CN102007913B - Synergistic sterilizing composition containing Cyprodinil - Google Patents
Synergistic sterilizing composition containing Cyprodinil Download PDFInfo
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- CN102007913B CN102007913B CN 201010567373 CN201010567373A CN102007913B CN 102007913 B CN102007913 B CN 102007913B CN 201010567373 CN201010567373 CN 201010567373 CN 201010567373 A CN201010567373 A CN 201010567373A CN 102007913 B CN102007913 B CN 102007913B
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- cyprodinil
- fenoxanil
- isoprothiolane
- iprobenfos
- bactericidal composition
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Abstract
The invention relates to a synergistic sterilizing composition containing Cyprodinil. The effective active ingredients of the composition contain (A), namely Cyprodinil and (B), namely one of Fenoxanil, isoprothiolane and Kitazin P, wherein the weight ratio of A to B is 50:1 to 1:50; and auxiliaries and excipients are added into the effective active ingredients to prepare into water dispersible granules, suspending agents and the like, and the composition is mainly used for preventing and curing rice Magnaporthe grisea.
Description
Technical field
The invention belongs to technical field of pesticide, relate to a kind of bactericidal composition that contains cyprodinil and fenoxanil, Isoprothiolane, iprobenfos.
Technical background
Rice blast claims again rice blast, is that global important rice is sick, is listed in the large disease of paddy rice three in its same banded sclerotial blight of China, bacterial leaf-blight.Rice blast is a kind of epidemic disease of propagating by air-flow.Have the place of rice cropping that generation is arranged China is all, especially few with sunshine, mist reveals long mountain area of duration and weather relatively mild riverine and growth period duration of rice and is in the area in rainy season and occurs serious.This disease threatens greatly Rice Production, the popular time, and general underproduction 10%-20%, the heavy 40-50% that reaches, local field even has no harvest.It is caused harm generally, often causes heavy loss, and even No kernels or seeds are gathered, as in a year of scarcity.Cause some peasant household's grain ration shortage and rural society unstable.
Cyprodinil (cyprodinil), molecular formula: C
14H
15N
3, chemical name: 4-cyclopropyl-6-methyl-N-phenyl pyrimidine-2-amine.
Structural formula:
Cyprodinil belongs to the miazines bactericide.By suppressing the biosynthesis of methionine moral, suppress the secretion of hydrolase.Absorbed rapidly by blade in plant corpus, be penetrated into more than 30% in tissue, protected sediment is stored in blade; transmit in xylem, also transmit between blade, at high temperature metabolism is relatively rapid; sediment quite stable under low temperature in blade, the metabolite inanimate object is active.
Fenoxanil (fenoxanil) is the acid amide fungicides of BASF and Japanese agricultural chemicals company joint development, and molecular formula is C
15H
18Cl
2N
2O
2, chemical name: N-(1-itrile group-1,2-dimethyl propyl)-2-(2,4-dichlorophenoxy) propionamide, structural formula is:
Fenoxanil is inhaled and residual activity in having well, is melanin (melanin) biosynthesis inhibitor.Be mainly used in preventing and treating rice blast, to crop, mammal, Environmental security.
Isoprothiolane (isoprothiolane) molecular formula: C
12H
18O
4S
2, chemical name: diisopropyl-1,3-dithiolane-a-phenyl malonic ester.
Isoprothiolane is systemic fungicide, and rice blast is had special efficacy.Rice plant accumulates on leaf texture after absorbing medicament, concentrates on especially cob and branch stalk, invades thereby suppress germ, hinders the germ lipid-metabolism, suppresses pathogen growth, plays prevention and treatment.
Iprobenfos (iprobenfos), molecular formula are C
13H
21O
3PS, chemical name: O, O-diisopropyl-S-benzyl thiolophosphate.
Iprobenfos is the isopropyl kitazine, belongs to organophosphorus fungicide.Main interference cell membrane permeability stops some lipophilic chitin precursor by cytoplasma membrane, and chitinous biosynthesis block is hindered, and cell wall can not be grown, and suppresses the normal development of thalline.
No matter be cyprodinil, fenoxanil, Isoprothiolane, iprobenfos or other efficient germicides, long-term use separately, disease is developed immunity to drugs, cause the problem that dosage strengthens, preventive effect reduces, the lasting period shortens, be unfavorable for environment sustainable development.If a kind ofly do not have the novel pesticide of cross resistance to prevent and treat pathogen and want newly developed, need screen 10,000~1.5 ten thousand compounds, cost 1~1.5 hundred million dollar, the construction cycle is 6~10 years.And that the active ingredient of the different mechanisms of action is carried out is composite, is to delay the disease method commonly used that develops immunity to drugs, and according to the effect in production application, judge this composite be synergistic effect or antagonism.Complex role is significantly filled a prescription, and can obviously improve preventive effect, greatly reduces the dosage of agricultural chemicals, also can enlarge fungicidal spectrum, improves germicidal efficiency.
Cyprodinil and fenoxanil, Isoprothiolane, the iprobenfos mechanism of action are different, and mutually composite have good synergistic effect within the specific limits.And composite about cyprodinil and fenoxanil, Isoprothiolane, iprobenfos there is not yet relevant report at present at home and abroad.
Summary of the invention
The objective of the invention is to propose a kind of generation or delaying drug resistance speed that can prevent disease drug resistance, the bactericidal composition that use cost is low, preventive effect is good.
The inventor is by a large amount of indoor biometricses and field control effectiveness test, finds unexpectedly the use that is mixed within the specific limits of cyprodinil and fenoxanil, Isoprothiolane, iprobenfos, and rice blast is had good synergistic effect.And cyprodinil and fenoxanil, Isoprothiolane, the composite of iprobenfos at home and abroad there is not yet openly.
The present invention is achieved through the following technical solutions:
A kind of bactericidal composition that contains cyprodinil, wherein cyprodinil and fenoxanil, Isoprothiolane, iprobenfos weight ratio are 50: 1~1: 50.
The described bactericidal composition that contains cyprodinil, wherein the weight ratio of cyprodinil and fenoxanil, Isoprothiolane, iprobenfos is 20: 1~1: 20.。
The described bactericidal composition that contains cyprodinil, wherein the weight ratio of cyprodinil and fenoxanil, Isoprothiolane, iprobenfos is 10: 1~1: 10.
The described bactericidal composition that contains cyprodinil, wherein the weight ratio of cyprodinil and fenoxanil is 10: 1~1: 3.
The described bactericidal composition that contains cyprodinil, wherein the weight ratio of cyprodinil and Isoprothiolane is 5: 1~1: 5.
The described bactericidal composition that contains cyprodinil, wherein the weight ratio of cyprodinil and iprobenfos is 5: 1~1: 10.
The described bactericidal composition that contains the cyprodinil connection, wherein the effective active component content accounts for 1~90% of gross weight, is preferably 10~80%.
The described bactericidal composition that contains cyprodinil adds corresponding additive and filler according to method known in those skilled in the art, makes the upper any formulation that allows of agricultural, more preferably as: water dispersible granules, suspending agent, suspension emulsion, aqueous emulsion, microemulsion.
Following active components A is cyprodinil, and active component B is a kind of in pest acid amides, Isoprothiolane, iprobenfos.
When making water dispersible granules, composition comprises following constituent content: active components A 1~80%, active component B1~80%, dispersant 3~12%, wetting agent 1~8%, disintegrant 1~10%, binding agent 1~8%, filler 10~90%.
The former medicine of active components A, the former medicine of active component B, dispersant, wetting agent, disintegrant, filler etc. are obtained through air-flow crushing the particle diameter that needs together, then add other auxiliary agent such as binding agent, obtain the materials of granulating.With item quantitatively send in the fluidized bed granulation dryer through granulation and drying after, make water dispersible granules product of the present invention.
Comprise following constituent content when composition is made suspending agent: active components A 1~50%, active component B 1~50%, dispersant 2~10%, wetting agent 2~10%, defoamer 0.1~1%, thickener 0.1~2%, antifreeze 0.1~8%, deionized water add to 100%.
Dispersant, wetting agent, defoamer, thickener, antifreeze in above-mentioned formulation material are mixed through high speed shear, add the former medicine of active components A, the former medicine of active component B, ball milling is 2~3 hours in ball mill, make diameter of particle all below 5 μ m, make suspending agent product of the present invention.
Comprise following constituent content when composition is made suspension emulsion: active components A 1~50%, active component B 1~50%, emulsifier 2~12%, dispersant 2~10%, defoamer 0.1~2%, thickener 0.1~2%, antifreeze 0.1~8%, stabilizing agent 0.05~3%, water add to 100%.
Dispersant, defoamer, thickener, antifreeze, stabilizing agent in above-mentioned formulation material are mixed through high speed shear, add the former medicine of active components A, ball milling is 2~3 hours in ball mill, make diameter of particle all below 5 μ m, make the cyprodinil suspending agent, then with the former medicine of active component B, emulsifier and various auxiliary agent with the direct emulsification of high speed agitator in suspending agent, make suspension emulsion product of the present invention.
Comprise following constituent content when composition is made aqueous emulsion: active components A 1~50%, active component B 1~50%, solvent 1~30%, emulsifier 1~15%, co-emulsifier 0~8%, antifreeze 0~10%, thickener 0.1~2%, defoamer 0.01~2%, deionized water are supplied surplus.
Above-mentioned formulation material is mixed, effective active composition, solvent, emulsifier, co-emulsifier are added together, make to be dissolved into even oil phase; Water, antifreeze, thickener, defoamer are mixed, become the homogeneous water.Under high-speed stirred, water is added oil phase, make aqueous emulsion product of the present invention.
Comprise following constituent content when composition is made microemulsion: active components A 1~50%, active component B1~50%, solvent 1~30%, emulsifier 3~20%, co-emulsifier 0~12%, antifreeze 0~10%, thickener 0.1~2%, defoamer 0.01~2%, stabilizing agent 0~4%, deionized water is supplied surplus.
The former medicine of active components A and the former medicine of active component B are dissolved in the homogenizer that solvent and cosolvent are housed; Give strong the mixing and homogenize after emulsifier, stabilizing agent and antifreeze, water being joined in the homogenizer that mentioned solution is housed, obtain at last the as clear as crystal microemulsion product of the present invention of outward appearance.
Described auxiliary agent has dispersant, wetting agent, disintegrant, binding agent, emulsifier, co-emulsifier, defoamer, antifreeze, thickener, solvent.
described dispersant is selected from alkylnaphthalene sulfonate, two (alkyl) naphthalenesulfonate formaldehyde condensation compound, naphthalene sulfonic acid-formaldehyde condensation product, aryl phenol polyoxyethylene succinate sulfonate, octylphenol polyethylene oxyethylene group ether sulfate, polycarboxylate, lignosulfonates, the phonetic formaldehyde condensation products sulphate of alkylphenol-polyethenoxy, alkyl benzene sulfonate calcium salt, the naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol-polyethenoxy is phonetic, aliphatic amine polyoxyethylene is phonetic, polyoxyethylene carboxylate, one or more during the ester polyoxyethylene is phonetic.
Described wetting agent is selected from: one or more in lauryl sodium sulfate, neopelex, Nekal BX, wetting and penetrating agent F, spaonin powder, silkworm excrement, soapberry powder.
Described binding agent is selected from: one or more in diatomite, starch, PVA, carboxymethyl (ethyl) cellulose.
Described antifreeze is selected from: one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol.
Described defoamer is selected from: silicone, C
8~10Aliphatic alcohols, C
10~20One or more in saturated fat acids (as capric acid) and acid amides, silicone oil, silicone compound.
Described thickener is selected from: one or more in xanthan gum, polyvinyl alcohol, polyethylene glycol.
Described disintegrant is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, glucose.
Described emulsifier is selected from one or more in alkyl benzene sulfonate calcium salt, styrene polyoxyethylene ether ammonium sulfate salt, alkyl biphenyl ether disulfonic acid magnesium salts, triethanolamine salt, phenethyl phenol polyethenoxy ether, 506#, phenethyl phenol polyoxy ethyl polypropylene-base ether, alkylphenol-formaldehyde resin polyoxy ethyl ether, NP-10 phosphate, OP-10 phosphate, castor oil polyoxyethylene ether, sorbester p17, Tween 80;
Described co-emulsifier is one or more in butanols, isobutanol, dodecanol-1, tetradecanol-1, octadecanol-1;
Described solvent is selected from one or more in toluene, dimethylbenzene, methyl alcohol, ethanol, acetone, ether, cyclohexanone, vegetable oil, dimethyl formamide, acetonitrile, polyethylene glycol, pyrrolidones, solvent N-chain alkyl pyrrolidones;
Described stabilizing agent is selected from a kind of of organic acid, organic base, ester class, alcohols, antioxidant, surface-active substance.
Described filler is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate.
Composition of the present invention is mainly used in preventing and treating rice blast.
Beneficial effect of the present invention:
(1) present composition effective active composition cyprodinil and fenoxanil, Isoprothiolane, iprobenfos belong to the bactericide of two kinds of different mechanisms of action, and both mutually are mixed and can produce conflict;
(2) present composition shows good synergistic effect in given scope, and preventive effect is apparently higher than single dose, and dosage is little;
(3) the present invention not with an organic solvent, is difficult for producing poisoning, is convenient to transportation and storage;
(4) present composition has special efficacy to rice blast.
Embodiment
To further instruction of the present invention, but the present invention is not limited thereto below in conjunction with embodiment.Percentage in following examples all is weight percentage.
The embodiment of the present invention is the method that adopts Toxicity Determination and field trial to combine.
Implementation of an application example one: cyprodinil and fenoxanil, Isoprothiolane, iprobenfos are composite to the rice blast Toxicity Determination
After the effective inhibition concentration scope of each medicament was determined in prerun, each medicament was established respectively 5 dosage by active constituent content and is processed, and established the clear water contrast.Carry out with reference to " farm-chemical indoor determination test rule bactericide ", adopt the mycelial growth rate method to measure medicament to the virulence of rice blast.Measure colony diameter with the right-angled intersection method after 72h, calculate and respectively process net growth, mycelial growth inhibition rate.
Net growth (mm)=measurement colony diameter-5
Mycelial growth inhibition rate is converted into probit value (y), and liquor strength (μ g/mL) converts logarithm value (x) to, tries to achieve virulence regression equation (y=a+bx) with method of least squares, and calculates thus the EC of every kind of medicament
50Value.Calculate the different proportioning synergy ratios (SR) of two medicaments according to the Wadley method simultaneously, SR<0.5 is antagonism, and 0.5≤SR≤1.5 are summation action, and SR>1.5 are synergistic effect.Computing formula is as follows:
Wherein: a, b are respectively cyprodinil and fenoxanil, Isoprothiolane, iprobenfos shared ratio in combination
A is cyprodinil
B is fenoxanil, Isoprothiolane, iprobenfos
Toxicity test result one
Result of the test is as shown in the table:
Table 1 cyprodinil, fenoxanil and composite toxicity test analysis of results table to rice blast thereof
As shown in Table 1, cyprodinil, the fenoxanil EC to rice blast
50Be respectively 1.42mg/L and 0.16mg/L.The virulence of cyprodinil is lower than the virulence of fenoxanil.Cyprodinil and fenoxanil were mixed in scope at 50: 1~1: 20 and all show obvious synergistic effect.Wherein, both mixed synergies in 10: 1~1: 10 scope are comparatively desirable, and mixed synergies is particularly outstanding in 10: 1~1: 3 scope.
Toxicity test result two
Table 2 cyprodinil, Isoprothiolane and composite toxicity test analysis of results table to rice blast thereof
As shown in Table 2, cyprodinil, the Isoprothiolane EC to rice blast
50Be respectively 1.42mg/L and 0.97mg/L.Cyprodinil and Isoprothiolane were mixed in scope at 50: 1~1: 50 and all show obvious synergistic effect.Wherein, both mixed synergies in 10: 1~1: 10 scope are comparatively desirable, and mixed synergies is particularly outstanding in 5: 1~1: 5 scope.
Toxicity test result three
Table 3 cyprodinil, iprobenfos and composite toxicity test analysis of results table to rice blast thereof
As shown in Table 3, cyprodinil, the iprobenfos EC to rice blast
50Be respectively 1.46mg/L and 9.31mg/L.The virulence of cyprodinil is higher than the virulence of iprobenfos.Cyprodinil and Isoprothiolane were mixed in scope at 20: 1~1: 50 and all show obvious synergistic effect.Wherein, both mixed synergies in 10: 1~1: 10 scope are comparatively desirable, and mixed synergies is particularly outstanding in 5: 1~1: 10 scope.
Implementation of an application example two the implementation of Formulation Example
Embodiment 1 80% cyprodinil 'Daowenling ' water dispersible granule
Cyprodinil 60%, Isoprothiolane 20%, alkylphenol-polyethenoxy are phonetic 3%, lignosulfonates 3%, lauryl sodium sulfate 4%, starch 5%, kaolin add to 100%, mix making 80% cyprodinil 'Daowenling ' water dispersible granule.
Embodiment 2 70% cyprodinil fenoxanil water dispersible granules
Cyprodinil 60%, fenoxanil 10%, polycarboxylate 3%, polyoxyethylene carboxylate 3%, lauryl sodium sulfate 4%, sodium bicarbonate 3%, starch 7%, kaolin add to 100%, mix to make 70% cyprodinil fenoxanil water dispersible granules.
Embodiment 3 60% cyprodinil iprobenfos water dispersible granules
Cyprodinil 10%, iprobenfos 50%, alkylphenol-polyethenoxy are phonetic 5%, dodecyl benzene sulfonate 3%, starch 18%, bentonite add to 100%, mix making 60% cyprodinil iprobenfos water dispersible granules.
Embodiment 4 40% cyprodinil fenoxanil suspending agents
Cyprodinil 30%, fenoxanil 10%, alkyl benzene sulfonate calcium salt 5%, Sodium Polyacrylate 2%, DBSA 4%, silicone oil 0.1%, xanthan gum 0.3%, phenyl phenol polyoxy ethyl ether 2%, deionized water adds to 100%, mixes to make 40% cyprodinil fenoxanil suspending agent.
Embodiment 5 48% cyprodinil Isoprothiolane suspension emulsions
Cyprodinil 8%, Isoprothiolane 40%, alkylbenzenesulfonate 8%, polycarboxylate 4%, soapberry powder 5%, silicone compound 0.1%, hydroxyethylcellulose 0.1%, ethylene glycol 2%, alkyl benzene calcium sulfonate 2%, deionized water adds to 100%, mixes to make 48% cyprodinil Isoprothiolane suspension emulsion.
Embodiment 6 30% cyprodinil iprobenfos suspension emulsions
Cyprodinil 20%, iprobenfos 10%, castor oil polyoxyethylene ether 6%, polycarboxylate 2%, Nekal BX 2%, C
10-20Saturated fat acid compounds 0.1%, polyethylene glycol 0.5%, ethylene glycol 4%, phenethyl phenol polyoxy ethyl polypropylene-base ether 1%, deionized water adds to 100%, mixes to make 30% cyprodinil iprobenfos suspension emulsion.
Embodiment 7 40% cyprodinil fenoxanil aqueous emulsions
Cyprodinil 10%, fenoxanil 30%, ethyl acetate 20%, acetonitrile 5%, castor oil polyoxyethylene ether 5%, polyvinyl alcohol 1%, propane diols 5%, lauric acid 0.5%, deionized water adds to 100%, mixes to make 40% cyprodinil fenoxanil aqueous emulsion.
Embodiment 8 36% cyprodinil isoprothiolane emulsion in waters
Cyprodinil 6%, Isoprothiolane 30%, methyl alcohol 18%, acetone 8%, alkylphenol polyoxyethylene 5%, polyvinyl alcohol 1%, glycerine 5%, silicone oil 0.5%, deionized water adds to 100%, mixes to make 36% cyprodinil fenoxanil aqueous emulsion.
Embodiment 9 30% cyprodinil Iprobenfos aqueous emulsions
Cyprodinil 20%, iprobenfos 10%, methyl alcohol 15%, dimethyl sulfoxide (DMSO) 8%, fatty alcohol-polyoxyethylene ether 5%, xanthans 1%, glycerine 5%, aluminium-magnesium silicate 0.3%, deionized water adds to 100%, mixes to make 30% cyprodinil fenoxanil aqueous emulsion.
Embodiment 10 30% cyprodinil fenoxanil microemulsions
Cyprodinil 15%, fenoxanil 15%, acetonitrile 20%, alkylphenol-formaldehyde resin polyoxy ethyl ether 8%, butanols 5%, hydroxyethylcellulose 2%, sodium sorbate 2%, silicone defoaming agent 0.5%, deionized water adds to 100%, mixes to make 30% cyprodinil fenoxanil microemulsion.
Embodiment 11 25% cyprodinil iprobenfos microemulsions
Cyprodinil 10%, iprobenfos 15%, methyl alcohol 15%, phenethyl phenol polyethenoxy ether 8%, tetradecanol-1 5%, polyvinyl alcohol 2%, sodium sorbate 2%, silicone defoaming agent 0.5%, deionized water adds to 100%, mixes to make 25% cyprodinil iprobenfos microemulsion.
Embodiment 12 20% cyprodinil Isoprothiolane microemulsions
Cyprodinil 10%, Isoprothiolane 10%, ethyl acetate 12%, castor oil polyoxyethylene ether 8%, isobutanol 5%, hydroxyethylcellulose 2%, sodium sorbate 2%, silicone defoaming agent 0.5%, deionized water adds to 100%, mixes to make 20% cyprodinil Isoprothiolane microemulsion.
The ratio of active components A in above-mentioned the implementation of Formulation Example (cyprodinil) and B (in fenoxanil, Isoprothiolane, iprobenfos a kind of) can be adjusted in the synergy scope of 20: 1~1: 20, thereby forms new the implementation of Formulation Example.
Embodiment uses three bactericidal compositions that contain cyprodinil and prevents and treats the rice blast test of pesticide effectiveness
It is the village that this experimental establishment is practiced the township rabbit in Asia, Yongde County, Lincang city, test medicine is researched and developed, is provided by Shaanxi agricultural chemicals Co., Ltd of U.S. nation, contrast medicament 20% fenoxanil suspending agent (commercial), 40% Isoprothiolane wetting powder (commercial), 40% iprobenfos missible oil (commercial), 50% cyprodinil water dispersible granules (commercial).
The investigation rice blast state of an illness before medicine, in the dispenser for the first time of state of an illness initial stage, dispenser in every 7 days once is total to dispenser 3 times.Investigated respectively the rice blast disease index and calculated preventive effect in 7 days, 14 days, 30 days after the last dispenser.Experimental result is as follows:
Table 3 contains the bactericidal composition control rice blast test of pesticide effectiveness of cyprodinil
As can be seen from Table 3, can effectively prevent and treat rice blast after cyprodinil and fenoxanil, Isoprothiolane, iprobenfos are composite, control efficiency all is better than contrasting medicament, and the lasting period is long.In the test scope of medication, the target crop is had no adverse effects, and rice green smut is had good preventive effect, preventive effect reaches more than 90%.
Claims (7)
1. a Synergistic bactericidal composition that contains cyprodinil, is characterized in that bactericidal composition effective active composition is cyprodinil and fenoxanil, and the weight ratio of cyprodinil and fenoxanil is 50 ︰ 1 ~ 1 ︰ 20.
2. bactericidal composition according to claim 1, it is characterized in that: wherein the weight ratio of cyprodinil and fenoxanil is 20 ︰ 1 ~ 1 ︰ 20.
3. bactericidal composition according to claim 2, it is characterized in that: wherein the weight ratio of cyprodinil and fenoxanil is 10:1 ~ 1:3.
4. bactericidal composition according to claim 1, it is characterized in that: wherein the effective active component content accounts for 1~90% of gross weight.
5. bactericidal composition according to claim 4, it is characterized in that: wherein the effective active component content accounts for 10~80% of gross weight.
6. bactericidal composition according to claim 1, it is characterized in that: bactericidal composition is made water dispersible granules, suspending agent, suspension emulsion, aqueous emulsion or microemulsion.
7. bactericidal composition according to claim 1 is used for the application of control rice blast.
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