, prothioconazoles, dispersion moisture agent, disintegrant, the filler premixed of formula ratio, mixed material mixes again, then pulverize through airslide disintegrating mill, material after pulverizing is changed in kneader, adding water and formula ratio binding agent mediates, extruder grain is drying to obtain.
According to another concrete aspect of the present invention, the formulation of ternary built bactericidal composition is suspending agent, in weight percentage, it is composed as follows: active component 5%~90%, wetting dispersing agent 1%~15%, thickener 0.5%~3%, antifreezing agent 0.1%~10%, stabilizing agent 0.01%~3%, defoamer 0.1%~1% and deionized water surplus.
In suspending agent, described wetting dispersing agent preferably is comprised of by weight 1:1~20 polycarboxylate and lignosulfonates.
In suspending agent, described thickener preferably is comprised of by weight 1:5~20 polyvinyl alcohol and Magnesiumaluminumsilicate.
In suspending agent, antifreezing agent can be for being selected from one or several in glycerine, isopropyl alcohol, ethylene glycol, propane diols, diethylene glycol (DEG), butyl glycol ether, propandiol butyl ether, butyl glycol ether, acetate, calcium chloride, sodium acetate and magnesium chloride.
A preparation process of suspending agent is as follows: oxime bacterium ester, carbendazim, prothioconazoles, wetting dispersing agent, thickener, antifreezing agent and the deionized water of formula ratio are mixed, adopt high-speed shearing machine to carry out just pulverizing, then change in the serialization sand mill and grind, make 95% above material particular diameter below 3 μ m, and get final product.
According to another concrete aspect of the present invention, when bactericidal composition is effervescent tablet, in weight percentage, it is composed as follows: active component 5%~90%, disintegrant 3%~15%, wetting dispersing agent 2~10%, binding agent 2%~10%, filler 5%~80%, wherein disintegrant comprises acid disintegrant and alkaline disintegrant, and wherein acid disintegrant is a kind of or its composition in citric acid or fumaric acid, and alkaline disintegrant is a kind of or its composition in sodium bicarbonate, sodium carbonate or ammonium sulfate; Binding agent is one or more in sodium carboxymethylcellulose, methylcellulose, CMC, hydroxypropyl methylcellulose, polyvinylpyrrolidone;
A preparation process of effervescent tablet is as follows: with formula ratio oxime bacterium ester, carbendazim, prothioconazoles, disintegrant, wetting dispersing agent, binding agent, filler premixed, coarse crushing, mix again, then change in cone-type mixer after airslide disintegrating mill is pulverized and mix, in tablet press machine, that gained dry powder direct pressing is in blocks again, and get final product.
Bactericidal composition of the present invention has good control efficiency to Common Diseases on fruit tree, vegetables and cereal crop, particularly corn downy mildew, black spot of fruit tree, cercospora leaf spot, soybean anthracnose disease is had special efficacy.The present invention also is particularly related to the application of above-mentioned ternary built bactericidal composition in the leaf spot of preventing and treating soybean, soybean anthracnose, corn downy mildew, black spot of fruit tree for this reason.
Owing to adopting above technical scheme, the present invention compared with prior art has following advantage:
The present invention's innovation is composite according to special ratios with oxime bacterium ester, prothioconazoles and carbendazim, obtained the synergistic function of highly significant, compare the further fungicidal spectrum that enlarged with their binary built, the diseases such as the downy mildew of fruit tree, vegetables and cereal crop, leaf spot, anthracnose, scab are had special efficacy.In addition, through experimental results demonstrate, composite do not have increase afterwards to mammalian toxicity.Applicant further discovery can further promote the composite effect of active component by specific wetting dispersing agent and dispersion moisture agent, allows to bring into play to the full extent synergistic effect.
Embodiment
Embodiment 1 50% oxime bacterium ester prothioconazoles carbendazim water dispersing granule
The composition of raw materials of water dispersible granules is referring to table 1, and wherein disintegrant is carboxymethyl cellulose, and binding agent is starch, and filler is diatomite.
The water dispersible granules preparation method is as follows:, pulverizes through airslide disintegrating mill with each material premixed except starch, mix again by formula, then changes over to and add water and starch kneading in kneader, and extruder grain, drying, and get final product.
The technical indicator of water dispersible granules is as follows: technical indicator is as follows: suspensibility 〉=88%; Disintegration time≤45s; Wetting time≤60s; Moisture≤2.5%; PH value 6.0~9.0; Dispersed 〉=88%; Screen analysis (by 75 μ m hole sizers) 〉=97%; Lasting foaming characteristic (after 1min)≤20ml; Particle size range (0.8mm~1.5mm) 〉=97%; 54 ± 2 ℃ of heat are store suspensibility 〉=84% after 30 days.
Embodiment 2 35% oxime bacterium ester prothioconazoles carbendazim water dispersing granules
The composition of raw materials of water dispersible granules is referring to table 1, and wherein disintegrant is carboxymethyl cellulose, and binding agent is starch, and filler is kaolin.
The water dispersible granules preparation method is with embodiment 1, and technical indicator is as follows: suspensibility 〉=90%; Disintegration time≤45s; Wetting time≤60s; Moisture≤2.5%; PH value 6.0~9.0; Dispersed 〉=88%; Screen analysis (by 75 μ m hole sizers) 〉=97%; Lasting foaming characteristic (after 1min)≤20ml; Particle size range (0.8mm~1.5mm) 〉=97%; 54 ± 2 ℃ of heat are store suspensibility 〉=85% after 30 days.
Embodiment 3 50% oxime bacterium ester prothioconazoles carbendazim water dispersing granules
The composition of raw materials of water dispersible granules is referring to table 1, and wherein disintegrant is alkyl phenol polyether, and binding agent is starch, and filler is diatomite.
The water dispersible granules preparation method is with embodiment 1, and technical indicator is as follows: suspensibility 〉=90%; Disintegration time≤45s; Wetting time≤60s; Moisture≤2.5%; PH value 6.0~9.0; Dispersed 〉=88%; Screen analysis (by 75 μ m hole sizers) 〉=97%; Lasting foaming characteristic (after 1min)≤20ml; Particle size range (0.8mm~1.5mm) 〉=97%; 54 ± 2 ℃ of heat are store suspensibility 〉=85% after 30 days.
Embodiment 4 40% oxime bacterium ester prothioconazoles carbendazim water dispersing granules
The composition of raw materials of water dispersible granules is referring to table 1, and wherein disintegrant is alkyl phenol polyether, and binding agent is polyvinyl acetate, and filler is attapulgite.
The water dispersible granules preparation method is with embodiment 1, and technical indicator is as follows: suspensibility 〉=92%; Disintegration time≤45s; Wetting time≤60s; Moisture≤2%; PH value 6.0~9.0; Dispersed 〉=88%; Screen analysis (by 75 μ m hole sizers) 〉=97%; Lasting foaming characteristic (after 1min)≤20ml; Particle size range (0.8mm~1.5mm) 〉=97%; 54 ± 2 ℃ of heat are store suspensibility 〉=88% after 30 days.
Embodiment 5 50% oxime bacterium ester prothioconazoles carbendazim water dispersing granules
The composition of raw materials of water dispersible granules is referring to table 1, and wherein disintegrant is alkyl phenol polyether, and binding agent is gum Arabic, and filler is silica gel.
The water dispersible granules preparation method is with embodiment 1, and technical indicator is as follows: suspensibility 〉=97.5%; Disintegration time≤45s; Wetting time≤60s; Moisture≤2%; PH value 6.0~9.0; Dispersed 〉=88%; Screen analysis (by 75 μ m hole sizers) 〉=97%; Lasting foaming characteristic (after 1min)≤20ml; Particle size range (0.8mm~1.5mm) 〉=97%; 54 ± 2 ℃ of heat are store suspensibility 〉=93% after 30 days.
Embodiment 6 40% oxime bacterium ester prothioconazoles carbendazim water dispersing granules
The composition of raw materials of water dispersible granules is referring to table 1, and wherein disintegrant is alkyl phenol polyether, and binding agent is starch, and filler is bentonite.
The water dispersible granules preparation method is with embodiment 1, and technical indicator is as follows: suspensibility 〉=96.5%; Disintegration time≤45s; Wetting time≤60s; Moisture≤2%; PH value 6.0~9.0; Dispersed 〉=88%; Screen analysis (by 75 μ m hole sizers) 〉=97%; Lasting foaming characteristic (after 1min)≤20ml; Particle size range (0.8mm~1.5mm) 〉=97%; 54 ± 2 ℃ of heat are store suspensibility 〉=92% after 30 days.
Embodiment 7 60% oxime bacterium ester prothioconazoles carbendazim water dispersing granules
The composition of raw materials of water dispersible granules is referring to table 1, and wherein disintegrant is alkyl phenol polyether, and binding agent is starch, and filler is diatomite.
The water dispersible granules preparation method is with embodiment 1, and technical indicator is as follows: suspensibility 〉=96.9%; Disintegration time≤45s; Wetting time≤60s; Moisture≤2%; PH value 6.0~9.0; Dispersed 〉=88%; Screen analysis (by 75 μ m hole sizers) 〉=97%; Lasting foaming characteristic (after 1min)≤20ml; Particle size range (0.8mm~1.5mm) 〉=97%; 54 ± 2 ℃ of heat are store suspensibility 〉=93% after 30 days.
The composition of raw materials of table 1 embodiment 1~7 oxime bacterium ester prothioconazoles carbendazim water dispersing granule
Figure BDA00002952243700041
Figure BDA00002952243700051
Embodiment 8 35% oxime bacterium ester prothioconazoles carbendazim suspending agents
The composition of raw materials of suspending agent is referring to table 2, and wherein antifreezing agent is ethylene glycol, and stabilizing agent is sodium alginate, and defoamer is dimethicone.
The preparation method of suspending agent is as follows: oxime bacterium ester, carbendazim, prothioconazoles, wetting dispersing agent, thickener, antifreezing agent and the deionized water of formula ratio are mixed, adopt high-speed shearing machine to carry out just pulverizing, then change in the serialization sand mill and grind, make 95% above material particular diameter below 3 μ m, and get final product.
The technical indicator of suspending agent is as follows: suspensibility 〉=90%; PH value 6.0~8.0; Screen analysis (by 75 μ m hole sizers) 〉=98%; Lasting foaming characteristic (after 1min)≤20ml; Pourability: topple over rear residue≤3.0%, residue after washing≤0.5%; 54 ± 2 ℃ of heat are store suspensibility 〉=85% after 14 days; 0 ± 2 ℃ of cold storage suspensibility 〉=85% after 7 days.
Embodiment 9 50% oxime bacterium ester prothioconazoles carbendazim suspending agents
The composition of raw materials of suspending agent is referring to table 2, and wherein antifreezing agent is ethylene glycol, and stabilizing agent is xanthans, and defoamer is dimethicone, deionized water polishing to 100%.
The preparation method of suspending agent is with embodiment 8, the key technical indexes: suspensibility 〉=94%; PH value 6.0~8.0; Screen analysis (by 75 μ m hole sizers) 〉=98%; Lasting foaming characteristic (after 1min)≤20ml; Pourability: topple over rear residue≤3.0%, residue after washing≤0.5%; 54 ± 2 ℃ of heat are store suspensibility 〉=90% after 14 days; 0 ± 2 ℃ of cold storage suspensibility 〉=90% after 7 days.
Embodiment 10 25% oxime bacterium ester prothioconazoles carbendazim suspending agents
The composition of raw materials of suspending agent is referring to table 2, and wherein antifreezing agent is glycerine, and stabilizing agent is guar gum, and defoamer is silicone defoaming agent, deionized water polishing to 100%.
The preparation method of suspending agent is with embodiment 8, the key technical indexes: suspensibility 〉=90%; PH value 6.0~8.0; Screen analysis (by 75 μ m hole sizers) 〉=98%; Lasting foaming characteristic (after 1min)≤20ml; Pourability: topple over rear residue≤3.0%, residue after washing≤0.5%; 54 ± 2 ℃ of heat are store suspensibility 〉=85% after 14 days; 0 ± 2 ℃ of cold storage suspensibility 〉=85% after 7 days.
Embodiment 11 45% oxime bacterium ester prothioconazoles carbendazim suspending agents
The composition of raw materials of suspending agent is referring to table 2, and wherein antifreezing agent is urea, and stabilizing agent is sodium carboxymethylcellulose, and defoamer is silicone defoaming agent, deionized water polishing to 100%.
The preparation method of suspending agent is with embodiment 8, the key technical indexes: suspensibility 〉=94%; PH value 6.0~8.0; Screen analysis (by 75 μ m hole sizers) 〉=98%; Lasting foaming characteristic (after 1min)≤20ml; Pourability: topple over rear residue≤3.0%, residue after washing≤0.5%; 54 ± 2 ℃ of heat are store suspensibility 〉=90% after 14 days; 0 ± 2 ℃ of cold storage suspensibility 〉=90% after 7 days.
Embodiment 12 45% oxime bacterium ester prothioconazoles carbendazim suspending agents
The composition of raw materials of suspending agent is referring to table 2, and wherein antifreezing agent is sodium chloride, and stabilizing agent is sodium carboxymethylcellulose, and defoamer is dimethicone, deionized water polishing to 100%.
The preparation method of suspending agent is with embodiment 8, the key technical indexes: suspensibility 〉=88%; PH value 6.0~8.0; Screen analysis (by 75 μ m hole sizers) 〉=98%; Lasting foaming characteristic (after 1min)≤20ml; Pourability: topple over rear residue≤3.0%, residue after washing≤0.5%; 54 ± 2 ℃ of heat are store suspensibility 〉=82% after 14 days; 0 ± 2 ℃ of cold storage suspensibility 〉=82% after 7 days.
Embodiment 13 45% oxime bacterium ester prothioconazoles carbendazim suspending agents
The composition of raw materials of suspending agent is referring to table 2, and wherein antifreezing agent is glycerine, and stabilizing agent is sodium alginate, and defoamer is silicone defoaming agent, deionized water polishing to 100%.
The preparation method of suspending agent is with embodiment 8, the key technical indexes: suspensibility 〉=96%; PH value 6.0~8.0; Screen analysis (by 75 μ m hole sizers) 〉=98%; Lasting foaming characteristic (after 1min)≤20ml; Pourability: topple over rear residue≤3.0%, residue after washing≤0.5%; 54 ± 2 ℃ of heat are store suspensibility 〉=92% after 14 days; 0 ± 2 ℃ of cold storage suspensibility 〉=92% after 7 days.
Embodiment 14 60% oxime bacterium ester prothioconazoles carbendazim suspending agents
The composition of raw materials of suspending agent is referring to table 2, and wherein antifreezing agent is glycerine, and stabilizing agent is sodium alginate, and defoamer is silicone defoaming agent, deionized water polishing to 100%.
The preparation method of suspending agent is with embodiment 8, the key technical indexes: suspensibility 〉=93%; PH value 6.0~8.0; Screen analysis (by 75 μ m hole sizers) 〉=98%; Lasting foaming characteristic (after 1min)≤20ml; Pourability: topple over rear residue≤3.0%, residue after washing≤0.5%; 54 ± 2 ℃ of heat are store suspensibility 〉=90% after 14 days; 0 ± 2 ℃ of cold storage suspensibility 〉=88% after 7 days.
The composition of raw materials of table 2 embodiment 8~14 oxime bacterium ester prothioconazoles carbendazim suspending agents
Figure BDA00002952243700061
Embodiment 15 60% oxime bacterium ester prothioconazoles carbendazim effervescent tablets
The composition of raw materials of effervescent tablet following (weight percentage): oxime bacterium ester 20%, carbendazim 20%, prothioconazoles 20%, sodium bicarbonate 2%, citric acid 3%, sodium lignin sulfonate 7%, glycerine 3%, ammonium sulfate 5%, sodium sorbate 0.5%, sodium carboxymethylcellulose 2%, deionized water 11%, kaolin polishing to 100%.
The effervescent tablet preparation method is as follows: with the material premixed, then coarse crushing, then mix changes in cone-type mixer after airslide disintegrating mill is pulverized and mixes, then in tablet press machine, that gained dry powder direct pressing is in blocks, and get final product by formula.
Embodiment 16 50% oxime bacterium ester prothioconazoles carbendazim effervescent tablets
The composition of raw materials of effervescent tablet following (weight percentage): oxime bacterium ester 10%, carbendazim 5%, prothioconazoles 35%, sodium carbonate 3%, citric acid 2.5%, sodium lignin sulfonate 7%, propane diols 2%, ammonium sulfate 10%, sodium sorbate 0.2%, sodium carboxymethylcellulose 1%, deionized water 10%, bentonite polishing to 100%.
The effervescent tablet preparation method is with embodiment 15.
Embodiment 17 50% oxime bacterium ester prothioconazoles carbendazim effervescent tablets
The composition of raw materials of effervescent tablet following (weight percentage): oxime bacterium ester 10%, carbendazim 5%, prothioconazoles 35%, sodium carbonate 3%, fumaric acid 2.5%, sodium lignin sulfonate 7%, propane diols 2%, sodium bicarbonate 2%, ammonium sulfate 10%, sodium sorbate 0.2%, sodium carboxymethylcellulose 1%, polyvinylpyrrolidone 1%, deionized water 10%, bentonite polishing to 100%.
The effervescent tablet preparation method is with embodiment 15.
The Toxicity Determination of ternary built bactericidal composition to corn downy mildew
1. indoor pot biologically active
The potted plant determination method of seedling is adopted in test, and trial crops is cultured to 3 true leaves in the greenhouse, carries out foliar spray by design flow and process on crops sprayer.After chemicals treatment, inoculation in 24 hours is for the spore suspension of examination pathogen, and postvaccinal test material is positioned in phytotron to be cultivated.Carry out the result investigation when the blank of not dispenser is fully fallen ill, disease scale also calculates preventive effect, does regression analysis according to each drug concentration numerical value and corresponding control probability value, calculates the EC of each medicament 50Value, disease scale standard, preventive effect computational methods, EC 50Value calculating method is with reference to the State Standard of the People's Republic of China.
Figure BDA00002952243700071
Figure BDA00002952243700072
Control efficiency is scaled probability value (y), and drug concentration (μ g/mL) is converted to logarithm value (x), calculates concentration EC in virulence equation and inhibition with method of least squares 50, then calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.
CTC≤80 expression composition performances are antagonism; When 80<CTC<120, the expression said composition shows as addition; When CTC 〉=120, the expression said composition shows as synergistic effect.
Actual measurement toxicity index (ATI)=(standard medicament EC 50/ reagent agent EC 50) * 100
The percentage composition of C in the percentage composition of B+C medicament toxicity index * mixture in the percentage composition of A+B medicament toxicity index * mixture in theoretical toxicity index (TTI)=A medicament toxicity index * mixture.
Co-toxicity coefficient (CTC)=[actual measurement toxicity index (ATI)/theoretical toxicity index (TTI)] * 100.
Result of the test is referring to table 3.Result shows, the composite bactericidal composition of oxime bacterium ester prothioconazoles carbendazim three components, and to having very excellent control efficiency for the examination target, the potted plant biologically active of three component mixtures is apparently higher than single dose and two component built agents thereof.
Table 3
Figure BDA00002952243700073
Figure BDA00002952243700081
The Toxicity Determination of ternary built bactericidal composition to cercospora leaf spot
The potted plant determination method of seedling is adopted in test, and trial crops is cultured to 3 true leaves in the greenhouse, carries out foliar spray by design flow and process on crops sprayer.After chemicals treatment, inoculation in 24 hours is for the spore suspension of examination pathogen, and postvaccinal test material is positioned in phytotron to be cultivated.Carry out the result investigation when the blank of not dispenser is fully fallen ill, disease scale also calculates preventive effect, does regression analysis according to each drug concentration numerical value and corresponding control probability value, calculates the EC of each medicament 50Value.
Result of the test is referring to table 4.Result shows, the composite bactericidal composition of oxime bacterium ester prothioconazoles carbendazim three components is to having very excellent control efficiency for the examination target.
Table 4
Figure BDA00002952243700082
The Toxicity Determination of complex composition to soybean anthracnose
Choose the consistent large bean seedlings (approximately 5 leaf phases) of growth, each processing selects 3 basins for the examination seedling.With test atomizer spray, the about 5ml of every basin.Inoculation in 24 hours after chemicals treatment, adopt the anthracnose spore suspension evenly to be seeded on plant, then Hot Pepper Seedling is put into hot-house culture, carry out state of an illness investigation according to the morbidity grade scale after 14 days, and calculating control efficiency, then calculate concentration EC50 in inhibition with method of least squares, then calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.Result is as shown in table 5.
Table 5
Figure BDA00002952243700091
Field control effectiveness test
The oxime bacterium ester prothioconazoles carbendazim composite germicide control field pear scab test of pesticide effectiveness
This experimental establishment is researched and developed by Jiangsu Qizhou Green Chemical Co., Ltd for reagent in suburb, Lianshui County, Jiangsu Province, and contrast medicament 36% oxime bacterium ester prothioconazoles SC, 36% carbendazim prothioconazoles SC are provided.
The investigation pear scab state of an illness before medication, in the dispenser for the first time of state of an illness initial stage, dispenser in every 10 days is once executed 2 times altogether.After dispenser 7 days for the second time, 14 days, investigated respectively the pear scab disease index and calculated preventive effect in 28 days.Experimental result is as shown in table 6.
Table 6
As can be seen from Table 6, can effectively prevent and treat pear scab after oxime bacterium ester prothioconazoles carbendazim is composite, control efficiency all is much better than contrast agents, in the scope of application, the target crop is had no adverse effects.
The oxime bacterium ester prothioconazoles carbendazim composite germicide control field apple tree scab test of pesticide effectiveness
This experimental establishment is researched and developed by Jiangsu Qizhou Green Chemical Co., Ltd for reagent in suburb, Lianshui County, Jiangsu Province, and contrast medicament 36% oxime bacterium ester prothioconazoles SC, 36% carbendazim prothioconazoles SC are provided.
The investigation apple tree scab state of an illness before medication, in the dispenser for the first time of state of an illness initial stage, dispenser in every 10 days is once executed 2 times altogether.After dispenser 7 days for the second time, 14 days, investigated respectively apple tree scab disease index and calculated preventive effect in 28 days.Experimental result is as shown in table 7.
Table 7 oxime bacterium ester prothioconazoles carbendazim and composite toxicity test interpretation of result to the apple tree scab thereof
Figure BDA00002952243700111
The present invention can produce higher synergistic function owing to adopting above-mentioned formula.Compare with single dose oxime bacterium ester or prothioconazoles or carbendazim control corps diseases, enlarged and prevented and treated the disease scope, delayed drug-fast generation.Obviously improve drug effect, reduced dosage and the spraying times of every mu of use, alleviated peasant burden, promote peasant's increasing both production and income, ensured better agriculture safety in production and protected ecotope.Be applied to agricultural plant chemoproection field, to fruit tree, vegetables, the leaf spot of the cereal crops such as soybean, corn, downy mildew, scab, the harm of anthracnose germ have excellence, protection and therapeutic action efficiently.
Toxicity test
Ternary recompounded composite has been carried out the acute toxicity detection.Result is referring to table 8.
Table 8 toxicity test result
Figure BDA00002952243700121
As can be seen from Table 8, in the scope of application, the target crop is had no adverse effects after oxime bacterium ester, prothioconazoles, carbendazim are composite, it is for toxicity and the single dose indifference of honeybee, toxicity indifference for Japanese quail, carp, setting due to test dose, belong to low toxicity, for the toxicity of rat, complex preparation toxicity rank all belongs to low toxicity or little poison.Toxicity test shows, the present invention is with oxime bacterium ester, prothioconazoles, the composite increase that does not cause toxicity of carbendazim.If consider medicament to multiple mammiferous toxicity, bactericidal composition of the present invention is all superior than single dose, Risk Reduction.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics; its purpose is to allow person skilled in the art scholar can understand content of the present invention and implement according to this; can not limit protection scope of the present invention with this; all equivalences that Spirit Essence is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.

Claims (10)

1. ternary built bactericidal composition, it is comprised of active component and pesticidal preparations auxiliary element, it is characterized in that: described active component is formed by weight 0.1 ~ 1:0.1 ~ 1:1 is composite by oxime bacterium ester, prothioconazoles and carbendazim.
2. ternary built bactericidal composition according to claim 1 is characterized in that: described active component is formed by weight 0.2 ~ 0.5:0.2 ~ 0.5:1 is composite by oxime bacterium ester, prothioconazoles and carbendazim.
3. ternary built bactericidal composition according to claim 2 is characterized in that: described active component is formed by weight 0.3 ~ 0.35:0.3 ~ 0.35:1 is composite by oxime bacterium ester, prothioconazoles and carbendazim.
4. the described ternary built bactericidal composition of any one claim according to claim 1 to 3, it is characterized in that: the formulation of described ternary built bactericidal composition is water dispersible granules, suspending agent or effervescent tablet.
5. ternary built bactericidal composition according to claim 4, it is characterized in that: the formulation of described ternary built bactericidal composition is water dispersible granules, in weight percentage, it is composed as follows: active component 5% ~ 90%, dispersion moisture agent 1% ~ 15%, disintegrant 2% ~ 15%, binding agent 1% ~ 15% and filler surplus.
6. ternary built bactericidal composition according to claim 5 is characterized in that: described dispersion moisture agent is comprised of by weight 1:1 ~ 10 lignosulfonates and dodecane sulfonate.
7. ternary built bactericidal composition according to claim 4, it is characterized in that: the formulation of described ternary built bactericidal composition is suspending agent, in weight percentage, it is composed as follows: active component 5% ~ 90%, wetting dispersing agent 1% ~ 15%, thickener 0.5% ~ 3%, antifreezing agent 0.1% ~ 10%, stabilizing agent 0.01% ~ 3%, defoamer 0.1% ~ 1% and deionized water surplus.
8. ternary built bactericidal composition according to claim 7 is characterized in that: described wetting dispersing agent is comprised of by weight 1:1 ~ 20 polycarboxylate and lignosulfonates.
9. ternary built bactericidal composition according to claim 7 is characterized in that: described thickener is comprised of by weight 1:5 ~ 20 polyvinyl alcohol and Magnesiumaluminumsilicate.
10. the application of the described composition pesticide of any one claim in the leaf spot of control soybean, soybean anthracnose, corn downy mildew, black spot of fruit tree according to claim 1-9.
CN2013100951731A 2013-03-22 2013-03-22 Ternary compound sterilizing composition containing trifloxystrobin and application of sterilizing composition Pending CN103168785A (en)

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CN105330656A (en) * 2015-11-02 2016-02-17 许自协 Compound for inhibiting growth of corn downy mildew
CN114532342A (en) * 2022-03-17 2022-05-27 溧阳中南化工有限公司 Prothioconazole and thiocyclam antibacterial composition and application thereof
CN115697060A (en) * 2020-04-24 2023-02-03 Upl有限责任公司 Fungicidal compositions

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CN102258043A (en) * 2011-08-18 2011-11-30 陕西美邦农药有限公司 Germicide composition containing protioconazole
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WO2010043552A1 (en) * 2008-10-16 2010-04-22 Basf Se Pesticidal mixtures comprising metaflumizone and an azole fungicide
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105330656A (en) * 2015-11-02 2016-02-17 许自协 Compound for inhibiting growth of corn downy mildew
CN115697060A (en) * 2020-04-24 2023-02-03 Upl有限责任公司 Fungicidal compositions
CN114532342A (en) * 2022-03-17 2022-05-27 溧阳中南化工有限公司 Prothioconazole and thiocyclam antibacterial composition and application thereof

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