CN100444731C - Germicide composition - Google Patents

Germicide composition Download PDF

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CN100444731C
CN100444731C CNB2007100252360A CN200710025236A CN100444731C CN 100444731 C CN100444731 C CN 100444731C CN B2007100252360 A CNB2007100252360 A CN B2007100252360A CN 200710025236 A CN200710025236 A CN 200710025236A CN 100444731 C CN100444731 C CN 100444731C
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difenoconazole
methyl
agent
water
composition
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CN101084752A (en
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谢平
李文明
汪贵艳
杨耀武
汪志稳
刘成社
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Anhui Huaxing Chemical Co Ltd
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Abstract

A bactericide composition comprises difenoconazole (A) and at least one bactericide (B) selected from 1-(4-chlorophenoxy)-3, 3-dimethyl-1-(1H-1, 2, 4-triazole-1-methyl)-2-butanone, 1-(4-chlorophenoxy)-3, 3-dimethyl-1-(1H-1, 2, 4triazole-1methyl)butyl-2-alcohol, bi-(4-fluorophenyl)methyl(1H-1, 2, 4-triazole-1-kya methylene)silicane, and 2-(4-chlorphenyl)-2-(1H, 1, 2, 4-triazole-1-methyl) capronitrile. The composition can be used for preventing and treating rice sheath blight disease and wheat powdery mildew.

Description

Microbicide compositions
Technical field
The present invention relates to a kind of microbicide compositions and uses thereof, especially a kind of preparation of compositions and application with Difenoconazole and some systemic fungicide.
Background technology
(difenoconazole) is suitable for Difenoconazole, and be anti--3-chloro-4-[4-methyl-2-(1H-1,2,4-triazole-1 ylmethyl)-1,3-dioxolane-2-yl] phenyl-4-chlorphenyl ether
Figure C20071002523600031
Be that a kind is efficient, wide spectrum, new type bactericide, mainly use cereal crop, paddy rice, wheat, barley, cotton, soybean, fruit tree, various crop such as vegetables, control is because of imperfect fungus, sac fungi, fungus-caused multiple diseases such as basidiomycetes, if tree, the scab of vegetables, leaf spot, powdery mildew, rust, rice sheath blight disease, rice kernel smut, sheath is rotten sick, false smut, the short bunt of wheat, bunt, dust-brand looses, glume blight, root rot, banded sclerotial blight, full rot, early stage rust, powdery mildew, stinking smut of barley, loose kernel smut, stripe disease, net blotch, full rot, soybean, cotton seedling blight, root rot etc. all have preventive effect preferably.Difenoconazole not only has the bactericidal activity of wide spectrum, also a lot of pathogens is had lasting protection and therapeutic activity simultaneously.Be one of national agricultural [technology center project verification recommended variety.But the difenoconazole technical material domestic production is less, and price is high, is difficult to prevent and treat in the farmland aspect the disease large tracts of land and generally applies.And if the long-term single use of a kind of medicine all produces resistance inevitably, bactericide is all the more so.Therefore, by composite channel, employing Difenoconazole and other bactericide are that the bactericidal composition of primary activity composition will be an effective way of resisting resistance, delaying drug resistance development.
The inventor's result of study has confirmed The above results, through a large amount of research and tests, filtered out with Difenoconazole and can reach synergy after composite, doublely control, resist pesticide resistance, delay pesticide resistance, reduce triazolone, Triadimenol, nitrile bacterium azoles, the Flusilazole of purpose such as Difenoconazole consumption, and the combination of these bactericide made various formulation products, thereby the present invention is proposed.
Summary of the invention
The purpose of this invention is to provide a kind of bactericidal composition that contains Difenoconazole and at least a systemic fungicide compound as active component,, improve bactericidal activity, enlarge fungicidal spectrum by composite, and reduce Difenoconazole consumption, reduce cost; With the combination of this active ingredient, be equipped with proper assistant, thinner etc. and make operable formulation product and uses thereof.The largest benefit of said composition is to advance coordinate plant growth sterilization same, when plant is ripe, reaches sterilization effects and facilitates for the farmland mechanized operation.
The objective of the invention is to realize by following measures;
A kind of bactericidal composition comprises Difenoconazole (A) and at least a (B) bactericide as active component, and its two weight ratio is 1: 50-50: 1.
The B bactericide that is specially adapted to composition of the present invention is as follows:
1. the chemical name of triazolone (triadimefon) is 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)-2-butanone;
2. the chemical name of Triadimenol (triadimenol) is 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4 triazoles-1 base) butyl-2-alcohol;
3. the chemical name of Flusilazole (flusilazole) is two (4-fluorophenyl) methyl (1H-1,2, the support of 4-triazol-1-yl methylene) silane;
4. the chemical name of nitrile bacterium azoles (myclobutani) is the own nitrile of 2-(4-chlorphenyl)-2-(1H, 1,2,4-triazole-1-methyl);
Above-mentioned active component all is bactericide well known in the art, can buy by various commercial channel.
Separately amount of application and both portfolio ratios and synergy degree when the consumption of the active component of using depends on independent use in the bactericidal composition of the present invention, simultaneously also relevant with the target bacterial classification.The weight ratio of Difenoconazole and systemic fungicide is 1 generally speaking: 50-50: 1, but preferred proportion is 1: 20-20: 1.
Also can comprise carrier and/or thinner in the bactericidal composition of the present invention, the 0.5%-95% that its existing active component weight is gross weight.Present composition carrier and/or thinner can be any addible components, active component and carrier and/or thinner are mixed with each application target final products, as the preparation of missible oil, soluble liquid, aqueous emulsion, microemulsion, suspending agent, suspended emulsion, the agent of kind clothing, wetting powder, water dispersible granules, dry suspending agent, granule or other formulations.
The present invention also comprises the method for preparing above-mentioned microbicide compositions, and it comprises active component is mixed mutually with at least a carrier and/or thinner.Carrier and thinner refer to filler, solvent, surfactant etc.Also can add other functional aids such as antifreeze, thickener, stabilizing agent, defoamer, disintegrant in case of necessity.
Described carrier, filler are white carbon, precipitated calcium carbonate, potter's clay, attapulgite, kaolin, diatomite, swollen ravine soil, sepiolite, zeolite, river sand, quartz sand, talcum powder, can use separately, also can two kinds or above mixing use.
Described stabilizing agent has BHT, triphenyl phosphite, epoxychloropropane, tributyl phosphate, triethanolamine, diethanol amine, monoethanolamine, can use separately, also can mix use.
Described solvent, cosolvent are toluene, dimethylbenzene, chlorobenzene, solvent naphtha, alpha-methyl-naphthalene, turpentine oil, carrene, chloroform, methyl alcohol, ethanol, isopropyl alcohol, butanols, isoamyl alcohol, cyclohexanone, isophorone, acetophenone, ethyl acetate, butyl acetate, N.N-dimethyl formamide, dimethyl sulfoxide (DMSO), methyl cellosolve, ethyl cellosolve etc., and the use of the mixing between the different solvents is regular.
Described antifreeze is ethylene glycol, glycerine, propane diols, urea, glycerine, ether diglycol, diglycol, polyethylene glycol, isopropyl alcohol etc.
Surfactant can be emulsifier, dispersant, wetting agent or bleeding agent.Surfactant can be nonionic with ionic, also can be two or more compound uses.Described emulsifier is alkylphenol-polyethenoxy (polyoxypropylene) ether, benzylphenol APEO, phenethyl phenol polyethenoxy ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene carboxylate, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, alkylphenol polyoxyethylene formaldehyde condensation products, and the phosphate of these compounds, alkyl benzene sulphonate (sodium salt or calcium salt) or directly use commercially available emulsifier monomer and composite product.The newborn 500# series of concrete example such as farming, 600# series, 1600# series, NP series, OP series, AEO series, 700#, 400# series and composite kind 2201,0203B, 2021B, 4103 etc., these all are emulsifier productions well known in the art, and market is on sale.
Described dispersant; wetting agent; bleeding agent is lignosulfonates (sodium salt or calcium salts); Negel; condensation compound of methyl naphthalene sulfonic acid and formaldehyde sulphate; naphthalene sulfonic acid-formaldehyde condensation product; methanonaphthalene sodium sulfonate dibutyl naphthalene sulfonic acid-formaldehyde condensation product; N-methyl fatty acyl group sodium taurocholate; alkylphenol polyoxyethylene formaldehyde condensation products sulphate; polymerization of carboxylic acid sodium; the alkylphenol polyoxyethylene phosphate; the withered powder of tea; saponin; lignosulfite; aliphatic alcohol sulfate; lauryl sodium sulfate; alkylbenzenesulfonate; penetrant t; bleeding agent OT; fatty acid amide-N methyl taurine sodium salt; sodium sulfate of polyethenoxy ether of fatty alcohol; draw back powder; JFC; can use separately, also can compoundly use.Above-mentioned surfactant all is materials well known in the art, can obtain by various commercial channel.
Described thickener has gum Arabic, CMC, xanthans, Magnesiumaluminumsilicate, hydroxyethylcellulose, polyvinyl alcohol, PAA, bentonite, silicic acid, can use separately, also can two or more mixing use.
Described disintegrant has sodium alginate, sodium carboxymethyl starch, ammonium sulfate, bentonite, urea, calcium chloride.
Described defoamer has bubble enemy, silicone, C 8-10Fatty alcohol, C 10-20Saturated fat acids (as capric acid, stearic acid etc.) and amide-type.
Described binding agent is starch, dextrin, gum Arabic, soybean protein, gelatine, sodium sulphate, gypsum, polyvinyl alcohol, polyethylene glycol, rosin, paraffin wax, CMC, sodium silicate.Can use separately, also can two or morely use with.
Can contain toner in the preparation, inorganic pigment iron oxide for example, titanium oxide or Prussia orchid; Organic dyestuff is as A Lizhalin, azo dyes, metal phthalocyanine or kiton colors.In water-base preparation, for preventing moldy metamorphism, need add a certain amount of preservative of people, described preservative has Sodium Benzoate, polyformaldehyde, sorbitol, formalin, citric acid, to yl benzoic acid methyl esters, O-SyL sodium, 1,2-benzisothiazole-3-ketone (code name BIT) etc.
According to the preparation type difference, the weight percentage of active constituent is distinguished to some extent: in missible oil, soluble liquid, microemulsion, aqueous emulsion, suspension emulsion, the agent of kind clothing, active constituent accounts for 5-50%, and preferable content is 5-40%; Active constituent accounts for 5-90% in wettable powder granula, water dispersible granules, the dried suspension emulsion, is preferably 10-80%.In addition, also composition of the present invention can be made the granule or the seed dressing of direct use.
The present composition can be used by commonsense method, as adds water spray and make cauline leaf and handle, but also root is executed, and can also dress seed and seed pelleting uses.Amount of application of the present invention changes with weather condition and crop state, can prevent and treat purpose by using suitable formulation to reach.
Embodiment
The present invention is elaborated with following specific embodiment, but the present invention only limits to these examples absolutely not.Percentage all is weight percentage in all prescriptions.The processing technology of the various preparations of the present composition and equipment are known.
Missible oil preparation: press formula rate, with the solubilization of active ingredient of capacity in solvent, adding surfactant (using after the heating for dissolving in case of necessity) and other components, mixing is transparency liquid.Process equipment mainly is to mix still, can adopt enamel reaction still, stainless steel stirred tank etc.
The processing of microemulsion, aqueous emulsion: press formula rate, solubilization of active ingredient in solvent and cosolvent, is added surfactant, mix and make oil phase.With water-soluble component and water mixed water, again oil phase is added aqueous phase or water is added in the oil phase, the limit edged stirs, and makes microemulsion or aqueous emulsion.According to the kind difference, water only is a water sometimes, does not need special preparation.Process equipment mainly is to mix still, during the preparation aqueous emulsion, must adopt even matter mixer to carry out water, oil phase mixing, and oil phase can be prepared with enamel reaction still.The available even matter mixer of the preparation of microemulsion, also available other stirring mixers.
The processing of suspending agent, suspended emulsion: press formula rate, with the pesticide activity component of capacity, surfactant, after thickener, film forming agent, carrier or filler and part water mix, through high speed shear, the wet method sand milling, semi-finished product, add water after the analysis and mix to filter and get product.The production technology of suspended emulsion according to the kind difference, can directly adopt this method, also the former medicine of solid can be made suspending agent, and the former medicine of liquid is made decomposite technology behind the aqueous emulsion.Capital equipment is batching still, colloid mill or even matter mixer, sand mill.
Wetting powder processing: pesticide activity component, auxiliary agent, filler are mixed the mixed again wetting powder that gets after airslide disintegrating mill is pulverized in proportion.
The processing of water-dispersible granules: pesticide activity component, auxiliary agent and filler are mixed in proportion; through comminution by gas stream; the water that adds 15-20% then; make the water dispersible granules product through kneading, granulation, drying, screening, maybe the powder that will pulverize water spray, granulation, dry in the fluidized granulating machine goes on foot successfully.Go out sieve behind the machine the water dispersible granules product.Capital equipment: mixer, airslide disintegrating mill, kneader, Squeezinggranulator.Drying equipment (can be drying room, fluid-bed drying), or fluidized granulating machine, screening machine.
The processing of dry suspending agent: after pesticide activity component, auxiliary agent, filler mixed by proportioning, carry out the slurry that the wet method sand milling obtains,, make and do outstanding agent through mist projection granulating.Capital equipment also needs autoclave pressure, sponging granulator and cleaner except that the suspending agent process equipment.
Formulation Example 1 (missible oil), Difenoconazole 5.5%, Triadimenol 0.5%;
Formulation Example 2 (microemulsion), Difenoconazole 6%, Flusilazole 6%;
Formulation Example 3 (aqueous emulsion), Difenoconazole 2%, triazolone 10%;
Formulation Example 4 (suspending agent), Difenoconazole 25%, nitrile bacterium azoles 5%;
Formulation Example 5 (suspending agent), Difenoconazole 8%, Flusilazole 2%;
Formulation Example 6 (wetting powder), Difenoconazole 8%, Triadimenol 2%.
The composition of Difenoconazole and triazolone, Triadimenol, Flusilazole, nitrile bacterium azoles is as follows to the toxicity test method and the effect of Rhizoctonia solani Kuhn:
Rhizoctonia solani Kuhn is a separation and Culture 72 hours on the paddy rice diseased plant of gathering from the field, gets a certain amount of medicament, prepares the mother liquor of each medicament with acetone by the active ingredient of medicament, is diluted to the respective concentration soup with sterile water then and is prepared into medium.Then Rhizoctonia solani Kuhn is inoculated on the medium that contains soup, other is provided with a contrast, is placed in the insulating box to cultivate 72 hours.
Mycelial growth inhibition rate (%)=(contrast colony diameter-processing colony diameter)/(contrast colony diameter-bacterium cake diameter) * 100
Each is handled mycelial growth inhibition rate according to medicament, calculate each medicament EC50, calculate the toxicity index of medicament and the co-toxicity coefficient of using with (CTC) according to the abundant method of Sun Yun again, the CTC value is synergistic effect greater than 100, equaling 100 and be addition, is antagonism less than 100.
Table 1, composition are to rice sheath blight disease co-toxicity coefficient measurement result
Medicament Inhibiting rate % (0.05mg/ml) EC 50(mg/L) Co-toxicity coefficient CTC
Difenoconazole 82.9 0.0045 /
Triazolone 90.5 0.0039 /
Triadimenol 91.5 0.0041 /
Flusilazole 91.7 0.0052 /
Nitrile bacterium azoles 90 0.0059
The Difenoconazole triazolone 94.2 0.0029 267.24
The Difenoconazole Triadimenol 92.4 0.0030 232.74
The Difenoconazole Flusilazole 91.8 0.0038 220.65
Difenoconazole nitrile bacterium azoles 90.8 0.0041 187.56
The composition of Difenoconazole and triazolone, Triadimenol, Flusilazole, nitrile bacterium azoles all shows certain inhibition effect and synergistic effect preferably to Rhizoctonia solani Kuhn.
Embodiment 7,
The preparation of Formulation Example 1 and Difenoconazole missible oil and triazolone missible oil are done the test of control rice sheath blight disease controlling.
Trial crops: paddy rice China excellent 86
Use the phase: paddy rice booting stage
The test region is divided into four sub-districts, respectively at paddy rice spray water after booting stage, 20% Difenoconazole EC, 20% triazolone EC and 20% Difenoconazole+triazolone EC, two parallel lines great-jump-forward sampling methods are adopted in the laggard line sampling investigation of two weeks, and each sub-district is all spot-check 200 clumps.Check weighing is carried out to every cell production in the harvesting back, and spike of rice is carried out the medicament residue analysis.
Test data such as following table:
Medicament Morbidity strain number Incidence of disease % Volume increase (kilogram)
Blank 192 96 0
Difenoconazole EC 106 53 31
Triazolone EC 126 63 20
Difenoconazole+triazolone EC 47 23.5 60
The result shows that Difenoconazole+triazolone has higher preventive effect to rice sheath blight disease, than its single agent height, and also to rice safety, noresidue, to the increasing production of rice effect also clearly.
Embodiment 8,
The control that control wheat powdery mildew, rust are done in preparation and Difenoconazole, the agent of Triadimenol list of Formulation Example 6 is tested.
Trial crops: wheat
Use the phase: wheat seedling is neat
The test region is divided into four sub-districts, respectively at the neat back of wheat seedling water spray, 10% Difenoconazole WP, 15% Triadimenol WP and 10% Difenoconazole+Triadimenol WP, disease tassel yield is respectively handled in investigation before the wheat maturation, adopts two parallel lines great-jump-forward sampling methods, each sub-district is all spot-check 200 clumps, calculates preventive effect.Check weighing is carried out to every cell production in wheat harvesting back, is reference with the blank district.And the wheat head carried out the medicament residue analysis, the result shows that Difenoconazole+Triadimenol is to wheat safety, noresidue.
Test data such as following table:
Medicament Morbidity strain number Average preventive effect % Volume increase (kilogram)
Blank 100 0 0
Difenoconazole 10%WP 42 79 30
Triadimenol 15%WP 60 70 23
Difenoconazole+Triadimenol 10%WP 22 89 57
Embodiment 9, the preparation of Formulation Example 5 and Difenoconazole, the agent of Flusilazole list are done the control test that prevents and treats pear scab.
Control crop: pears (kind is the susceptible variety pear)
Crop target: scab (Venturia nashicola)
Environmental condition: test site is positioned at Xinji City, Hebei province, and the test orchard age of tree 13 years, pear scab take place throughout the year and fall ill heavylier, and physical features is smooth, and soil property is a sandy loam, and water and fertilizer condition is better, 3 meters of spacing in the rows, 6 meters of line-spacings.The cultivation condition uniformity, the Pass Test requirement.In pear scab premorbid first time medicine for the first time.Adopting high pressure power driven sprayer spray medicine, is blank with the clear water.Dosage is 12.5L/ strain tree, even spraying.
Disease index value and field efficacy such as following table:
Show that through field control effectiveness test kresoxim-methyl and triazole bactericidal agent Flusilazole are composite to have preventive effect preferably to pear scab.
Figure C20071002523600131

Claims (3)

1, a kind of bactericidal composition, it is characterized in that active ingredient is Difenoconazole (A) and a kind of following (B) bactericide: 1-(4-chlorophenoxy)-3 that is selected from, 3-dimethyl-1-(1H-1,2, the 4-triazol-1-yl)-2-butanone, 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4 triazoles-1 base) butyl-2-alcohol, two (4-fluorophenyl) methyl (1H-1,2, the support of 4-triazol-1-yl methylene) silane, 2-(4-chlorphenyl)-2-(1H, 1,2,4-triazole-1-methyl) own nitrile, A and B weight ratio are 1: 50-50: 1.
2, bactericidal composition according to claim 1 is characterized in that A and B weight ratio are 1: 20-20: 1.
3, composition according to claim 1 and 2 is characterized in that containing carrier and/or thinner.
CNB2007100252360A 2007-07-19 2007-07-19 Germicide composition Active CN100444731C (en)

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Publication number Priority date Publication date Assignee Title
CN101647452A (en) * 2009-08-06 2010-02-17 陕西先农生物科技有限公司 45% hexaconazole-carbendazim suspension concentrate
CN102428931B (en) * 2011-12-23 2013-09-18 江阴苏利化学股份有限公司 Bacteriocidal composition containing Boscalid and triazole bactericide
CN102659468A (en) * 2012-04-23 2012-09-12 赵国彬 Bactericide containing triazoles
CN103141348A (en) * 2013-03-06 2013-06-12 赵伟 Protection and yield increase management method of wheat leaves at later stage
CN103548835B (en) * 2013-09-27 2015-04-29 中国农业大学 SYP-1620-difenoconazole blended reagent for prevention and treatment of Ustilaginoidea virens
CN103503880B (en) * 2013-09-27 2015-07-08 中国农业大学 Triadimenol and difenoconazole mixed medicament for preventing ustilaginoidea virens
CN107593755B (en) * 2017-09-01 2020-05-19 中国热带农业科学院环境与植物保护研究所 Preparation method of aqueous emulsion
CN107668040A (en) * 2017-09-01 2018-02-09 中国热带农业科学院环境与植物保护研究所 One kind sterilization sustained-release micro-spheres and preparation method thereof
CN107593699A (en) * 2017-09-01 2018-01-19 中国热带农业科学院环境与植物保护研究所 A kind of sustained-release micro-spheres for being used to sterilize and preparation method thereof
CN107593694B (en) * 2017-09-01 2020-07-24 中国热带农业科学院环境与植物保护研究所 Aqueous emulsion

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