CN101933514B - Bactericidal composite with triazole bactericide and chlorothalonil - Google Patents

Bactericidal composite with triazole bactericide and chlorothalonil Download PDF

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Publication number
CN101933514B
CN101933514B CN 201010271034 CN201010271034A CN101933514B CN 101933514 B CN101933514 B CN 101933514B CN 201010271034 CN201010271034 CN 201010271034 CN 201010271034 A CN201010271034 A CN 201010271034A CN 101933514 B CN101933514 B CN 101933514B
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tpn
epoxiconazole
composition
suspending agent
bactericide
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CN101933514A (en
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祁鸣
周炜
陶伟
胡荣
谷文喆
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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 bactericidal composite with triazole bactericide and chlorothalonil. The bactericidal composite mainly comprises the following raw materials by weight percent: 10%-30% of triazole bactericide, 10%-60% of chlorothalonil and 3%-15% of assistant, wherein the triazole bactericide is selected from one or more components of epoxiconazole, flutriafol, cyproconazole and penconazole; the assistant is formed by polycarboxylate dispersant and lignosulfonate wetting agent in a weight ratio of 1:0.15-3. When in use, good formulation stability can be maintained between the two active components of the bactericidal composite; and compared with the bactericide using a single component for controlling crop diseases, the range of the controlled diseases of the invention is expanded, the occurrence of resistance to drugs can be delayed, the drug effect is obviously increased, the drug dosage and frequency of administration per mu are reduced, the agricultural safety production is better ensured, and the ecological environment is protected.

Description

A kind of bactericidal composition that contains triazole bactericidal agent and tpn
Technical field
The invention belongs to pesticide field, particularly a kind of bactericidal composition.
Background technology
At present, according to the effect of medicament to disease, bactericide generally can be divided three classes:
1, protective fungicide: this series bactericidal agent can be protected not by the dispenser position of infection process, exempts from infecting of germ, need to just can receive effect by the spray medicine before crop does not touch disease or disease generation.Such as bordeaux mixture, lime sulfur, mancozeb, zineb etc.
2, the property rooted out bactericide: this class medicament can directly kill the invasion before germ and the treatment infected the dispenser position, seldom be directly used on the crop.Such as the infected seed of sterilizing with formalin, triadimefon has an eradicant action to stripe rust of wheat, powdery mildew using method are proper.
3, curative fungicide agent: this series bactericidal agent is also named interior absorption agent.After it is conducted by plant absorbing, can stop the germ development at each position of plant.Such as carbendazim, topsin, kasugarnycin etc.
Known, triazole bactericidal agent is a kind of broad spectrum activity systemic fungicide, is sterol demethylation inhibitor, destroys and stop the biosynthesis of the cell membrane important composition composition ergosterol of germ, causes cell membrane not form, and makes germ dead.Because absorption in having well, therefore can be promptly by plant absorbing, and in conducted inside, have good protection and therapeutic activity.Can prevent and treat the cereal crop powdery mildew, Helminthosporium, Puccinia, shell pin Pseudomonas pathogen also can be cooked seed treatment, prevents and treats soil-borne disease and seed-borne disease.The cereal powdery mildew there is special efficacy.
Tpn is a kind of wide spectrum, protective fungicide, its can with the fungal cell in glyceraldehyde 3-phosphate dehydro-genase in the combined with protein of cysteine, destroy the metabolism of cell and loss of life power.Main Function is the prevention fungal infection, does not have interior suction conduction, but at plant surface good adhesivity is arranged, and is not subject to rain drop erosion, and the long drug effect phase is arranged.But because it belongs to conventional sterilization agent kind, the long-term frequent use of large tracts of land has produced serious resistance.
Chinese invention patent application 200610011131.5 discloses a kind of composite bactericide, its active component is comprised of strobilurin fungicide, triazole bactericidal agent and tpn, wherein, strobilurin fungicide can be Enestroburin, Fluoxastrobin, kresoxim-methyl; Triazole bactericidal agent can be triazolone, Flusilazole, fluorine bacterium azoles, Difenoconazole, the ratio of strobilurin fungicide, triazole bactericidal agent and tpn is: 1~50: 1~50: 1~100, this composite bactericide shows synergistic effect in diseases such as preventing and treating cladosporium leaf and fruit mould of tomato, when active component was comprised of according to weight ratio 1: 1: 2~3 alkene oxime acid esters or kresoxim-methyl, triazolone and tpn, synergistic effect was particularly remarkable.Yet this bactericidal composition is formed by three kinds of composite reagents, the stability of composition is not fine, this has affected the performance of its composition drug effect to a certain extent, therefore, although three kinds of composite reagents show synergy than single medicament, yet its drug effect still remains to be improved, and cost also remains further to be reduced.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of stable bactericidal composition is provided, and its drug effect is good and cost is low.
For solving above technical problem, a kind of technical scheme of the present invention is: a kind of bactericidal composition, and by weight, its composition of raw materials is as follows: triazole bactericidal agent 10%~30%; Tpn 10%~60%; Auxiliary agent 3%~15% and deionized water 20%~70%, wherein, described triazole bactericidal agent is one or more the combination that is selected from epoxiconazole, Flutriafol, Cyproconazole and the penconazole, and described auxiliary agent is comprised of by weight 1: 0.15~3 polycarboxylate salt dispersant and lignosulfonates wetting agent; The preparation process of described bactericidal composition is as follows: at first each raw material with formula ratio mixes, pre-dispersed under high-speed stirred, then add the sand milling medium and carry out sand milling, make the particle diameter of 90% material below 3 μ m, stop sand milling, remove by filter the bactericidal composition that the sand milling medium namely gets suspending agent type.
According to the present invention, high-speed stirred refers to that mixing speed greater than 8000r/min, is generally 8000~10000r/min.
Preferably, in the above-mentioned bactericidal composition, the mass ratio of triazole bactericidal agent and tpn is 1: 1~3.In the described auxiliary agent, the mass ratio of polycarboxylate and lignosulfonates is preferably 1: 1~and 3.
Another technical scheme provided by the invention is: a kind of bactericidal composition, and by weight, its composition of raw materials is as follows: triazole bactericidal agent 10%~30%; Tpn 10%~60%; Auxiliary agent 3%~15%, ammonium sulfate 10%~40%; Sodium carboxymethylcellulose 0~2% and filler 0~70%, wherein triazole bactericidal agent is one or more the combination that is selected from epoxiconazole, Flutriafol, Cyproconazole and the penconazole, and auxiliary agent is comprised of by weight 1: 0.15~3 polycarboxylate salt dispersant and lignosulfonates wetting agent; The preparation process of this bactericidal composition is as follows: at first with each raw material premixed of formula ratio, mixed material is pulverized through coarse crushing, again mixing, airslide disintegrating mill successively, then entering into cone-type mixer is mixed to fineness of materials and reaches 99% by 325 mesh standard sieves, afterwards, in material, add the water kneading, extruder grain, the bactericidal composition of oven dry water-dispersible grain formulation.
Preferably, in the above-mentioned bactericidal composition, the mass ratio of triazole bactericidal agent and tpn is 1: 1~3.The mass ratio of polycarboxylate and lignosulfonates is preferably 1: 1~and 3.
According to a preferred version of the present invention: the composition of raw materials of described bactericidal composition is: epoxiconazole 10%~15%, tpn 15%~30%, polycarboxylate 2%~4%, lignosulfonates 4%~6%, ammonium sulfate 30%~40%, sodium carboxymethylcellulose 1~2% and filler 5%~15%.
Filler of the present invention can be for being selected from one or more the combination in kaolin, bentonite, diatomite, white carbon and the precipitated calcium carbonate.
Because adopt above technical scheme, the present invention compared with prior art has following advantage:
The active component of bactericidal composition of the present invention is comprised of specific triazole bactericidal agent and tpn, wherein, triazole bactericidal agent has extremely strong interior suction bactericidal action, the germ that produces resistance is had excellent control efficiency, but the single dose usage amount is high, fungicidal spectrum is narrow; The good tackness of tpn on plant surface, but produced higher resistance.The applicant is surprised to find that, when by means of specific auxiliary agent during with the two composite use, compound drug has embodied the synergistic effect (co-toxicity coefficient CTC surpasses 170) of highly significant, and during particularly with epoxiconazole and chlorothalonil compound, co-toxicity coefficient CTC reaches about 250.In addition, the combination medicament ratio that the present invention and existing alkene oxime acid esters or kresoxim-methyl, triazolone and chlorothalonil compound form, cost is lower, preparation is more simple, and drug effect is better.
Embodiment
The chemical name of the epoxiconazole that the present invention relates to is (2RS, 3SR)-1-[3-(2-chloro benzene)-2,3-epoxy-2-(4-fluorophenyl) propyl group]-1H-1,2,4-triazole.Former medicine is white crystal, be used for the seed treatment of Important Economic crop or the efficient germicide that face sprays, can good preventive and therapeutic effect be arranged to ten multiple diseases such as a series of cereal crop diseases such as damping off, powdery mildew, eyeprint diseases, the diseases such as the anthracnose on leaf spot, powdery mildew, rust and the grape on the crops such as banana, green onion garlic, celery, Kidney bean, melon, asparagus, peanut, beet, white rot are had good preventive effect.
The chemical name of the Flutriafol that the present invention relates to is α-(2-fluorophenyl)-α-(4-fluorophenyl)-1H-1,2,4-triazole-1-ethanol.Former medicine is clear crystal; be used for the seed treatment of Important Economic crop or the efficient germicide that face sprays; basidiomycetes and the microbial multiple diseases of ascus are had good protection and therapeutic action, can effectively prevent and treat wheat crops powdery mildew, rust, smut, smut of maize etc.
The chemical name of the Cyproconazole that the present invention relates to is: 2-(4-chlorphenyl)-3-cyclopropyl-1-(1H-1,2,4-triazol-1-yl) fourth-2-alcohol.Former medicine is clear crystal, is sterol demethylation inhibitor, is used for the seed treatment of Important Economic crop or the efficient germicide that face sprays, can effectively prevent and treat cereal and coffee rust, cereal, fruit tree and grape powdery mildew, peanut, beet tops pinta, apple scab and peanut white rot.Use with other bactericide, can fine cereal eye spot disease, leaf spot and the net blotch of preventing and treating.
The chemical name of the penconazole that the present invention relates to is: 1-[2-(2,4-dichlorophenyl)-4-propyl group-DOX-2-methyl]-1-hydrogen-1,2, the 4-triazole.Former medicine is white crystal; a kind of interior absorption triazole bactericidal agent that has protection, treatment and eradicant action concurrently can be absorbed by tissues such as root of the crop, stem, leaves, and upwards conduction; show that through toxicity mensuration and field control effectiveness test result fruit white rot of grape is had preferably control efficiency.
The tpn chemical name that the present invention relates to is: 2,4,5,6-tetrachloro-1,3-dicyanobenzenes.Sterling is white tasteless powder, its mechanism of action be can with the fungal cell in glyceraldehyde 3-phosphate dehydrogenase have an effect, combine with the protein that contains cysteine in this enzyme, thereby destroy this enzymic activity, fungal cell's metabolism is damaged and loses one's life power.Tpn does not have interior suction conduction, but after being sprayed onto on the plant corpus, can good tackness be arranged at body surface, be difficult for being fallen by rain drop erosion, so the drug effect phase is longer.Tpn can be used for the diseases such as the downy mildew, powdery mildew of control vegetables, fruit tree, but since its service time for a long time, the large tracts of land frequent application, it has produced higher resistance, affects its drug effect.
Invention thought of the present invention is by auxiliary agent triazole bactericidal agent is mutually composite with tpn, at utmost brings into play the synergistic effect of the two.Below in conjunction with specific embodiment technical scheme of the present invention is further described, but the present invention should not only limit to these embodiment.
Embodiment 1
A kind of suspending agent that contains Flutriafol and tpn, by weight, its composition of raw materials comprises Flutriafol 5%, tpn 15%, polycarboxylate 8%, lignosulfonates 4% and 68% deionized water.
The preparation method of above-mentioned suspending agent is as follows: by prescription each raw material is joined in the sand cylinder, after stirring, use again the high shear machine pre-dispersed, then change the sand mill sand milling over to, add sand milling medium zirconium oxide bead, the beginning sand milling, make the particle diameter of 90% material below 3 μ m, stop sand milling after 5 hours, filter, remove zirconium oxide bead, namely make the bactericidal composition suspending agent that contains Flutriafol and tpn.
Embodiment 2
A kind of suspending agent that contains Cyproconazole and tpn, its composition of raw materials comprise Cyproconazole 5%, tpn 15%, polycarboxylate 10%, lignosulfonates 5% and 65% deionized water, and the preparation process of this suspending agent is with embodiment 1.
Embodiment 3
A kind of suspending agent that contains epoxiconazole and tpn, its composition of raw materials comprise epoxiconazole 5%, tpn 15%, polycarboxylate 6%, lignosulfonates 8% and 66% deionized water, and the preparation process of this suspending agent is with embodiment 1.
Embodiment 4
A kind of suspending agent that contains penconazole and tpn, its composition of raw materials comprise penconazole 5%, tpn 15%, polycarboxylate 7%, lignosulfonates 7% and 66% deionized water, and the preparation process of this suspending agent is with embodiment 1.
Embodiment 5
A kind of water dispersible granules that contains epoxiconazole and tpn, by weight, its composition of raw materials comprises epoxiconazole 10%, tpn 30%, polycarboxylate 3%, lignosulfonates 5%, white carbon 10%, sodium carboxymethylcellulose 2%, ammonium sulfate 40%.
The preparation method of water dispersible granules is as follows: by filling a prescription each raw material premixed, through coarse crushing, after again mixing, airslide disintegrating mill are pulverized, join in the cone-type mixer, mixed fineness of materials reaches 99% by 325 mesh standard sieves, mediates through adding water, extruder grain is dried and be get final product.
Embodiment 6
A kind of water dispersible granules that contains penconazole and tpn, by weight, its composition of raw materials comprises penconazole 20%, tpn 60%, polycarboxylate 5%, lignosulfonates 5% and ammonium sulfate 10%.The preparation process of this water dispersible granules is with embodiment 5.
Embodiment 7
A kind of suspending agent that contains epoxiconazole, Cyproconazole and tpn, its composition of raw materials comprises epoxiconazole 5%, Cyproconazole 5%, tpn 10%, polycarboxylate 9%, lignosulfonates 4% and 67% deionized water, and the preparation process of this suspending agent is with embodiment 1.
Comparative Examples 1
A kind of suspending agent that contains epoxiconazole and tpn, its composition of raw materials comprise epoxiconazole 15%, tpn 5%, alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate 1%, alkylaryl polyoxyethylene ether 12% and deionized water 67%.The preparation process of this suspending agent is with embodiment 1.
Comparative Examples 2
A kind of water dispersible granules that contains Flutriafol and tpn, by weight, its composition of raw materials comprises Flutriafol 5%, tpn 30%, alkyl naphthalene formaldehyde condensate sulfonates 7%, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 9%, diatomite 40% and urea 9%.
The preparation process of this water dispersible granules is as follows: by filling a prescription each raw material premixed, through coarse crushing, after again mixing, airslide disintegrating mill are pulverized, join again material in the cone-type mixer, mixed fineness of materials reaches 99% by 325 mesh standard sieves, mediate through adding 0.05% polyvinyl alcohol water solution, extruder grain is dried and be get final product.
Performance test
With compound drug the toxicity of pepper anthracnose is measured, and to embodiment 1 to 7, Comparative Examples 1 and 2 and several bactericide of prior art carry out field control effectiveness test.
1, test method
Choose the consistent Hot Pepper Seedling (about 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 the chemicals treatment, adopt the anthracnose spore suspension evenly to be seeded on the 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 the inhibition with method of least squares, calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun again.
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 EC50/ reagent agent EC50) * 100
The percentage composition of B 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.
2, test result
See Table 1 and table 2.
The different bactericidal agents of table 1 are to the Toxicity Determination result of pepper anthracnose
Bactericide EC 50(μg/ml) ATI TTI Co-toxicity coefficient CTC
Tpn 11.08 100.0 --- ---
Flutriafol 8.37 132.4 --- ---
Epoxiconazole 5.38 205.9 --- ---
Cyproconazole 5.89 188.1 --- ---
Penconazole 7.64 145.3 --- ---
Tpn: Flutriafol=3: 1 (weight ratio) 5.75 192.7 108.1 178.3
Tpn: epoxiconazole=3: 1 (weight ratio) 3.47 319.3 126.5 252.4
Tpn: Cyproconazole=3: 1 (weight ratio) 4.65 238.3 122.0 195.3
Tpn: penconazole=3: 1 (weight ratio) 5.32 208.3 111.3 187.2
Can find out that from the test result of table 1 bactericidal composition according to triazole bactericidal agent of the present invention and tpn composition has good control efficiency to pepper anthracnose, CTC is obviously greater than 170, and synergistic effect is remarkable, can improve preventive effect in actual the use, reduce dosage, reduce and use farming originally.
The field control effectiveness test result of table 2 chemical control pepper anthracnose of the present invention
Reagent agent Mu consumption (g) Anthracnose is prevented and treated result (%)
20% tpn suspending agent 50 52.65%
20% Flutriafol suspending agent 50 59.36%
20% epoxiconazole suspension concentrate 50 70.62%
20% Cyproconazole suspending agent 50 66.44%
20% penconazole suspending agent 50 63.12%
Embodiment 1 50 73.71%
Embodiment 2 50 80.46%
Embodiment 3 50 85.19%
Embodiment 4 50 76.49%
Embodiment 5 25 89.87%
Embodiment 6 12.5 76.64%
Embodiment 7 50 87.65%
Comparative Examples 1 50 77.03%
Comparative Examples 2 50 72.98%
The clear water contrast / /
To sum up; bactericidal composition of the present invention; remain good composite stability between two kinds of active components in use, compare expanding prevention disease scope with single dose triazole bactericidal agent or tpn control corps diseases; delay 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, the harm of the germs such as fruit tree, vegetables, wheat, paddy rice is had excellence, efficiently protection and therapeutic action.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics; its purpose is to allow the personage who is familiar with technique can understand content of the present invention and according to this enforcement; 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, and all should be encompassed within protection scope of the present invention.

Claims (2)

1. suspending agent that contains epoxiconazole and tpn, it is characterized in that: its composition of raw materials comprises epoxiconazole 5%, tpn 15%, polycarboxylate 6%, lignosulfonates 8% and 66% deionized water, the preparation process of this suspending agent is as follows: by prescription each raw material is joined in the sand cylinder, after stirring, use again the high shear machine pre-dispersed, then change the sand mill sand milling over to, add sand milling medium zirconium oxide bead, the beginning sand milling, make the particle diameter of 90% material below 3 μ m, stop sand milling after 5 hours, filter, remove zirconium oxide bead, namely make the suspending agent that contains epoxiconazole and tpn.
2. water dispersible granules that contains epoxiconazole and tpn, it is characterized in that: by weight, its composition of raw materials comprises epoxiconazole 10%, tpn 30%, polycarboxylate 3%, lignosulfonates 5%, white carbon 10%, sodium carboxymethylcellulose 2%, ammonium sulfate 40%, the preparation method of water dispersible granules is as follows: by filling a prescription each raw material premixed, through coarse crushing, after again mixing, airslide disintegrating mill are pulverized, join in the cone-type mixer, mixed fineness of materials reaches 99% by 325 mesh standard sieves, mediate through adding water, extruder grain is dried and be get final product.
CN 201010271034 2010-09-03 2010-09-03 Bactericidal composite with triazole bactericide and chlorothalonil Active CN101933514B (en)

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CN102017951B (en) * 2010-11-21 2013-07-24 陕西美邦农药有限公司 Germicide composition containing cyproconazole and chlorothalonil
CN104705310A (en) * 2013-12-12 2015-06-17 南京华洲药业有限公司 Sterilization composition containing penconazole and cyproconazole, and applications thereof
CN104705312A (en) * 2013-12-12 2015-06-17 南京华洲药业有限公司 Sterilization composition containing penconazole and triadimenol, and applications thereof

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CN101743973A (en) * 2010-01-05 2010-06-23 陕西美邦农资贸易有限公司 Bactericidal composition containing penconazole and chlorothalonil
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