CN107873710A - A kind of complex composition and preparation of the lactams of ketoxime containing isolonglifolene and fludioxonil - Google Patents
A kind of complex composition and preparation of the lactams of ketoxime containing isolonglifolene and fludioxonil Download PDFInfo
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- CN107873710A CN107873710A CN201711215409.5A CN201711215409A CN107873710A CN 107873710 A CN107873710 A CN 107873710A CN 201711215409 A CN201711215409 A CN 201711215409A CN 107873710 A CN107873710 A CN 107873710A
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- Prior art keywords
- fludioxonil
- lactams
- isolonglifolene
- ketoxime
- complex composition
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/46—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom rings with more than six members
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings
Abstract
The invention discloses a kind of lactams of ketoxime containing isolonglifolene and the complex composition and preparation of fludioxonil.The complex composition is made up of isolonglifolene ketoxime lactams and fludioxonil.Complex composition and its preparation provided by the invention have obvious synergistic effect relative to single dose; the bacterial disease and some fungi venereal disease evil of various crop can effectively be prevented and treated; so as to reduce the dosage of agricultural chemicals; drug cost is saved; fungicidal spectrum is more extensive, is advantageous to environmental protection and the comprehensive regulation of agricultural pests.
Description
Technical field
The present invention relates to technical field of pesticide, more particularly to the compounding of a kind of ketoxime containing isolonglifolene lactams and fludioxonil
Composition and preparation.
Background technology
The resistance problem of agricultural pests is a global problem.With the continuity of disease chemical prevention, Pesticide use
The increase of amount and not scientifical use agricultural chemicals, the resistance getting worse of germ, the germ species for producing resistance are on the increase.Especially
It is bacterial disease, resistance level is high, and resistance development speed is fast.
As people constantly strengthen the consciousness of environmental protection and social sustainable development, especially 21 century, from plant
New natural drug is found and excavated in resource applied to medical science or agriculturally, has become countries in the world important subject.
It is increasingly difficult to using traditional bactericide of the synthetic method synthesis with excellent activity, and this bactericide that is synthesized is past
It is past that there is certain toxicity, the resistance to the action of a drug and pollution environment etc., for example the agricultural chemicals such as DDT, BHC organochlorine is due to environmental disruption
Property it is relatively strong and be gradually backed out market or be eliminated.Therefore, researching and developing and formulate the newtype drug with autonomous property right turns into medicine
Learn the focus with Pesticide Science research.Oximido ether compound tool has been widely used, for example as bactericide, antifungal agent, weeding
Agent etc., and there is hypotoxicity, low-residual, high activity, widely attract the research interest of research-on-research.Recently, people
Find 1,2,3,4,5,6- hexahydros -1,1,5,5- tetramethyl -7H-2,4 α-methanonaphthalene -7- ketone (Isolongifolenone) is to suppressing
Junket ammonia enzyme and anti-breast cancer have preferably activity, and Isolongifolenone is highly effective to prevention tick and bite by mosquitos, effect
Fruit is better than traditional Metadelphene.
Fludioxonil has efficient, wide spectrum, safer bactericidal action, has preferable bactericidal action to bacterium, fungi etc..
But because its long-time uses, alone its prevents and treats crop disease, and prevention effect is undesirable, and disease also generates certain anti-medicine to it
Property.Therefore, it is necessary to develop a kind of pesticide complex composition efficiently, less toxic, environmentally friendly.
Isolonglifolene ketoxime lactam structure formula is as follows:
The step of preparation process of the compound：Using Isolongifolenone as raw material, different come into leaves is synthesized by addition elimination reaction
Ketenes oxime, then acyl in described isolonglifolene ketoxime should be prepared by the progress Beckmann rearrangement reactions of isolonglifolene ketoxime
Amine.
The content of the invention
Applicant further study show that, show isolonglifolene ketoxime lactams to bacterial disease by substantial amounts of experiment
It is respectively provided with preferable prevention effect and inhibitory action.Bacterium such as staphylococcus aureus, ETEC, pneumonia gram can be suppressed
The primary Salmonella of thunder, proteus vulgaris and pseudomonas aeruginosa and fungi Ru Aspergillus, Exserohilum turcicum, corn line it is withered, fragrant
Any of several broadleaf plants lotus lattice bacterium, banana anthrax etc.；Superior insecticidal action is shown to insect pests such as aphid and planthoppers.The compound has height
Effect, wide spectrum, it is safe to use the characteristics of, be with exploitation for large tonnage product potential quality bactericide.Acute toxicity and environment poison
Property experiment show that isolonglifolene ketoxime lactams belongs to low toxicity compounds, there are good market prospects.
However, a kind of appearance of new drug, if long-term single use, is all inevitably generated resistance, Isolongifolenone
This new type bactericide of oxime lactams is no exception, and single dose uses, and its preventing and treating to pest and disease damage is also difficult to obtain its optimum efficiency.
Therefore, it is to improve the effect of preventing and treating crop disease by isolonglifolene ketoxime lactams and fludioxonil compounding by compounding channel, and
The effective way of delaying drug resistance development.
In view of this, the purpose of the present invention solves above-mentioned technical problem, there is provided a kind of lactams of ketoxime containing isolonglifolene with
The complex composition of fludioxonil, the complex composition have obvious synergistic function relative to single dose, reduce the use of agricultural chemicals
Dose, while delay the resistance to the action of a drug of the pathogen to isolonglifolene ketoxime lactams and fludioxonil.
To realize above-mentioned purpose, use following technical scheme of the invention：A kind of lactams of ketoxime containing isolonglifolene with
The complex composition of fludioxonil, the complex composition are made up of isolonglifolene ketoxime lactams and fludioxonil；Wherein described is different
The mass ratio of longifolene ketoxime lactams and fludioxonil is (40~1)：(1~40).
The complex composition of the above-described lactams of ketoxime containing isolonglifolene and fludioxonil, it is preferable that described different length
The mass ratio of leaf ketenes oxime lactams and fludioxonil is (10~1):(1~10).
The complex composition of the above-described lactams of ketoxime containing isolonglifolene and fludioxonil, it is preferable that described different length
The mass ratio of leaf ketenes oxime lactams and fludioxonil is (5~1):(1~5).
The present invention also provides a kind of preparation of the lactams of ketoxime containing isolonglifolene and fludioxonil, including of the invention provided above
Complex composition and agricultural chemicals on acceptable adjuvant, be then prepared into disinfectant use in agriculture.
The preparation of the above-described lactams of ketoxime containing isolonglifolene and fludioxonil, in order to ensure that bactericide is preferably prevented and treated
Effect, preferably, the weight/mass percentage composition that described complex composition accounts for the disinfectant use in agriculture is 0.1%~90%.
The preparation of the above-described lactams of ketoxime containing isolonglifolene and fludioxonil, it is preferable that described complex composition
The weight/mass percentage composition for accounting for the disinfectant use in agriculture is 1%~80%.
In order to meet different the needs of using, disinfectant use in agriculture of the present invention can be made into a variety of formulations, preferably,
In the offer embodiment of the present invention, the formulation of bactericide is wettable powder, aqueous emulsion, water dispersible granules, seed treatment are done
Pulvis or granule.It is not limited only to formulation provided by the invention.
In order to ensure bactericide in use, having more preferable moisture dispersibility.The present invention disinfectant use in agriculture except including
Also include acceptable adjuvant on agricultural chemicals outside pesticide complex composition.Wherein adjuvant for one kind in filler and solvent and helps
The mixture of agent.
Filler is selected from white carbon, clay, attapulgite, clay, bentonite, kaolin, soil powder, urea or lightweight carbonic acid
One or more in calcium.
Solvent is selected from dimethylbenzene, trimethylbenzene, methyl oleate, ethanol, solvent naphtha, methyl naphthalene or 1-METHYLPYRROLIDONE.
Auxiliary agent of the present invention can according to different dosage forms require to include emulsifying agent, wetting agent, dispersant, defoamer,
Thickener, disintegrant and antifreezing agent, other auxiliary agents that the industry is commonly used can also be included as needed.
Emulsifying agent is selected from polyoxyethylene sorbitan fatty acid ester, AEO, alkyl phenol and epoxy second
Alkane condensation product, NPE, three phenethyl phenol polyethenoxy ethers, double phenethyl phenol polyethenoxy ethers.
Wetting agent is selected from EO/PO block polyethers, AEO, fat alcohol ethoxyl compound, tallow second
Epoxide ammonium salt, alkylnaphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, acyl group glutamate.
Dispersant be selected from naphthalene sulfonic acid condensate sodium salt, phenolsulfonic acid condensation product sodium salt, methyl naphthalene sulfonate formaldehyde condensate,
Sodium lignin sulfonate, sodium metnylene bis-naphthalene sulfonate, acrylate homopolymer sodium salt, polymeric polycarboxylic acid salt, dioctyl sodium sulfosuccinates
Acid sodium-salt, maleic acid-acrylic acid copolymer sodium salt.
Antifreezing agent is selected from ethylene glycol, propane diols, glycerine, isopropanol, urea.
Disintegrant is selected from sodium chloride, potassium carbonate, sodium sulphate, ammonium dihydrogen phosphate.
Binding agent includes polyvinylpyrrolidone, starch, polyvinyl alcohol.
Application of the pesticide complex composition provided by the invention in controlling plant diseases, especially prevent and treat it is bacillary and/
Or the application in fungal disease.
Bactericidal composition of the present invention is applied to preventing and treating crop bacterium venereal disease evil, such as citrus bacterial canker disease, melon bacterium
Property angular leaf spot, solanaceous crops bacterial wilt, soft rot of cabbage, bacterial leaf streak of rice and bacterial leaf-blight, soft rot of cabbage, peanut
Bacterial wilt etc..
Bactericidal composition of the present invention apply also for prevent and treat crop upper part fungal disease, as citrus scab,
Cucurbits fusarium wilt and gray mold, rice blast, rice sheath blight disease, grey mould fruit rot of strawberry etc..
Bactericide of the present invention can be applied by commonsense method, such as be watered spraying cauline leaf process, can also root apply, can be with
Seed dressing or seed pelleting use.It is mainly used in the work such as rice, cucumber, tobacco, tomato, citrus, peanut, soybean, capsicum, grape
Thing.
Complex composition and preparation of the present invention have following advantage compared with prior art：
1st, complex composition and preparation of the invention have obvious synergistic effect relative to single dose, in certain proportioning model
The co-toxicity coefficient for enclosing interior controlling disease is more than 120.Two active components in complex composition are lived in the mechanism of action, interior inhale simultaneously
Property etc. rise complementation, be not both simple superposition.Plant growth, activated plant disease resistance can also be promoted.
2nd, wide sterilization spectrum, lasting period length.Multiple diseases are respectively provided with good prevention effect, is prevented and treated within 14 days after second of medicine
Effect is up to more than 78%.
3rd, delay the service life of new medicament isolonglifolene ketoxime lactams, reduce the development cost of new medicament.
4th, dosage is few, and residual is low, meets the trace standard of pesticide, ecological, environmental protective.
Embodiment
The present invention is illustrated with the following example, but is not limited the scope of the invention.It is used in the present invention different to come into leaves
Ketenes oxime lactams active compound is provided by Guangxi National Univ., and other active compounds used and preparation are purchased in market.Wherein active component
(A) be isolonglifolene ketoxime lactams, active component (B) be fludioxonil.
Preparation prepares embodiment：
First, the formulation of bactericide is the preparation of wettable powder
The isolonglifolene ketoxime lactams fludioxonil wettable powder (40 of embodiment 1 41%:1)
Isolonglifolene ketoxime lactams 40%, fludioxonil 1%, EO/PO block polyethers 5%, naphthalene sulfonic acid condensate sodium salt
8%, attapulgite adds to 100%, and mixture carries out air-flow crushing, and 41% isolonglifolene ketoxime lactams fludioxonil is made can
WP.
The isolonglifolene ketoxime lactams fludioxonil wettable powder (60 of embodiment 2 90%:30)
Isolonglifolene ketoxime lactams 60%, fludioxonil 30%, AEO 1%, methylene dinaphthalene sulfonic acid
Sodium 4%, clay add to 100%, and mixture carries out air-flow crushing, and it is wettable that 90% isolonglifolene ketoxime lactams fludioxonil is made
Property pulvis.
The isolonglifolene ketoxime lactams fludioxonil wettable powder (25 of embodiment 3 30%:5)
Isolonglifolene ketoxime lactams 25%, fludioxonil 5%, alkylnaphthalene sulfonate 4%, acrylate homopolymer sodium salt 9%,
Kaolin adds to 100%, and mixture carries out air-flow crushing, and 30% isolonglifolene ketoxime lactams fludioxonil wettable powder is made
Agent.
The isolonglifolene ketoxime lactams wettable powder of comparative examples (abbreviation CK1) 20%
Isolonglifolene ketoxime lactams 20%, alkylnaphthalene sulfonate 5%, acrylate homopolymer sodium salt 5%, kaolin adds to
100%, mixture carries out air-flow crushing, and 20% isolonglifolene ketoxime lactams wettable powder is made.
The isolonglifolene ketoxime lactams fludioxonil wettable powder (5 of embodiment 4 15%:10)
Isolonglifolene ketoxime lactams 5%, fludioxonil 10%, fatty alcohol polyoxyethylene ether sulfate 8%, maleic acid-the third
Olefin(e) acid copolymer sodium salt 8%, diatomite add to 100%, and mixture carries out air-flow crushing, and acyl in 15% isolonglifolene ketoxime is made
Amine fludioxonil wettable powder.
The isolonglifolene ketoxime lactams fludioxonil wettable powder (20 of embodiment 5 22%:2)
Isolonglifolene ketoxime lactams 20%, fludioxonil 2%, fatty alcohol polyoxyethylene ether sulfate 6%, maleic acid-the third
Olefin(e) acid copolymer sodium salt 3%, bentonite add to 100%, and mixture carries out air-flow crushing, and acyl in 22% isolonglifolene ketoxime is made
Amine fludioxonil wettable powder.
The isolonglifolene ketoxime lactams fludioxonil wettable powder (1 of embodiment 6 41%:40)
Isolonglifolene ketoxime lactams 1%, fludioxonil 40%, acyl group glutamate 4%, sodium lignin sulfonate 10%, mud
Native powder adds to 100%, and mixture carries out air-flow crushing, and 41% isolonglifolene ketoxime lactams fludioxonil wettable powder is made
Agent.
2nd, the formulation of bactericide is the preparation of aqueous emulsion
The isolonglifolene ketoxime lactams fludioxonil aqueous emulsion (1 of embodiment 7 6%：5)
Isolonglifolene ketoxime lactams 1%, fludioxonil 5%, ethanol 15%, 1-METHYLPYRROLIDONE 12%, solvent naphtha
13%, polyoxyethylene sorbitan fatty acid ester 5%, three phenethyl phenol polyethenoxy ethers are 1%, are obtained after stirring oily
Phase；Part water, isopropanol 3% are mixed into uniform aqueous phase；Oil phase is added while high-speed stirred in a kettle
Enter aqueous phase, open cutter and carry out high speed shear, and add remaining water and supply 100%, shearing about half an hour, it is different to be made 6%
Longifolene ketoxime lactams fludioxonil aqueous emulsion.
The isolonglifolene ketoxime lactams fludioxonil aqueous emulsion (0.75 of embodiment 8 1%:0.25)
Isolonglifolene ketoxime lactams 0.75%, fludioxonil 0.25%, 1-METHYLPYRROLIDONE 3%, dimethylbenzene 6% are double
Phenethyl phenol polyethenoxy ether 5%, oil phase is obtained after stirring；Part water, ethylene glycol 7% are mixed into uniform water
Phase；Oil phase is added into aqueous phase while high-speed stirred in a kettle, cutter is opened and carries out high speed shear, and add remaining
Water supplies 100%, shearing about half an hour, 1% isolonglifolene ketoxime lactams fludioxonil aqueous emulsion is made.
The isolonglifolene ketoxime lactams fludioxonil aqueous emulsion (2.5 of embodiment 9 5%:2.5)
Isolonglifolene ketoxime lactams 2.5%, fludioxonil 2.5%, ethanol 5%, trimethylbenzene 12%, aliphatic alcohol polyethenoxy
Ether 3%, double phenethyl phenol polyethenoxy ethers 3%, oil phase is obtained after stirring；Part water, propane diols 7% are mixed into
Uniform aqueous phase；Oil phase is added into aqueous phase while high-speed stirred in a kettle, cutter is opened and carries out high speed shear, and add
Enter remaining water and supply 100%, shearing about half an hour, 5% isolonglifolene ketoxime lactams fludioxonil aqueous emulsion is made.
The isolonglifolene ketoxime lactams fludioxonil aqueous emulsion (1 of embodiment 10 3%:2)
Isolonglifolene ketoxime lactams 1%, fludioxonil 2%, ethanol 8%, methyl naphthalene 10%, alkyl phenol contract with oxirane
Compound 7%, double phenethyl phenol polyethenoxy ethers 3%, oil phase is obtained after stirring；Part water, glycerine 6% are mixed
Into uniform aqueous phase；Oil phase is added into aqueous phase while high-speed stirred in a kettle, cutter is opened and carries out high speed shear, and
Add remaining water and supply 100%, shearing about half an hour, 3% isolonglifolene ketoxime lactams fludioxonil aqueous emulsion is made.
The isolonglifolene ketoxime lactams fludioxonil aqueous emulsion (0.5 of embodiment 11 2.5%:2)
Isolonglifolene ketoxime lactams 0.5%, fludioxonil 2%, dimethylbenzene 5%, three phenethyl phenol polyethenoxy ethers 7%,
Condensation compound of alkyl phenol and epoxy ethane 5%, oil phase is obtained after stirring；Part water, urea 6% are mixed into uniform
Aqueous phase；Oil phase is added into aqueous phase while high-speed stirred in a kettle, cutter is opened and carries out high speed shear, and add residue
Water supply 100%, shearing about half an hour, 2.5% isolonglifolene ketoxime lactams fludioxonil aqueous emulsion is made.
The isolonglifolene ketoxime lactams fludioxonil aqueous emulsion (1 of embodiment 12 10%:9)
Isolonglifolene ketoxime lactams 1%, fludioxonil 9%, dimethylbenzene 4%, methyl oleate 6%, aliphatic alcohol polyethenoxy
Ether 3%, NPE 1%, oil phase is obtained after stirring；Part water, ethylene glycol 6% are mixed into uniform
Aqueous phase；Oil phase is added into aqueous phase while high-speed stirred in a kettle, cutter is opened and carries out high speed shear, and add surplus
Remaining water supplies 100%, shearing about half an hour, 10% isolonglifolene ketoxime lactams fludioxonil aqueous emulsion is made.
3rd, the formulation of bactericide is the preparation of water dispersible granules
The isolonglifolene ketoxime lactams fludioxonil water dispersible granules (38 of embodiment 13 40%：2)
Isolonglifolene ketoxime lactams 38%, fludioxonil 2%, phenolsulfonic acid condensation product sodium salt 3%, dioctyl sodium sulfosuccinates
Acid sodium-salt 6%, potassium carbonate 15%, clay adds to 100%, after airslide disintegrating mill crushes, stirs 30min, is mediated with water, rear to add
It is granulated, dried in fluidized bed granulating and drying machine, 40% isolonglifolene ketoxime lactams fludioxonil water-dispersible grain is made
Agent.
The isolonglifolene ketoxime lactams fludioxonil water dispersible granules (20 of embodiment 14 25%：5)
Isolonglifolene ketoxime lactams 20%, fludioxonil 5%, EO/PO block polyethers 1%, maleic acid-acrylic acid copolymer
Sodium salt 3%, sodium sulphate 8%, soil powder adds to 100%, after airslide disintegrating mill crushes, stirs 30min, is mediated with water, rear to add
It is granulated, dried in fluidized bed granulating and drying machine, 25% isolonglifolene ketoxime lactams fludioxonil water-dispersible grain is made
Agent.
The isolonglifolene ketoxime lactams fludioxonil water dispersible granules (1 of embodiment 15 21%：20)
Isolonglifolene ketoxime lactams 1%, fludioxonil 20%, fat alcohol ethoxyl compound 8%, methylene dinaphthalene sulfonic acid
Sodium 4%, sodium sulphate 15%, attapulgite 15%, precipitated calcium carbonate adds to 100%, after airslide disintegrating mill crushes, stirring
30min, mediated with water, rear add in fluidized-bed granulation dryer is granulated, dried, acyl in 21% isolonglifolene ketoxime is made
Amine fludioxonil water dispersible granules.
The isolonglifolene ketoxime lactams fludioxonil water dispersible granules (4 of embodiment 16 80%：76)
Isolonglifolene ketoxime lactams 4%, fludioxonil 76%, acyl group glutamate 5%, naphthalene sulfonic acid condensate sodium salt 3%,
Sodium chloride 2%, clay adds to 100%, after airslide disintegrating mill crushes, stirs 30min, is mediated with water, and the rear fluid bed that adds is made
It is granulated in grain drying machine, dried, 80% isolonglifolene ketoxime lactams fludioxonil water dispersible granules is made.
The isolonglifolene ketoxime lactams fludioxonil water dispersible granules (1 of embodiment 17 11%：10)
Isolonglifolene ketoxime lactams 1%, fludioxonil 10%, NPE 3%, polymeric polycarboxylic acid salt
6%, the white carbon 12% of sodium sulphate 7%, clay adds to 100%, after airslide disintegrating mill crushes, stirs 30min, is mediated with water,
Add afterwards in fluidized-bed granulation dryer and be granulated, dried, 11% isolonglifolene ketoxime lactams fludioxonil moisture is made
Shot agent.
The isolonglifolene ketoxime lactams fludioxonil water dispersible granules (27 of embodiment 18 30%：3)
Isolonglifolene ketoxime lactams 27%, fludioxonil 3%, three phenethyl phenol polyethenoxy ethers 5%, acrylate homopolymer
Sodium salt 1%, starch 6%, kaolin adds to 100%, after airslide disintegrating mill crushes, stirs 30min, is mediated with water, rear to add
It is granulated, dried in fluidized-bed granulation dryer, 30% isolonglifolene ketoxime lactams fludioxonil water dispersible granules is made.
The isolonglifolene ketoxime lactams fludioxonil water dispersible granules (56 of embodiment 19 60%：4)
Isolonglifolene ketoxime lactams 56%, fludioxonil 4%, fat alcohol ethoxyl compound 6%, sodium lignin sulfonate
5%, polyvinyl alcohol 1%, soil powder adds to 100%, after airslide disintegrating mill crushes, stirs 30min, is mediated with water, rear to add
It is granulated, dried in fluidized-bed granulation dryer, 60% isolonglifolene ketoxime lactams fludioxonil water dispersible granules is made.
4th, the formulation of bactericide is the preparation of seed treatment dry powder doses
The isolonglifolene ketoxime lactams fludioxonil seed treatment dry powder doses (4.5 of embodiment 20 5%:0.5)
Isolonglifolene ketoxime lactams 4.5%, fludioxonil 0.5%, polymeric polycarboxylic acid salt 9%, starch 6%, white carbon
8%, diatomite supplies 100%, is sufficiently mixed, then by ultra-fine grinding to certain particle diameter, obtains acyl in 5% isolonglifolene ketoxime
Amine fludioxonil seed treatment dry powder doses.
The formulation of five bactericide is the preparation of granule
The isolonglifolene ketoxime lactams fludioxonil granule (0.05 of embodiment 21 0.1%：0.05)
Isolonglifolene ketoxime lactams 0.05%, fludioxonil 0.05%, alkylnaphthalene sulfonate 3%, polyvinylpyrrolidone
0.3%, urea adds to 100%, above-mentioned material is well mixed in closed compounding kettle, coating method is granulated, in 120 DEG C of conditions
Lower drying is sieved, 4000 microns of particle size range (μm), through after the assay was approved, that is, obtaining 0.1% different length to particle water content 1%
Leaf ketenes oxime lactams fludioxonil granule.
The isolonglifolene ketoxime lactams fludioxonil granule (1 of embodiment 22 3%：2)
Isolonglifolene ketoxime lactams 1%, fludioxonil 2%, Sodium Polyacrylate 0.6%, acyl group glutamate 7% are wooden
Plain sodium sulfonate 5%, ammonium dihydrogen phosphate 5%, polyvinyl alcohol 6%, clay adds to 100%, above-mentioned material in closed compounding kettle
In be well mixed, coating method is granulated, and is dried under the conditions of 120 DEG C to particle water content 1%, screening, 4000 microns of particle size range
(μm), through after the assay was approved, that is, obtaining 3% isolonglifolene ketoxime lactams fludioxonil granule.
Toxicity Determination
Following indoor biometricses experiment calculates co-toxicity coefficient (CTC) to evaluate mixed effect using the abundant methods of Sun Yun.
Toxicity index TI (B)=(standard agent A EC50The EC of ÷ B agent50)×100
Actual toxicity index ATI (AB)=(A EC50÷ AB EC50)×100
Percentage+TI (B) × B percentages in mixture of theoretical toxicity index TTI (AB)=TI (the A) × A in mixture
Number
Survey toxicity index (ATI)=(standard agent EC50÷ reagent agents EC50)×100
A percentage composition+B medicament toxicity index in theoretical toxicity index (TTI)=A medicament toxicity index × mixture × mixed
B percentage composition in agent
Co-toxicity coefficient (CTC)=[mixture surveys toxicity index (ATI) ÷ mixtures theoretical toxicity index (TTI)] × 100
Evaluation criterion is：Co-toxicity coefficient >=120 show as synergistic effect；Co-toxicity coefficient≤80 show as antagonism；80<
Co-toxicity coefficient<120 show as summation action.
Toxicity Determination embodiment one：Prevent and treat citrus bacterial canker disease
Test method：Experiment reference《Pesticide bioassay technology》(old spring chief editor, publishing house of Beijing Agricultural University go out
Version) and《Farm-chemical indoor determination test rule NY/T1156.2-2006》.This experiment uses inhibition zone method.In sterile behaviour
Make on platform, NA culture mediums are poured on NA flat boards, after drying, take 0.1ml citrus processing bacteria suspension spreading rod uniform
Ground is applied on NA flat boards.After drying, punched with diameter 7mm card punch in flat board center, then take 100 μ l decoctions in aperture
In.5 repetitions of each concentration.To add the processing of sterilized water in aperture as blank control.28 ± 0.5 DEG C of perseverance is placed on after processing
Incubator sterile culture, take out after 2d.Crossing method is used to measure the antibacterial circle diameter (in units of millimeter) of each processing respectively,
And calculate the average value of antibacterial circle diameter, inhibiting rate.Statistical analysis is carried out with DPS data processing softwares, calculates each medicament
EC50, then calculate co-toxicity coefficient (CTC) by the abundant methods of Sun Yun.
The Toxicity Determination result of the isolonglifolene ketoxime lactams of table 1 and fludioxonil compounding preventing and treating citrus bacterial canker disease
From table 1, isolonglifolene ketoxime lactams and fludioxonil are compounded in above ratio, in 14 proportionings, (40~
1)：The co-toxicity coefficient of different ratio preventing and treating citrus bacterial canker disease is all higher than 120 between (1~40), has synergy in varying degrees
Effect；When proportioning is in (10~1)：When between (1~10), co-toxicity coefficient is more than 150, and synergy is especially pronounced.
Toxicity Determination embodiment two：Prevent and treat tobacco bacterial wilt
Test method：After tobacco bacterial wilt pathogen is activated on NA culture mediums, bacterium stoste is made into sterilized water, by bacterium
Stoste is diluted to the bacteria suspension that the clump count grown after coated plate 100ul is 100 or so, standby.
Take 400ul bacteria suspensions to be mixed with equivalent agricultural chemicals single dose, take 100ul with liquid-transfering gun, be placed in the NA flat boards being ready for
On, bacteria suspension is coated with to uniform, 28 DEG C of culture 48h, counting clump count with sterilized " L " shape glass bar, and calculate by formula
Bacteriostasis rate, bacterium colony inhibiting rate (%)=(control clump count-processing clump count)/control clump count × 100, often processing repeat 4
It is secondary, replace pesticide-treated to use Excel software analysis as control, the result of gained, calculate the EC of each medicament using sterilized water50, and
Co-toxicity coefficient is calculated according to the abundant methods of Sun Yun.
The Toxicity Determination result of the isolonglifolene ketoxime lactams of table 2 and fludioxonil compounding preventing and treating tobacco bacterial wilt
From table 2, isolonglifolene ketoxime lactams and fludioxonil are compounded in above ratio, in 14 proportionings, (40~
1)：Between (1~40), the co-toxicity coefficient of different ratio preventing and treating tobacco bacterial wilt is all higher than 120, has synergy in varying degrees
Effect；When proportioning is in (10~1)：When between (1~10), co-toxicity coefficient is more than 153, and synergy is especially pronounced.
Toxicity Determination embodiment three：Prevent and treat Muskmelon Fusarium wilt
Test method：Experiment reference《Pesticide bioassay technology》(old spring chief editor, publishing house of Beijing Agricultural University go out
Version) and《Farm-chemical indoor determination test rule NY/T1156.2-2006》.This experiment uses inhibition zone method.In sterile behaviour
Make on platform, NA culture mediums are poured on NA flat boards, after drying, take 0.1ml Muskmelon Fusarium wilt bacteria suspension spreading rod equably
It is applied on NA flat boards.After drying, punched with diameter 7mm card punch in flat board center, then take 100 μ l decoctions in aperture.
5 repetitions of each concentration.To add the processing of sterilized water in aperture as blank control.28 ± 0.5 DEG C of constant temperature is placed on after processing
Case sterile culture, take out after 2d.Crossing method is used to measure the antibacterial circle diameter (in units of millimeter) of each processing respectively, and
Calculate average value, the inhibiting rate of antibacterial circle diameter.Statistical analysis is carried out with DPS data processing softwares, calculates the EC of each medicament50,
Then co-toxicity coefficient (CTC) is calculated by the abundant methods of Sun Yun.
The Toxicity Determination result of the isolonglifolene ketoxime lactams of table 3 and fludioxonil compounding preventing and treating Muskmelon Fusarium wilt
From table 3, isolonglifolene ketoxime lactams and fludioxonil are compounded in above ratio, in 14 proportionings, (40~
1)：The co-toxicity coefficient of different ratio preventing and treating Muskmelon Fusarium wilt is all higher than 120 between (1~40), has synergy in varying degrees
Effect；When proportioning is in (10~1)：When between (1~10), co-toxicity coefficient is more than 150, and synergy is especially pronounced.
Field efficacy embodiment
Indoors on the basis of toxicity test, in order to further verify isolonglifolene ketoxime lactams and fludioxonil compounding group
Whether compound has synergistic effect and its control in field effect to bacterial disease and fungal disease, invention in field
People passes through substantial amounts of field control effectiveness test, and result of the test is as follows：
CK1：20% isolonglifolene ketoxime lactams WP (self-control)
CK2：15% fludioxonil wettable powder, it is purchased in market.
Note：Isolonglifolene ketoxime lactams is referred to as with lower part Isolongifolenone oxime lactams
Field test embodiment one：Prevent and treat citrus bacterial canker disease field control effectiveness test
Test method：With reference to the part of GB/T17980.103-2004 pesticide field efficacy medicine tests criterion (two) the 103rd：Sterilization
Agent prevents and treats citrus bacterial canker disease；
Controlling object：Citrus bacterial canker disease
Test site：Nanning Shi Bu
Experimental plot：24 cells, random alignment are chosen, each 3 plants of cell each handles 4 repetitions into age fruit tree；
Test method：Using directed spraying method, first time dispenser is away from second of spraying time at intervals of 7 days.
Investigation method：Two plants are investigated per cell, 5 points are taken on every plant, every is chosen 10 fruits and two blade tips, before dispenser
Investigation once, is investigated once for 20 days after first time dispenser.
Table 4 prevents and treats the field control effectiveness test result of citrus bacterial canker disease
From result of the test table 4, when preventing and treating citrus bacterial canker disease, isolonglifolene ketoxime lactams+fludioxonil and single dose
Isolonglifolene ketoxime lactams or fludioxonil are compared, in the case where active ingredient dosage is less, acyl in isolonglifolene ketoxime
Amine+fludioxonil (active ingredient dosage 20g/667m2) the 7d prevention effects of preventing and treating citrus bacterial canker disease are higher by that single dose is different to come into leaves
Ketenes oxime lactams (active ingredient dosage 25g/667m2) and single dose fludioxonil (active ingredient dosage 25g/667m2)；And
And remained in 14d preventive effect up to more than 79%, the lasting period is grown.
Field test embodiment two：Prevent and treat tobacco bacterial wilt field control effectiveness test
Test method：With reference to the part of NY/T 1464.32-2010 pesticide field efficacy medicine tests criterion the 32nd：Bactericidal agent for preventing and treating
Bacterial wilt of tomato；
Controlling object：Tobacco bacterial wilt
Test site：Nanning Shi Bu
Experimental plot：36 cell is chosen, random alignment, 9 groups is divided into, every group of 4 repetitions, totally 9 corresponds to 9 processing.
Test method：Using directed spraying method, first time dispenser is away from second of spraying time at intervals of 7 days.
Investigation method：Before medicine, 7 days and 14 days after medicine, each cell whole plant is investigated respectively, records total strain number and diseased plant number
Table 5 prevents and treats the field control effectiveness test result of tobacco bacterial wilt
From result of the test table 5, when preventing and treating tobacco bacterial wilt, isolonglifolene ketoxime lactams+fludioxonil and single dose
Isolonglifolene ketoxime lactams or fludioxonil are compared, in the case where active ingredient dosage is less, acyl in isolonglifolene ketoxime
Amine+fludioxonil (active ingredient dosage 25g/667m2) the 7d prevention effects of preventing and treating tobacco bacterial wilt are higher by that single dose is different to come into leaves
Ketenes oxime lactams (active ingredient dosage 30g/667m2) and single dose fludioxonil (active ingredient dosage 30g/667m2)；And
And remained in 14d preventive effect up to more than 80%, the lasting period is grown.
Field test embodiment three：Prevent and treat Muskmelon Fusarium wilt field control effectiveness test
Test method：With reference to the part of GB/T17980.113-2004 pesticide field efficacy medicine tests criterion (two) the 113rd：Sterilization
Agent prevents and treats cucurbits fusarium wilt.
Controlling object：Muskmelon Fusarium wilt；
Test site：Nanning Shi Bu；
Experimental plot：36 cells are chosen, random alignment, each ㎡ of cell 20, each handle 4 repetitions；
Test method：Using directed spraying method, first time dispenser is away from second of spraying time at intervals of 7 days.
Investigation method：Muskmelon morbidity strain number and total strain number in cell are investigated, is investigated before dispenser once, 7 days and 14 after dispenser
It is investigated once respectively.
Table 6 prevents and treats the field control effectiveness test result of Muskmelon Fusarium wilt
From result of the test table 6, when preventing and treating Muskmelon Fusarium wilt, isolonglifolene ketoxime lactams+fludioxonil and single dose
Isolonglifolene ketoxime lactams or fludioxonil are compared, and in active ingredient dosage, identical (active ingredient dosage is 20g/
667m2) in the case of, the 7d prevention effects of isolonglifolene ketoxime lactams+fludioxonil preventing and treating Muskmelon Fusarium wilt are above single dose
Isolonglifolene ketoxime lactams and single dose fludioxonil, illustrate that the two compounding use synergy is obvious；And remain to reach in 14d preventive effect
More than 78%, lasting period length.
Claims (8)
- A kind of 1. complex composition of lactams of ketoxime containing isolonglifolene and fludioxonil, it is characterised in that the complex composition It is made up of isolonglifolene ketoxime lactams and fludioxonil；Wherein described isolonglifolene ketoxime lactams and the mass ratio of fludioxonil For (40~1)：(1~40).
- 2. the complex composition of the lactams of ketoxime containing isolonglifolene according to claim 1 and fludioxonil, it is characterised in that The mass ratio of the isolonglifolene ketoxime lactams and fludioxonil is (10~1):(1~10).
- 3. the complex composition of the lactams of ketoxime containing isolonglifolene according to claim 2 and fludioxonil, it is characterised in that Described isolonglifolene ketoxime lactams and the mass ratio of fludioxonil are (5~1):(1~5).
- 4. the preparation of a kind of lactams of ketoxime containing isolonglifolene and fludioxonil, it is characterised in that including described in claims 1 to 3 Complex composition and agricultural chemicals on acceptable adjuvant, be then prepared into disinfectant use in agriculture.
- 5. the preparation of the lactams of ketoxime containing isolonglifolene according to claim 4 and fludioxonil, it is characterised in that described multiple The weight/mass percentage composition that the disinfectant use in agriculture is accounted for composition is 0.1%~90%.
- 6. the preparation of the lactams of ketoxime containing isolonglifolene according to claim 5 and fludioxonil, it is characterised in that described multiple The weight/mass percentage composition that the disinfectant use in agriculture is accounted for composition is 1%~80%.
- 7. the preparation of the lactams of ketoxime containing isolonglifolene according to claim 4 and fludioxonil, it is characterised in that the agriculture It is wettable powder, aqueous emulsion, water dispersible granules, seed treatment dry powder doses or granule with the formulation of bactericide.
- 8. application of the complex composition as described in any one of claims 1 to 3 in controlling plant diseases, described phytopathy Evil is crops are bacillary and/or fungal disease.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102017954A (en) * | 2010-12-22 | 2011-04-20 | 陕西韦尔奇作物保护有限公司 | Fludioxonil-containing bactericidal composition |
| CN106588772A (en) * | 2016-12-19 | 2017-04-26 | 广西中医药大学 | Heavy turpentine longifolene derivative, preparation thereof and application |
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2017
- 2017-11-28 CN CN201711215409.5A patent/CN107873710A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102017954A (en) * | 2010-12-22 | 2011-04-20 | 陕西韦尔奇作物保护有限公司 | Fludioxonil-containing bactericidal composition |
| CN106588772A (en) * | 2016-12-19 | 2017-04-26 | 广西中医药大学 | Heavy turpentine longifolene derivative, preparation thereof and application |
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