CN100360020C - Flusilazole-and kresoxim methyl bactericide composition and its prepn process - Google Patents
Flusilazole-and kresoxim methyl bactericide composition and its prepn process Download PDFInfo
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- CN100360020C CN100360020C CNB2006100130299A CN200610013029A CN100360020C CN 100360020 C CN100360020 C CN 100360020C CN B2006100130299 A CNB2006100130299 A CN B2006100130299A CN 200610013029 A CN200610013029 A CN 200610013029A CN 100360020 C CN100360020 C CN 100360020C
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Abstract
The present invention relates to a bactericide composition, the preparation thereof and the application thereof. The present invention discloses a bactericide composition containing hydrofluosilicic oxazole and kresoxim-methyl. The present invention is characterized in that the part by weight ratio of the hydrofluosilicic oxazole to the kresoxim-methyl on the basis of active components is from 1:50 to 50:1, and if right quantities of auxiliary agents or carriers are added to the composition, an emulsifiable solution, wettable powder, an aqueous emulsion, a suspension agent, a water dispersion granule and an oil solution can be prepared. The composition can be used for preventing and curing various plant diseases caused by disease fungi, and through the certification of indoor tests, the composition has an obvious synergistic effect. Simultaneously, the composition can delay the occurrence and the development of the agricultural chemical resistance of two single agents.
Description
Technical field
The present invention relates to microbicide compositions, preparation method and application.
Background technology
Flusilazole is the outstanding kind in the azoles fungicide.The multiple diseases that sac fungi, basidiomycetes, imperfect fungus are caused has good control efficiency, is widely used in the chemical control of diseases such as apple, pears, scab of cucumber, powdery mildew, cladosporium leaf and fruit mould of tomato, anthracnose of grape, room rot, vegetables powdery mildew, beans rust.Have prevention and result of treatment simultaneously.The mechanism of action of this bactericide is to suppress the biosynthesis of ergosterol in the fungus body, and ergosterol is the constituent of fungal cell membrane.Therefore ergosterol is suppressed, and can cause damaged membrane, thalline death.This medicament began to use in China from nineteen nineties, and at first obtained great success in pears, scab of cucumber aspect preventing and treating.After this continue to expand to the chemical control of other crop multiple diseases again, be still the outstanding kind in China's bactericide so far.But Flusilazole is the same with other ergosterol biosynthesis inhibitors, all has a perplexing problem in use.Here it is, and access times are too much continuously, all can suppress the growth of crop to a certain extent.In addition, Flusilazole promptly is under normal working concentration, also can exert an influence to kind young fruits such as crisp pears or southern part of the country pears, causes that pericarp thickens, quality descends.
Kresoxim-methyl is the outstanding kind in the methoxy acrylate series bactericidal agent.Be widely used in crops such as cereal crop, apple, pears, grape, strawberry, vegetables, most of diseases that pathomycetes such as sac fungi, imperfect fungus and oomycetes are caused have protection, treat and root out activity.Have characteristics such as efficient, wide spectrum, lasting period be long.The mechanism of action of this bactericide is the electron transfer process of cytochrome b and cytochrome c in the blocking-up respiratory chain, belongs to the mitochondrial respiratory inhibitor.Because therefore its mechanism of action uniqueness does not have mutual pesticide resistance with other common fungicides.
In addition, no matter be kresoxim-methyl, or Flusilazole, the same with many efficient germicides, long-term, continuous, single use, problem all can develop immunity to drugs.How prolonging the useful life of these medicaments, is the problem that people pay close attention to.
Summary of the invention
Be postponement Flusilazole, the drug-fast generation of kresoxim-methyl or development, and overcome Flusilazole, the invention discloses a kind of microbicide compositions, preparation of compositions and application that contains Flusilazole and kresoxim-methyl in use to the adverse effect of some crop.
Flusilazole (english common name flusilazole), chemical name: two (4-fluorophenyl) methyl (1H-1,2, the support of 4-triazol-1-yl methylene) silane
Kresoxim-methyl (english common name kresoxim-methyl), chemical name: methyl (E)-2-methoxyimino-2-[2-(0-toloxyl) phenyl] methyl acetate
Have now found that the present invention proposes contains Flusilazole and kresoxim-methyl sterilizing composite, plant diseases such as wheat powdery mildew, scab of cucumber, pepper anthracnose is had obvious synergistic effect, and can overcome the negative effect of Flusilazole to some crop.In addition, because Flusilazole is different with kresoxim-methyl chemical constitution type, have diverse mechanism of action, the two is composite to delay drug-fast generation of pathogen and development.
Two kinds of active component ratios of weight and number of Flusilazole in the microbicide compositions of the present invention and kresoxim-methyl are 1: 50 to 50: 1.
Two kinds of preferred ratios of weight and number of active component of Flusilazole in the microbicide compositions of the present invention and kresoxim-methyl are 1: 25 to 25: 1.
The active component weight percentage is 1% to 90% in the bactericidal composition of the present invention.
The present composition can be prepared into missible oil, wetting powder, aqueous emulsion, suspending agent or water dispersion granule and finish.
At least contain a kind of carrier and a kind of auxiliary agent in the present composition, wherein at least a is surfactant.
The organic solvent that the present invention is fit to comprises that the polar solvent of aromatic hydrocarbons, chlorinated aromatic hydrocarbons, chlorinated aliphatic hydrocarbon, aliphatic hydrocarbon, particularly suitable is, for example isopropyl alcohol, butanols, ethylene glycol, diethylene glycol (DEG), triethylene glycol, propane diols, glycerine, sorbierite, phenmethylol, cyclohexanol, and No. two, acetone, MEK, methyl iso-butyl ketone (MIBK), cyclohexanone, butyrolactone, dimethyl formamide, pyrrolidones, aromatic hydrocarbons.Simultaneously, also have vegetable oil and the molten fiber of methyl.
Surfactant can be emulsifier, dispersant or wetting agent.Can make nonionic or ionic.For example, lauryl sodium sulfate, Teepol, neopelex, calcium dodecyl benzene sulfonate, polyoxyethylene fatty acid ester, polyoxyethylene aliphatic alcohol ether, the polyoxyethylene fatty amine, or directly use commercially available emulsifier, as the newborn 0201B of farming, the newborn 0203B of farming etc., the material that is used as dispersant and wetting agent has: sodium lignin sulfonate, draw back powder, calcium lignosulfonate and lauric acid sodium sulphate, alkylol polyoxyethylene groups ether sodium sulfate, octylphenol polyethylene oxyethylene group ether sulfate, alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, sodium alkyl sulfonate, neopelex etc.
Adhesive; can be for example carbonyl methyl cellulose, polyvinyl alcohol or the polyvinyl acetate that synthesize or natural water-soluble polymer for example xanthans, gelatin, gum Arabic, polyvinylpyrrolidone, aluminium-magnesium silicate, polyvinyl alcohol, polyethylene glycol phenolic resins, shellac, sodium alginate etc., add in the preparation with powder, particle or latex form.
Defoamer is: bubble enemy, silicone, phosphoric acid ester and acid amides etc.
The solid carrier that is fit to comprises natural or synthetic clay and silicate, is applicable to that the solid carrier of pulvis comprises rock dust, quartz, clay, imvite, silica, diatomite, float stone, gypsum, talcum, bentonite, kaolin, potter's clay, the white carbon of natural formation and for example microdispersed silicic acid of the mineral matter that grinds or the aluminium oxide that synthesizes.The particulate vector that is fit to comprises pulverizing and natural rock classification for example calcite, marble, float stone, sepiolite and dolomite and the synthetic particle made by the powder of organic matter and inorganic matter.
Composition of the present invention can be used for control by disease fungus such as imperfect fungus, sac fungi, the microbial plurality of plant diseases of load, as the powdery mildew on cereal, wheat, paddy rice, grape, strawberry, cucumber, custard squash, capsicum, pimento, eggplant, tomato, Kidney bean, cowpea, leek, lettuce, Chinese cabbage, sunflower, lichee, tobacco, rubber, banana and some Chinese herbal medicines, flowers, lawn etc., leaf mold, scab etc.
The present invention also comprises a kind of method of field control disease.Here it is before or after crop is susceptible, uses composition of the present invention to the place of crop or fruit and growth thereof.Can use by common method, as spraying, spray, dust and pouring.Amount of application of the present invention changes with weather condition and crop onset state.The duration of cover crop is relevant with the content of individualized compound in the composition, also relevant with the amount of application of composition usually.
The characteristics and the beneficial effect of the present composition are: 1, composition shows fabulous synergistic effect in certain ratio range, and the protection effect of composition is significantly improved than its single agent.2, overcome the negative effect of Flusilazole to some crop.3, because two single thinner architectural differences of this composition are very big, the mechanism of action is different fully, does not have mutual pesticide resistance, can delay two single agent and use the pesticide resistance problem that is produced separately.
Description of drawings
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Embodiment
The invention will be further described with following non-limiting embodiment in the present invention, and the percentage among the embodiment all is weight percentage, and the treatment dosage of biologically-active moiety is active constituent content.
1. the preparation of missible oil
By the prescription requirement, add solvent, former medicine, emulsifier respectively, mix, heat of solution a little in case of necessity promptly obtains transparence missible oil.Fill a prescription as embodiment 1-2.
Embodiment 1 (15% missible oil)
Flusilazole 2.0%
Kresoxim-methyl 13.0%
The newborn 500# 5.0% of farming
Dimethyl formamide 5.0%
Dimethylbenzene complements to 100%
Embodiment 2 (20% missible oil)
Flusilazole 1.5%
Kresoxim-methyl 18.5%
The newborn 500# 7.5% of farming
The newborn OX-653 2% of farming
Methyl alcohol 10%
Dimethylbenzene complements to 100%
2. wetting powder preparation
By the prescription requirement, former medicine, various auxiliary agent and filler etc. are fully mixed, after ultra tiny pulverizing machine is pulverized, promptly obtain product.Fill a prescription as embodiment 3-4.
Embodiment 3 (15% wetting powder)
Flusilazole 2.5%
Kresoxim-methyl 12.5%
Lauryl sodium sulfate 2%
White carbon 5%
Lignin matter sodium sulfonate 5%
Precipitated calcium carbonate is supplemented to 100%
Embodiment 4 (50% wetting powder)
Flusilazole 10%
Kresoxim-methyl 40%
Lauryl sodium sulfate 2%
White carbon 8%
Lignin matter sodium sulfonate 5%
Precipitated calcium carbonate is supplemented to 100%
3. aqueous emulsion preparation
Former medicine, solvent, emulsifier are added together, make and be dissolved into even oil phase, water, antifreeze etc. is mixed, become the homogeneous water.Under high-speed stirred, water is joined oil phase or oil phase is joined water, form the aqueous emulsion of favorable dispersibility.As embodiment 5 prescriptions.
Embodiment 5 (15% aqueous emulsion)
Flusilazole 3%
Kresoxim-methyl 12%
Polyvinyl alcohol 1%
Alkylaryl polyoxyethylene poly-oxygen propylene aether 9%,
Farming breast 2,201 13%
Dimethyl formamide 10%
Ethylene glycol 10%
Water complements to 100%
4. the preparation of water dispersion granule
Former medicine and powder carrier, wetting agent, spreader-sticker and binding agent etc. are mixed pulverizing, after adding water again and mediating, add in the comminutor that the certain specification screen cloth is housed and carry out granulation.Drying, screening (pressing the screen cloth scope) promptly get granular product again.As embodiment 6 prescriptions.
Embodiment 6 (40% water dispersion granule)
Kresoxim-methyl 35%
Flusilazole 5%
Methyl naphthalene sulfonate formaldehyde condensate 10%
Neopelex 15%
Soluble starch 15%
Protruding Attapulgite complements to 100%
5. the preparation of suspending agent
By the prescription requirement, be medium with water, former medicine, dispersant, suspending agent and antifreezing agent etc. are added in the sand milling still, carry out porphyrize, make suspending agent.As embodiment 7 prescriptions.
Embodiment 7 (25% suspending agent)
Kresoxim-methyl 20%
Flusilazole 5%
Methyl naphthalene sulfonate formaldehyde condensate 7%
0203B 5％
Aluminium-magnesium silicate 0.5%
Ethylene glycol 10%
Water complements to 100%
6, finish
By the prescription requirement, former medicine is dissolved in the mixed solvent adds surfactant, antifreeze, be heated into homogeneous phase solution slightly, filter and promptly make finish, available fog machine spraying hot mist.Also available ultra-low-volume sprayer sprays cold mist.
7. biologically active exsomatizes
Adopt biomass growth rate method (mycelium growth rate test). measure embodiment 5 (15% aqueous emulsion) to dosporium cucumerinumand its and embodiment 4 (40% wetting powder agent) co-toxicity to asparagus stem wilt bacteria.Reagent agent is diluted to design concentration, gets in 1 milliliter of injection culture dish, add 9 milliliters of PSA medium again, make the pastille flat board of 10 times of ultimate density dilutions after shaking up.Make blank to add 1 milliliter of aqua sterilisa.Get the bacterium dish with 4 millimeters card punch of diameter along beating for examination flora outer rim, place in the pastille flat board, 24 ± 1 ℃ of dark culturing 72 hours, bacterium dish expansion diameter is respectively handled in metering, calculate thalli growth and suppress percentage, calculate medicament 50% effective concentration (EC by concentration logarithm-inhibiting rate probability value method
50), further adopt the abundant method of Sun Yun to calculate co-toxicity coefficient.The result shows two mixture co-toxicity coefficients all obviously greater than 100, represents that this mixture has synergistic effect.Result of the test is seen embodiment 8-9.
The co-toxicity of 8 pairs of scabs of cucumber of embodiment (Cladosporium cucumerinum)
| Reagent agent | Experimental concentration (μ gml -1) | 50% effective concentration (EC 50) (μg·ml -1) | Co-toxicity coefficient | ||||
| 5.0 | 2.5 | 1.25 | 0.625 | 0.3125 | |||
| The former medicine embodiment 5 of the former medicine kresoxim-methyl of Flusilazole (15% aqueous emulsion) | 79.9 88.6 92.5 | 67.5 70.5 81.5 | 54.2 61.7 70.2 | 46.1 50.1 58.1 | 35.6 45.5 43.0 | 0.82 0.54 0.45 | - - 128.6 |
The co-toxicity of 9 pairs of asparagus stem wilts of embodiment (Phoma asparagi)
| Reagent agent | Experimental concentration (μ gml -1) | 50% effective concentration (EC 50) (μg·ml -1) | Co-toxicity coefficient | ||||
| 5.0 | 2.5 | 1.25 | 0.625 | 0.3125 | |||
| The former medicine embodiment 4 of the former medicine kresoxim-methyl of Flusilazole (40% wetting powder) | 86.3 95.7 97.1 | 73.0 76.1 85.6 | 58.5 66.6 73.7 | 49.8 54.1 61.0 | 38.4 49.1 45.2 | 0.66 0.46 0.43 | - - 115 |
8. greenhouse pot culture test
Trial crops is cultured to 2-3 leaf phase seedling in the greenhouse, by design concentration to the seedling leaves processing of spraying, inoculation test pathogen after 24 hours after the chemicals treatment.Result's investigation is carried out in the cultivation of then seedling being preserved moisture under 25 ± 1 ℃ after the blank of not dispenser is fully fallen ill.Disease classification, control efficiency computational methods are all undertaken by State Standard of the People's Republic of China's " pesticide field efficacy medicine test criterion ".Result of the test shows that Flusilazole and kresoxim-methyl are mixed and have tangible control efficiency.The results are shown in embodiment 10-11.
Embodiment 10 control wheat powdery mildew (Erysiphe graminis) effects
| Reagent agent | Experimental concentration (μ g.ml -1) | |||
| 50 | 25 | 12.5 | 6.25 | |
| 40% Flusilazole missible oil, 20% kresoxim-methyl missible oil embodiment 1 (15% missible oil) | 100 100 100 | 98.5 100 100 | 93.6 95.5 96.3 | 87.4 90.7 93.6 |
Embodiment 11 prevents and treats scab of cucumber (Cladosporium cucumerinum) effect
| Reagent agent | Experimental concentration (μ g.ml -1) | |||
| 50 | 25 | 12.5 | 6.25 | |
| 40% Flusilazole missible oil, 20% kresoxim-methyl missible oil embodiment 7 (25% suspending agent) | 100 100 100 | 100 98.7 100 | 90.6 84.5 93.4 | 77.8 66.5 83.8 |
9. field trial
The powdery mildew of strawberry test is carried out on protection ground, and the test of pears (southern part of the country pears) scab is carried out at the land milpa.Reagent agent is embodiment 1 (15% missible oil).If 3 dosage, 4 repetitions are made blank with not dispenser.The experimental field is natural occurrence and dispenser at the initial stage of a disease.When fully falling ill, blank carries out state of an illness investigation.Disease classification, preventive effect computational methods are all undertaken by State Standard of the People's Republic of China's " pesticide field efficacy medicine test criterion ".Result of the test shows that Flusilazole and kresoxim-methyl are mixed and not only control powdery mildew of strawberry, pear scab are had good control efficiency, and crop is had no effect.The results are shown in embodiment 12-13.
12 pairs of powdery mildew of strawberries of embodiment (Sphaerotheca humuli) control efficiency
| Reagent agent | Control efficiency (%) | Influence to crop | ||
| 100g.ai/ha | 50g.ai/ha | 25g.ai/ha | ||
| 40% Flusilazole missible oil | 85.9 | 67.5 | 51.1 | Plant has dwarfism |
| 20% kresoxim-methyl missible oil embodiment 1 (15% missible oil) | 91.7 92.2 | 85.9 87.6 | 70.9 78.8 | Normal |
13 pairs of pears scab of embodiment (Venturia irina) control efficiency
| Reagent agent | Control efficiency (%) | Influence to crop | ||
| 200g.ai/ha | 100g.ai/ha | 50g.ai/ha | ||
| 40% Flusilazole missible oil, 20% kresoxim-methyl missible oil embodiment 1 (15% missible oil) | 94.7 95.7 98.9 | 90.0 93.1 95.5 | 87.5 89.3 91.1 | The pericarp thickening is normal |
Claims (6)
1, a kind of microbicide compositions is characterized in that: the active component in the composition is Flusilazole and kresoxim-methyl, and the ratio of weight and number of Flusilazole and two kinds of active components of kresoxim-methyl is 1: 25 to 25: 1 in the composition.
2, Flusilazole and the kresoxim-methyl sterilizing composite of containing according to claim 1, it is characterized in that: the active component weight percentage in the composition is 1% to 90%.
3, Flusilazole and the kresoxim-methyl sterilizing composite of containing according to claim 1, it is characterized in that: said composition can be mixed with missible oil, aqueous emulsion, wetting powder, suspending agent or water dispersion granule and finish.
4, Flusilazole and the kresoxim-methyl sterilizing composite of containing according to claim 1 is characterized in that: contain a kind of carrier and a kind of auxiliary agent in the composition at least, wherein at least a is surfactant.
5, the described application that contains Flusilazole and kresoxim-methyl sterilizing composite of claim 1 is characterized in that: be used for control by imperfect fungus, sac fungi, the microbial plant disease of load.
6, the described application that contains Flusilazole and kresoxim-methyl sterilizing composite of claim 5 is characterized in that: the field control plant disease is before or after crop is susceptible, to crop applying claim 1 or 3 described bactericidal compositions.
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| CNB2006100130299A CN100360020C (en) | 2006-01-11 | 2006-01-11 | Flusilazole-and kresoxim methyl bactericide composition and its prepn process |
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| CN100360020C true CN100360020C (en) | 2008-01-09 |
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Families Citing this family (4)
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| CN101779656B (en) * | 2009-12-18 | 2013-04-10 | 陕西美邦农资贸易有限公司 | Bactericidal composite containing flusilazole and kresoxim-methyl |
| CN101720780B (en) * | 2010-01-05 | 2012-09-26 | 陕西美邦农资贸易有限公司 | Bactericidal composition containing flusilazole and probenazole |
| CN102349506B (en) * | 2011-09-13 | 2014-07-09 | 广西田园生化股份有限公司 | Ultralow-volume solvent containing Flusilazole |
| CN102835418A (en) * | 2012-08-22 | 2012-12-26 | 广西田园生化股份有限公司 | Sterilization combination containing simeconazole and methoxy acrylic ester germicides |
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|---|---|---|---|---|
| WO1997000012A1 (en) * | 1995-06-16 | 1997-01-03 | Novartis Ag | Crop protection compositions |
| CN1385070A (en) * | 2001-05-10 | 2002-12-18 | 沈阳化工研究院 | Disinfectant composition containing flumorph |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997000012A1 (en) * | 1995-06-16 | 1997-01-03 | Novartis Ag | Crop protection compositions |
| CN1385070A (en) * | 2001-05-10 | 2002-12-18 | 沈阳化工研究院 | Disinfectant composition containing flumorph |
Non-Patent Citations (1)
| Title |
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| 防治梨黑星病田间药效试验. 太一梅等.农药，第3期. 2004 * |
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