CN107897199A - A kind of composite bactericide composition of difenoconazole and pyraclostrobin - Google Patents
A kind of composite bactericide composition of difenoconazole and pyraclostrobin Download PDFInfo
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- CN107897199A CN107897199A CN201711476936.1A CN201711476936A CN107897199A CN 107897199 A CN107897199 A CN 107897199A CN 201711476936 A CN201711476936 A CN 201711476936A CN 107897199 A CN107897199 A CN 107897199A
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- difenoconazole
- pyraclostrobin
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- composite bactericide
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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Abstract
The invention discloses a kind of difenoconazole and the composite bactericide composition of pyraclostrobin, including following components in percentage by weight：Difenoconazole 1 85%；Pyraclostrobin 1 85%；Auxiliary material, surplus；Wherein, the auxiliary material is one kind or any combination in pH adjusting agent, dispersant, wetting agent, bleeding agent, disintegrant, antioxidant, binding agent, preservative, film forming agent, antifreeze, thickener, defoamer, filler and solvent.The composite bactericide composition realizes the effect for expanding fungicidal spectrum, extending the expiration date by the reasonable compounding of difenoconazole and pyraclostrobin；Actual bactericidal effect can be effectively improved at the same time, reduces the usage amount of fungicide, and the prevention effect to germ can be greatly improved, is the important means of pesticide integrated control.
Description
Technical field
The present invention relates to composition pesticide technical field, more particularly to the compounding of a kind of difenoconazole and pyraclostrobin
Microbicide compositions.
Background technology
The mechanism of action of difenoconazole (difenoconazole) is by suppressing the biosynthesis of the black alcohol of ergot and dry
The normal growth of germ is disturbed, the sporogenesis to phytopathogen has strong inhibitory action.Its structural formula is as follows：
Difenoconazole wide sterilization spectrum, it is to Ascomycetes, Basidiomycetes and mould including Alternaria, Ascochyta, tail spore
Partly know disease, powdery mildew including category, Colletotrichum, ball Cuo Pseudomonas, Phoma, Ramularia, Septoria, Venturia
Section, Uredinales and some Seedborne pathogens have lasting protection and therapeutic effect.To bitter rot or anthracnose of grape, white rot effect also very
It is good.Foliar treatment or seed treatment can improve the yield and guaranteed quality of crop.Absorbability as high-efficiency broad spectrum low-residual is killed
Microbial inoculum, compared with conventional sterilization agent, it is normal that difenoconazole compensate for carbendazim, thiophanate methyl, triazolone and Mancozeb etc.
The deficiencies of fungicide bactericidal range is narrow, preventive effect is poor is advised, long-time service and abuse due to conventional chemical fungicide, cause absolutely
Most of diseases produce resistance to it, cause its preventive effect to target disease to decline to a great extent, just effective when only heavy dose uses,
Cost accounting is increased, and pesticide residue is exceeded.And difenoconazole dosage is low, mu use cost is small, environmental pollution pressure
Power is also considerably reduced.
Pyraclostrobin (Pyraclostrobine) is a kind of mitochondrial respiratory function inhibitor.It is by preventing cell
Electron transmission between pigment b and c1 and suppress mitochondrial respiratory effect, prevent mitochondria from producing and providing cell eubolism institute
The energy needed, ultimately results in cell death.Its structure is：
Pyraclostrobin is widely used in prevention cereal, soybean, corn, peanut, cotton, grape, vegetables, potato, Xiang
On certain herbaceous plants with big flowers, banana, lemon, coffee, fruit tree, walnut, tea tree, tobacco, ornamental plant, lawn and other field crops by sac fungus,
Disease caused by the almost all kinds of fungal pathogens such as basidiomycetes, Fungi Imperfecti and oomycetes；It can be used for seed treatment.Pyrrole
Azoles kresoxim-methyl plays drug effect by suppressing spore germination and mycelial growth, have protect, treat, rooting out, permeating, it is strong in suction and
Resistance of rainwater washing against act on, can also produce as slow down aging, make blade it is greener, preferably tolerance biology and abiotic component stress
And effectively using physiological effects such as water and nitrogen.Pyraclostrobin can quickly be absorbed by crop, and mainly by leaf portion wax coat
It is detained, it can also be transmitted to blade back by leaf portion osmosis, so as to have prevention to the disease of blade tow sides
Effect.Pyraclostrobin in leaf portion Xiang Ding, to base transmission and fumigation action very little, but the conductive activity in plant is stronger.
But the one pack system pesticide of existing difenoconazole or pyraclostrobin, narrow there are fungicidal spectrum, dosage is high,
The defects of bactericidal effect is bad.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the present invention to provide a kind of difenoconazole and pyrazoles ether
The composite bactericide composition of bacterium ester, by the reasonable compounding of difenoconazole and pyraclostrobin come realize expand fungicidal spectrum,
The effect extended the expiration date；Actual bactericidal effect can be effectively improved at the same time, reduces the usage amount of fungicide, and can be significantly
The prevention effect to germ is improved, is the important means of pesticide integrated control.
An object of the present invention adopts the following technical scheme that realization：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：
Difenoconazole 1-85%；Pyraclostrobin 1-85%；Auxiliary material, surplus；
Wherein, the auxiliary material for pH adjusting agent, dispersant, wetting agent, bleeding agent, disintegrant, antioxidant, binding agent,
One kind or any combination in preservative, film forming agent, antifreeze, thickener, defoamer, filler and solvent.
Further, the weight ratio of pyraclostrobin and difenoconazole is 1：(0.3-3).
Further, including in percentage by weight following components：Difenoconazole 5-50%；Pyraclostrobin 3-
50%；Auxiliary material, surplus.
Further, in the auxiliary material, the dosage difference of each component is as follows in percentage by weight：PH adjusting agent 0-
10%, dispersant 0-10%, wetting agent 0-5%, bleeding agent 0-5%, disintegrant 0-10%, antioxidant 0-2%, binding agent 0-
10%, preservative 0-2%, film forming agent 0-10%, antifreeze 0-10%, thickener 0-5%, defoamer 0-2%, filler 0-
80%, solvent 0-80%.
Further, the pH adjusting agent is dihydric phosphate；The dispersant is lignosulfonates, acrylic acid copolymer
One kind or any combination in thing salt, polycarboxylate, naphthalenesulfonate formaldehyde condensation compound, alkyl benzene sulfonic acid ester；The wetting agent is
Dodecylphosphoric acid salt, dodecyl benzene sulfonate, fatty alcohol polyoxyethylene ether, sulfocarbolate formaldehyde condensation products, polysulfonate
With one kind or any combination in polyoxyethylene alkyl ether sulfate salt.
Further, the bleeding agent be sulfated castor oil, sodium alkyl sulfonate and sodium alkyl benzene sulfonate in one kind or
Any combination；The disintegrant is one kind or any combination that urea, sodium carbonate, sodium acid carbonate and cyclohexanone are condensed in sodium salt；
The antioxidant is in tert-butylhydroquinone, 2,6 di tert butyl 4 methyl phenol and butylated hydroxyarisol
A kind of or any combination.
Further, the binding agent is one kind in starch, sodium carboxymethylcellulose and gum arabic or any group
Close；The preservative is one kind or any combination in benzoic acid, dimethyl fumarate and benzoisothiazolinone；The film forming
Agent is one kind or any combination in polyvinyl alcohol, polyethylene glycol and gelatin.
Further, the filler for organobentonite, white carbon, glucose, starch, diatomite, clay, kaolin,
One kind or any combination in sodium chloride, potassium chloride, sodium sulphate and lactose；The solvent is water, ethanol, acetone, toluene, diformazan
Benzene, toluene, chlorobenzene, methanol, dimethylformamide, pyrrolidones, cyclohexanone, dimethyl carbonate, butanol, amylalcohol, lipid, diformazan
One kind or any combination in base sulfoxide, petroleum distillate, turpentine oil, mineral oil, methyl oleate and soybean oil.
Further, the antifreeze is one kind in ethylene glycol, propane diols, glycerine, urea, sodium chloride and ammonium chloride
Or any combination；The thickener for xanthans, hydroxymethyl cellulose, hydroxyethyl cellulose, positive cellulose, polyvinyl alcohol and
One kind or any combination in aluminium-magnesium silicate；The defoamer is silicone oil, organosilicon ketone compound, C10-20 saturated fatty acids
One kind or any combination in class compound and C8-10 aliphatic alcohols compounds.
Further, the composite bactericide composition is pulvis, water dispersible granules, aqueous dispersion tablets, missible oil, water and milk
One kind in agent, suspending agent, suspension emulsion, soluble concentrate, microemulsion, dispersible oil-suspending agent and suspension seed-coating agent.
Compared with prior art, the beneficial effects of the present invention are：
The composite bactericide composition of difenoconazole and pyraclostrobin provided by the present invention, passes through difenoconazole
With the reasonable effect compounded to realize expansion fungicidal spectrum, extend the expiration date of pyraclostrobin；It can effectively improve reality at the same time
The bactericidal effect on border, reduces the usage amount of fungicide, and can greatly improve the prevention effect to germ, is pesticide integrated control
Important means.
Embodiment
In the following, with reference to embodiment, the present invention is described further, it is necessary to which explanation is, what is do not collided
Under the premise of, new embodiment can be formed between various embodiments described below or between each technical characteristic in any combination.
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：
Difenoconazole 1-85%；Pyraclostrobin 1-85%；Auxiliary material, surplus；
Wherein, auxiliary material is pH adjusting agent, dispersant, wetting agent, bleeding agent, disintegrant, antioxidant, binding agent, anti-corrosion
One kind or any combination in agent, film forming agent, antifreeze, thickener, defoamer, filler and solvent.
As the mode that further carries out, the weight ratio of pyraclostrobin and difenoconazole is 1：(0.3-3)；It is more excellent
The weight ratio of selection of land, pyraclostrobin and difenoconazole is 3: 1；2∶1；1∶1；1: 2 or 1: 3；Most preferably, pyraclostrobin
Weight ratio with difenoconazole is 1: 1.
As the mode that further carries out, including following components in percentage by weight：Difenoconazole 5-50%；
Pyraclostrobin 3-50%；Auxiliary material, surplus.
As mode is further carried out, in auxiliary material, the dosage difference of each component is as follows in percentage by weight：pH
Conditioning agent 0-10%, dispersant 0-10%, wetting agent 0-5%, bleeding agent 0-5%, disintegrant 0-10%, antioxidant 0-2%,
Binding agent 0-10%, preservative 0-2%, film forming agent 0-10%, antifreeze 0-10%, thickener 0-5%, defoamer 0-2%, is filled out
Expect 0-80%, solvent 0-80%.
As the mode that further carries out, pH adjusting agent is dihydric phosphate, is more preferably preferably using di(2-ethylhexyl)phosphate
Hydrogen potassium, sodium dihydrogen phosphate.
As the mode that further carries out, dispersant is lignosulfonates, acrylic copolymer salt, polycarboxylate, naphthalene
One kind or any combination in sulfonate and formaldehyde condensation product, alkyl benzene sulfonic acid ester.
As the mode that further carries out, wetting agent is dodecylphosphoric acid salt, dodecyl benzene sulfonate, poly alkyl alcohol
Ethylene oxide ether, sulfocarbolate formaldehyde condensation products, polysulfonate and one kind or any combination in polyoxyethylene alkyl ether sulfate salt.
As the mode that further carries out, bleeding agent is in sulfated castor oil, sodium alkyl sulfonate and sodium alkyl benzene sulfonate
One kind or any combination.
As the mode that further carries out, disintegrant is urea, sodium carbonate, sodium acid carbonate and cyclohexanone are condensed in sodium salt
A kind of or any combination.
As the mode that further carries out, antioxidant is tert-butylhydroquinone, 2,6- di-tert-butyl-4-methy phenols
With one kind or any combination in butylated hydroxyarisol.
As the mode that further carries out, binding agent is one kind in starch, sodium carboxymethylcellulose and gum arabic
Or any combination.
As the mode that further carries out, preservative is in benzoic acid, dimethyl fumarate and benzoisothiazolinone
A kind of or any combination.
As the mode that further carries out, film forming agent is polyvinyl alcohol, polyethylene glycol, gelatin and macromolecular organic compound
In one kind or any combination.
As the mode that further carries out, filler is organobentonite, white carbon, glucose, starch, diatomite, clay,
One kind or any combination in kaolin, sodium chloride, potassium chloride, sodium sulphate and lactose.
As the mode that further carries out, solvent is water, ethanol, acetone, toluene, dimethylbenzene, toluene, chlorobenzene, methanol, two
Methylformamide, pyrrolidones, cyclohexanone, dimethyl carbonate, butanol, amylalcohol, lipid, dimethyl sulfoxide (DMSO), petroleum distillate, pine
One kind or any combination in fatty oil, mineral oil, methyl oleate and soybean oil.
As the mode that further carries out, antifreeze is ethylene glycol, propane diols, glycerine, urea, sodium chloride and ammonium chloride
In one kind or any combination.
As the mode that further carries out, thickener is xanthans, hydroxymethyl cellulose, hydroxyethyl cellulose, actively fibre
Dimension element, polyvinyl alcohol and one kind or any combination in aluminium-magnesium silicate.
As the mode that further carries out, defoamer is silicone oil, organosilicon ketone compound, C10-20 saturated fat acids
One kind or any combination in compound and C8-10 aliphatic alcohols compounds.
As the mode that further carries out, composite bactericide composition is pulvis, wettable powder, water dispersible granules, water
Disket, missible oil, aqueous emulsion, suspending agent, suspension emulsion, soluble concentrate, microemulsion, dispersible oil-suspending agent and suspension seed-coating agent
In one kind.
The difenoconazole and the composite bactericide composition of pyraclostrobin that the embodiment of the present invention is provided, pyrazoles ether bacterium
Ester is new-type wide-spectrum bactericide, and the mechanism of action is mitochondrial respiratory inhibitor, has protection, treatment, blade infiltration conduction；
Difenoconazole is triazole type absorbability sterol demethylation inhibitor fungicide, to fungi especially Basidiomycota and Ascomycota
Caused disease has the protection and therapeutic effect of broad spectrum activity.Pyraclostrobin not only has preferable increase with difenoconazole mixture
Effect act on, can suitably reduce dosage, delay and administers the resistance to the action of a drug of pathogen, but also can make mixture with protect,
Treatment and conduction, realize the purpose learnt from other's strong points to offset one's weaknesses, had complementary advantages, and expand prevention spectrum and use scope.Based on this, pyrazoles
Kresoxim-methyl will have preferable economic benefit and social benefit with the exploitation of difenoconazole mixture, have popularization should in agricultural production
With value.
It is specific embodiment of the present invention below, used raw material, equipment etc. remove special limit in the following embodiments
It can be obtained outside fixed by buying pattern.
Embodiment 1：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 10%；Pyraclostrobin 20%；Alkyl benzene sulfonic acid ester 5%；Polysulfonate 5%；Glucose 6.7%；
Butylated hydroxyarisol 0.1%；Kaolin, supplies 100%.
Above-mentioned composite bactericide composition is prepared into wettable powder, and specific preparation process is as follows：Above-mentioned material is thrown
Enter in mixer, through air-flow crushing after mixing, you can obtain difenoconazole pyraclostrobin wettable powder.After testing,
Preparation stability is qualified.
Embodiment 2：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 10%；Pyraclostrobin 10%；Polycarboxylate 5%；Sulfocarbolate formaldehyde condensation products 3%；Polyoxy second
Allylic alkylation ether sulfate 3%；Cyclohexanone is condensed sodium salt 3%；Diatomite, supplies 100%.
Above-mentioned composite bactericide composition is prepared into water dispersible granules, and specific preparation process is as follows：Above-mentioned material is thrown
Enter in mixer and mix, then add water to be granulated after air-flow crushing, difenoconazole pyraclostrobin water is can obtain after drying
Dispersible granule.After testing, preparation stability is qualified.
Embodiment 3：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 20%；Pyraclostrobin 20%；Alkyl benzene calcium sulfonate 5%；Fatty alcohol polyoxyethylene ether 4%；Hexamethylene
Ketone 15%；Sulfated castor oil amount 5%；150# solvent naphthas, supply 100%.
Above-mentioned composite bactericide composition is prepared into missible oil, and specific preparation process is as follows：By difenoconazole and pyrazoles
Kresoxim-methyl input has been added in the reaction kettle of cyclohexanone, solvent naphtha, other auxiliary materials are added after stirring and dissolving, are stirred evenly, you can
Obtain difenoconazole pyraclostrobin missible oil.After testing, preparation stability is qualified.
Embodiment 4：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 8%；Pyraclostrobin 12%；Alkyl benzene sulfonic acid ester 4%；Fatty alcohol polyoxyethylene ether 3%；Hexamethylene
Ketone is condensed sodium salt 2%；Silicone compound 0.1%；Dimethyl carbonate 20%；Water, supplies 100%.
Above-mentioned composite bactericide composition is prepared into aqueous emulsion, and specific preparation process is as follows：By difenoconazole, pyrazoles
Kresoxim-methyl is first put into dimethyl carbonate, rear other auxiliary materials added in addition to water after dissolving, by organic phase under high speed shear
It is added in water phase, difenoconazole pyraclostrobin aqueous emulsion is can obtain after clipping to suitable particle diameter.After testing, make
Agent qualified stability.
Embodiment 5：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 15%；Pyraclostrobin 15%；Alkyl benzene sulfonic acid ester 5%；Acrylic copolymer salt 5%；Cyclohexanone
It is condensed sodium salt 3%；Sodium chloride 3%；Dimethyl fumarate 0.1%；Xanthans 0.2%；Aliphatic alcohols compound 0.1%；Water, is mended
Foot 100%.
Above-mentioned composite bactericide composition is prepared into suspending agent, and specific preparation process is as follows：Above-mentioned material is put into
Have in the water of auxiliary agent, be sanded after shearing and arrive suitable particle diameter, you can obtain difenoconazole pyraclostrobin suspending agent.Through inspection
Survey, preparation stability is qualified.
Embodiment 6：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 15%；Pyraclostrobin 15%；APES formaldehyde condensation product 8%；Butanedioic acid two is pungent
Ester sodium sulfonate 8%；Alkylphenol polyoxyethylene ether 5%；Ethanol 2%；White carbon 0.2%；Organobentonite 0.1%；Methyl oleate,
Supply 100%.
Above-mentioned composite bactericide composition is prepared into dispersible oil-suspending agent, and specific preparation process is as follows：By phenylate first
Ring azoles and pyraclostrobin are put into the methyl oleate for being mixed with remaining auxiliary material, are sanded after shearing and are arrived suitable particle diameter, i.e.,
It can obtain the dispersible oil-suspending agent of difenoconazole pyraclostrobin.After testing, preparation stability is qualified.
Embodiment 7：
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 5%；Pyraclostrobin 5%；Alkyl benzene sulfonic acid ester 5%；Acrylic copolymer salt 5%；Cyclohexanone contracts
Close sodium salt 3%；Polyvinyl alcohol 3%；Glycerine 7%；Xanthans 0.2%；Benzoisothiazolinone 0.1%；Organosilicon ketone
Compound 0.1%；Water, supplies 100%.
Above-mentioned composite bactericide composition be prepared into can suspension seed-coating agent, specific preparation process is as follows：By phenyl ether methyl cyclic
Azoles and pyraclostrobin are put into the water of other auxiliary materials, are sanded after shearing and are arrived suitable particle diameter, you can obtain phenyl ether methyl cyclic
Azoles pyraclostrobin suspension seed-coating agent.After testing, preparation stability is qualified.
Embodiment 8
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 30%；Pyraclostrobin 10%；Polycarboxylate 2%；Lignosulfonates 3%；, detergent alkylate
Sulfonate 3%；Sodium carboxymethylcellulose 0.5%；Starch 1%；Sodium carbonate, supplies 100%.
Above-mentioned composite bactericide composition is prepared into aqueous dispersion tablets, and specific preparation process is as follows：Above-mentioned material is thrown
Enter in mixer and mix, then add hydraulic pressure piece after air-flow crushing, difenoconazole pyraclostrobin water is can obtain after drying
Disket.After testing, preparation stability is qualified.
Embodiment 9
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 10%；Pyraclostrobin 5%；Alkyl benzene sulfonic acid ester 4%；Fatty alcohol polyoxyethylene ether 3%；Hexamethylene
Ketone is condensed sodium salt 2%；Acrylic copolymer salt 5%；Dimethyl carbonate 20%；Glycerine 7%；Xanthans 0.2%；Benzisothia
Oxazoline ketone 0.1%；Organosilicon ketone compound 0.1%；Water, supplies 100%.
Above-mentioned composite bactericide composition is prepared into suspension emulsion, and specific preparation process is as follows：By above-mentioned difenoconazole
Put into the solvent of dimethyl carbonate, other auxiliary materials such as dispersant, wetting agent are added after dissolving, will under high speed shear
The mixed liquor that rises is added in water phase, adds pyraclostrobin after clipping to suitable particle diameter, sand milling arrives suitable particle diameter, you can
To difenoconazole pyraclostrobin suspension emulsion.After testing, preparation stability is qualified.
Embodiment 10
A kind of composite bactericide composition of difenoconazole and pyraclostrobin, including in percentage by weight with
Lower component：Difenoconazole 10%；Pyraclostrobin 30%；Alkyl benzene calcium sulfonate 5%；Naphthalenesulfonate formaldehyde condensation compound 4%；Fat
Fat alcohol polyoxyethylene ether 4%；Pyrrolidones 15%；Pyrrolidones 10%；Ethanol, supplies 100%.
Above-mentioned composite bactericide composition is prepared into soluble concentrate, and specific preparation process is as follows：By difenoconazole and
Pyraclostrobin input has been added in the reaction kettle of pyrrolidones, pyrrolidones and ethanol, other auxiliary materials are added after stirring and dissolving,
Stir evenly, you can obtain difenoconazole pyraclostrobin soluble concentrate.After testing, preparation stability is qualified.
Effect assessment and performance detection
First, to the toxicity test of citrus anthracnose bacterium
1st, test objective
The mixture that pyraclostrobin is determined indoors with difenoconazole and its different proportion is combined to citrus anthracnose
The virulence of bacterium, and carry out synegism evaluation, specifies the suitability of the two, for grinding for pyraclostrobin and difenoconazole mixture
Study carefully and provide scientific basis with exploitation.
2nd, experimental condition
2.1 for examination target
Citrus anthracnose bacterium (Colletotrichum gloeosporioides), by Hunan Chemical Research Institute's pesticide biology
Research center is measured to preserve and provide.
2.2 condition of culture
Condition of culture for target after examination target and experiment is 25 ± 5 DEG C of temperature, relative humidity 65 ± 5%.
2.3 instrument and equipment
Beaker, pipette, graduated cylinder, culture dish, high-pressure sterilizing pot, biochemical cultivation case etc..
3rd, experimental design
3.1 test medicine
96% active compound of pyraclostrobin (pyraclostrobin)；Difenoconazole (difenoconazole) 95% is former
Medicine, above medicament are provided by Shanghai Yuelian Biotechnology Co., Ltd..
3.2 drug concentrations and proportion design and solution are prepared
Pyraclostrobin solution：96% active compound of 0.0200g pyraclostrobins is weighed, is dissolved with 0.2mL DMF, addition contains
The sterile water 95.8mL of 0.1%Tween80 emulsifying agents, stirs evenly, and is configured to 200mg/L mother liquors, then be diluted to sterile water
100th, 50,25,12.5,6.25mg/L concentration is spare；
Difenoconazole solution：0.0100g95% difenoconazole technical materials are weighed, are dissolved with 0.2mL DMF, addition contains
The sterile water 94.8mL of 0.1%Tween80 emulsifying agents is configured to 100mg/L mother liquors, then with the emulsifying agent containing 0.1%Tween80
Sterile water is diluted to 50,10,5,1,0.5mg/L concentration it is spare；
Each mixture solution：Take 18 respectively, 20,10,10,6mL 100mg/L pyraclostrobin solution be added separately to 6,10,
10th, 20 100mg/L pyraclostrobins difenoconazole 3: 1, is made in 18mL100mg/L difenoconazole solution；2∶1；1∶
1；1: 2 and 1: 3 solution, then with the sterile water of the emulsifying agent containing 0.1%Tween80 be diluted to 50,10,5,1,0.5mg/L concentration it is standby
With；
Contrast solution：0.2mL DMF add the sterile water of 95mL emulsifying agents containing 0.1%Tween80.
4th, test method
Standard method NY/T1156.2-2006 is surveyed with reference to raw, using pastille culture medium method：Take each single dose and mixture series dense
The liquid 3mL of degree, adds in the PDA culture medium for the 27mL for being cooled to 45 DEG C, and the pastille culture medium of final concentration is put down required for being made
Plate.Then 6mm diameter mycelia blocks are produced from the citrus anthracnose bacterium colony edge of culture 7 days, moves to each serial pastille culture medium
On, mycelia is face-down, often handles 4 repetitions.It is disposed, is placed in 28 DEG C of constant temperature biochemical cultivation case and cultivates.
5th, data survey and statistical analysis
5.1 investigation method
Test process measures colony diameter after 4 days, calculate growth inhibition ratio (%).
D=D1- D2
In formula：D represents that bacterium colony increases diameter；D1 represents colony diameter；D2 represents bacteria cake diameter.
In formula：I represents mycelial growth inhibition rate；D0Represent that blank control bacterium colony increases diameter；DtRepresent chemicals treatment bacterium colony
Increase diameter.
Statistical result in experimentation is as shown in table 1 below：
Toxicity test initial data of 1 pyraclostrobin of table with difenoconazole mixture to citrus anthracnose bacterium
5.2 synegism evaluation methods
Standard method NY/T1156.6-2006 is surveyed with reference to raw, according to the co-toxicity coefficient method of Sun＆Johnson (1960)
(CTC) evaluate the synergistic effect of pharmacy mix, i.e. CTC≤80 are antagonism, 80<CTC<120 be summation action, CTC >=
120 be synergistic effect.
The toxicity index of mixture theoretical toxicity index (TTI)=medicament A × A medicaments percentage shared in mixture
The toxicity index of (%)+medicament B × B medicaments percentage (%) shared in mixture
5.3 data statistic analysis
All test datas are analyzed using SAS6.12 statistical softwares.Mycelial growth suppression is calculated according to test data
Rate (%) processed, obtains virulence regression equation, related coefficient (r) and EC50(95% confidence limit).6th, interpretation of result and discussion
6.1 evaluating drug effect
The mixture of pyraclostrobin and difenoconazole and its two different proportion combines the virulence to citrus anthracnose bacterium
Measurement result is shown in Table 2.By table 2 as it can be seen that pyraclostrobin and difenoconazole 3: 1,2: 1,1: 1,1: 2 and 1: 3 mixture group
In conjunction, five ratios show synergistic effect to citrus anthracnose bacterium, its EC50Value is respectively 1.20,0.97,0.70,0.71 and
0.75mg/L, co-toxicity coefficient are respectively 142.79,153.87,168.55,138.65 and 121.65.Wherein the two is with 1: 1 ratio
Example mixed synergies are more obvious.
Toxicity test result of 2 pyraclostrobin of table with difenoconazole mixture to citrus anthracnose bacterium
6.2 conclusions are with discussing
Indoor biometrics are the result shows that (being shown in Table 2), and pyraclostrobin is with difenoconazole with 3: 1,2: 1,1: 1,1: 2 and 1: 3
Ratio carry out mixture synergistic effect is shown to citrus anthracnose bacterium, wherein the two with 1: 1 ratio mixed synergies more
Substantially, therefore 1: 1 can be regarded as pyraclostrobin and the optimum proportioning of difenoconazole mixture.And with which kind of ratio in produce reality
Example carries out mixture, still needs and carries out considering decision with reference to synergy virulence, financial cost, processing technology and toxicity etc..
2nd, rabbit skin single irritant test
1st, test objective
The difenoconazole of research embodiment 1-10 and the composite bactericide composition of pyraclostrobin are to animal skin
It is no to have stimulation or corrosiveness, estimate the similar harm being likely to occur during human contact's pesticide.
2nd, criterion and bibliography
National Standard of the People's Republic of China GB15670-1995《Agriculture chemical registration toxicology test method》；
National Standard of the People's Republic of China GB 15670.7《Agriculture chemical registration toxicology test method》, the 7th part is acute
Skin Irritation Test (paper for approval).
3rd, the GLP deferred to
Pesticide toxicology safety evaluatio good laboratory specification (NY/T718-2003) is deferred in this experiment.
4th, materials and methods
4.1 experimental animal
Japan large ear rabbit 20, is provided, animal credit number by Qingdao Kang great bio tech ltd:SCXK (Shandong)
2016002, quality certification number：NO.3700300000289. half male and half female.Weight range 2488.9-3152.0g during body city.Animal
Health, meets Quality of Experimental Animals requirement.
Strain selects reason:Large ear rabbit is the generally acknowledged preferred animal of this kind of experiment, and the strain stabilization characteristics of genetics is right
It is sensitive to be tested test sample.
Health examination is with adapting to:Animal introduce after 24 it is small when interior carry out health examination, health examination qualification animal carry out cage
Card mark and laundering period observation, adapt to 11 days.
4.2 Rearing Condition
Rearing Condition:Animal experiment in this central animals laboratory in carrying out, facility credit number SYXK (L) 2012-
0004.Animal feeding is in feed rack (L167.0XW70.0XH171.0cm)) on suspension type stainless steel raise have cage
(L50.0XW40.0XH40.0cm) in, single cage is educated.
Environmental condition:Animal room temperature:17-23C, humidity:40-70%, artificial lighting, 12 is bright when small, and 12 is dark when small, makes an uproar
Sound is in below 60dB.
Animal welfare:Animal uses and observes National Animal welfare regulation《On treating the guiding opinion of animal kindly》(2006
Year, the Department of Science and Technology).Animal operational version is ratified through Institutional Animal administration committee (IACUC), and experiment process receives its supervision.Examination
Surviving animals are euthanized with being injected intravenously i.v. bolus 10%KCL parenteral solutions after free from worries general anesthesia at the end of testing, corpse
Commission professional institution is uniformly processed.
Ingest and drink water:Animal feed is rabbit upgrowth breeding feed, by Beijing Australia of section pull together feed corporation,Ltd provide.Raise
Material nutritional ingredient and pollutant meet national standard (GB/T14924.3-2010 and GB/T14924.2-2001), and producer provides
Determination of feeds quality is reported.Drink water and prepare pure water for this center HT-R01000 type water cleaning systems.Water quality detects once every year,
Testing index is roughly equal to《Standards for drinking water quality》(GB5749-2006).Any influence examination is not contained in feed and drinking water
Test purpose and test the polluter of integrality.
4.3 test method
4.3.1 dose design
Every animal gives test sample 0.5ml.20 large ear rabbits are divided into 10 groups, every group 2, distinguish EXPERIMENTAL EXAMPLE 1-
10 microbicide compositions, the dosage of every is 0.5ml.
Design considerations:According to National Standard of the People's Republic of China GB 15670-1995《Agriculture chemical registration toxicology test side
Method》Design.
Animal identification:Cage card marks and auricle mark.
4.3.2 animal prepares
Experiment before about 24 it is small when, be close to the hair that skin cuts off experimental animal back backbone both sides.Every piece of unhairing scope is each
About 5cm × 5cm, the dermatotome that only health should be selected lossless are tested.
4.3.3 test sample prepares
Test sample directly acts on animal.
4.3.4 contaminate red method
Test sample active compound is directly applied to plucked dermatotome, upper cover layer of plastic film on the right side of animal；Again with two layers of gauze
Block and covered rearing with plastic film；Then fixed with bandage, tested material is had good contact with skin, prevent that tested material is passive
Thing is licked or sucked.Left side dermatotome is as control.Contaminate after the duration, remaining tested material is removed with clear water cotton balls.
Contaminate the duration:4 it is small when.
4.3.5 observe, measure and check
Symptom Observation：When after removing test sample about 1,24,48,72 is small and recipient site skin was observed in the 4th day,
Do not observe that there is stimulation phenomenon at the red position of dye within the 4th day after contamination, terminate experiment.Every time standard GB/T 15670- is pressed during observation
Skin wound repair grade form carries out dermoreaction scoring (table 3) in 1995 acute skin irritation tests.
Weighing body weight：The weight of animals is weighed before experiment contamination is preceding and observation terminates.
3 skin stress reaction grade form of table
4.3.6 result evaluation
Each point of observation dermoreaction mean scores are calculated, are tried by standard GB/T 15670-1995 acute skin irritations
Test middle skin irritatin strength grading table and carry out strength assessment, be shown in Table 4.
4 skin irritatin strength grading of table
| Intensity | Score value |
| It is nonirritant | 0-0.4 |
| Slight stimulation | 0.5-1.9 |
| Medium irritation | 2.0-5.9 |
| Strong and stimulating | 6.0-8.0 |
4.3.7 experiment deviates
Nothing
4.4 results and conclusion
4.4.1 result
Symptom Observation:After contamination 1 it is small when, the contamination area skin of some rabbits occurs in erythema and oedema in 20 rabbits
There is visible erythema reluctantly and inadequate visible oedema poisoning symptom in toxication shape, some of rabbit contamination area skins, extremely
Symptom occurs and disappears within the 3rd day after contamination, recover normal, but have after the contamination of some rabbits 1 it is small when one contamination after the 1st day contamination position
There is obvious erythema and inadequate visible oedema in skin, and the 2nd day symptom mitigates after contamination, and the 4th day after contamination occurs disease
Shape disappears, and recovers normal.Skin irritation symptom is not observed after separately having the contamination of some rabbits, until observation end is showed no exception
(record for referring to table 5 below), each observing time point skin irritatin average integral be respectively 2.1 when small (1), 1.9 when small (24),
1.5 when small (48), 0.8 when small (72), 0 (4 days).
Weighing body weight:The weight of animals normally increases.
Animal skin stimulates observation result and weight result to be shown in Table 5 and subordinate list 6 respectively.
Result is observed in 5 skin irritatin of table
6 weight result of table
4.4.2 conclusion
It can be obtained from the data of table 5, highest skin irritatin average integral is 2.1 after animal removes test sample, therefore
The composite bactericide composition of embodiment 1-10 is slight stimulation to the skin irritation of rabbit.And from the number of table 6
According to that can obtain, after the test, all there is the phenomenon increased, well-grown in the weight of 20 rabbits.
The above embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The change and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (10)
1. the composite bactericide composition of a kind of difenoconazole and pyraclostrobin, it is characterised in that including according to weight hundred
Divide the following components than meter：
Difenoconazole 1-85%；Pyraclostrobin 1-85%；Auxiliary material, surplus；
Wherein, the auxiliary material is pH adjusting agent, dispersant, wetting agent, bleeding agent, disintegrant, antioxidant, binding agent, anti-corrosion
One kind or any combination in agent, film forming agent, antifreeze, thickener, defoamer, filler and solvent.
2. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that pyrrole
The weight ratio of azoles kresoxim-methyl and difenoconazole is 1：(0.3-3).
3. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that bag
Include following components in percentage by weight：
Difenoconazole 5-50%；Pyraclostrobin 3-50%；Auxiliary material, surplus.
4. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that
In the auxiliary material, the dosage difference of each component is as follows in percentage by weight：PH adjusting agent 0-10%, dispersant 0-10%,
Wetting agent 0-5%, bleeding agent 0-5%, disintegrant 0-10%, antioxidant 0-2%, binding agent 0-10%, preservative 0-2%,
Film forming agent 0-10%, antifreeze 0-10%, thickener 0-5%, defoamer 0-2%, filler 0-80%, solvent 0-80%.
5. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that institute
It is dihydric phosphate to state pH adjusting agent；The dispersant is lignosulfonates, acrylic copolymer salt, polycarboxylate, naphthalene sulphur
One kind or any combination in hydrochlorate formaldehyde condensation products, alkyl benzene sulfonic acid ester；The wetting agent is dodecylphosphoric acid salt, 12
Alkylbenzenesulfonate, fatty alcohol polyoxyethylene ether, sulfocarbolate formaldehyde condensation products, polysulfonate and polyoxyethylene alkyl ether sulfuric acid
One kind or any combination in salt.
6. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that institute
Bleeding agent is stated as one kind or any combination in sulfated castor oil, sodium alkyl sulfonate and sodium alkyl benzene sulfonate；The disintegrant
One kind or any combination in sodium salt are condensed for urea, sodium carbonate, sodium acid carbonate and cyclohexanone；The antioxidant is tertiary butyl
One kind or any combination in hydroquinone, 2,6 di tert butyl 4 methyl phenol and butylated hydroxyarisol.
7. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that institute
Binding agent is stated as one kind or any combination in starch, sodium carboxymethylcellulose and gum arabic；The preservative is benzene first
Acid, dimethyl fumarate and one kind or any combination in benzoisothiazolinone；The film forming agent is polyvinyl alcohol, poly- second two
One kind or any combination in alcohol and gelatin.
8. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that institute
Filler is stated as organobentonite, white carbon, glucose, starch, diatomite, clay, kaolin, sodium chloride, potassium chloride, sodium sulphate
With one kind or any combination in lactose；The solvent is water, ethanol, acetone, toluene, dimethylbenzene, toluene, chlorobenzene, methanol, two
Methylformamide, pyrrolidones, cyclohexanone, dimethyl carbonate, butanol, amylalcohol, lipid, dimethyl sulfoxide (DMSO), petroleum distillate, pine
One kind or any combination in fatty oil, mineral oil, methyl oleate and soybean oil.
9. the composite bactericide composition of difenoconazole as claimed in claim 1 and pyraclostrobin, it is characterised in that institute
Antifreeze is stated as one kind or any combination in ethylene glycol, propane diols, glycerine, urea, sodium chloride and ammonium chloride；The thickening
Agent is xanthans, hydroxymethyl cellulose, hydroxyethyl cellulose, positive cellulose, polyvinyl alcohol and one kind in aluminium-magnesium silicate or
Any combination；The defoamer is silicone oil, organosilicon ketone compound, C10-20 saturated fat acid compounds and C8-10 fat
One kind or any combination in fat alcohol compound.
10. the composite bactericide composition of the difenoconazole and pyraclostrobin as described in claim 1-9 any one, its
Be characterized in that, the composite bactericide composition for pulvis, water dispersible granules, aqueous dispersion tablets, missible oil, aqueous emulsion, suspending agent,
One kind in suspension emulsion, soluble concentrate, microemulsion, dispersible oil-suspending agent and suspension seed-coating agent.
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