CN104496678A - Compound composition containing methanesulphonyl myclobutanil and leaf fertilizer and preparation - Google Patents
Compound composition containing methanesulphonyl myclobutanil and leaf fertilizer and preparation Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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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
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
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- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B1/00—Superphosphates, i.e. fertilisers produced by reacting rock or bone phosphates with sulfuric or phosphoric acid in such amounts and concentrations as to yield solid products directly
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- C05C1/00—Ammonium nitrate fertilisers
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- C05C11/00—Other nitrogenous fertilisers
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- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
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- C05C5/00—Fertilisers containing other nitrates
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- C05C5/04—Fertilisers containing other nitrates containing calcium nitrate
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- C05C9/00—Fertilisers containing urea or urea compounds
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- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
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- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
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- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
- C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D271/00—Heterocyclic compounds containing five-membered rings having two nitrogen atoms and one oxygen atom as the only ring hetero atoms
- C07D271/02—Heterocyclic compounds containing five-membered rings having two nitrogen atoms and one oxygen atom as the only ring hetero atoms not condensed with other rings
- C07D271/10—1,3,4-Oxadiazoles; Hydrogenated 1,3,4-oxadiazoles
- C07D271/113—1,3,4-Oxadiazoles; Hydrogenated 1,3,4-oxadiazoles with oxygen, sulfur or nitrogen atoms, directly attached to ring carbon atoms, the nitrogen atoms not forming part of a nitro radical
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Abstract
The invention discloses a compound composition containing methanesulphonyl myclobutanil and a leaf fertilizer and a preparation. The compound composition comprises two active ingredients A and B, wherein A is the methanesulphonyl myclobutanil with the chemical name of 2-(p-fluorophenyl)-5-methylsulfonyl-1,3,4-oxadiazole; B is the leaf fertilizer which is humic acid, chitin, amino acid or alginic acid; preferably, the weight ratio of A to B is (100:0.01)-(0.01:100); the compound composition accounts for 0.1-90wt% of a bactericide. The compound composition and the bactericide have a remarkable synergetic interaction effect in comparison with single dosage and are capable of effectively controlling various crop bacterial diseases, promoting the plants to grow healthily and strongly, decreasing the medicament dosage, reducing the cost, delaying the drug resistance, improving the quality, keeping the output and increasing the output.
Description
Technical field
The present invention relates to technical field of pesticide, particularly relate to a kind of complex composition and the preparation that contain methylsulfonyl bacterium azoles and foliage fertilizer.
Background technology
Chemical agent is the important means of control bacterial disease, at present still based on chemical prevention, but at present for preventing and treating medicament mainly copper agent class and the antibiotics of bacterial disease, product category is few, update slow, and plantation family continuous several times uses similar medicament in a large number, cause pathogenetic bacteria to produce strong resistance to these medicaments, Guizhou University develops Xin Yao Ji oxadiazole sulfone compound for this reason.Secondly, after plant is caused harm by disease, the growing way of plant is faint.Therefore, we are when controlling disease, add some foliage fertilizers and give plant certain nutritional supplementation, strengthen its physique, improve its resistivity to disease, and strengthen the receptivity of plant to medicament.But during practical application, foliage fertilizer and agricultural chemicals are all arbitrarily now mix existing use, and the irrational medication of this not science, does not only reach synergism, also likely produce antagonistic action.
Guizhou University's independent research also has the new type bactericide " one class preventing and control crop Micobial Disease oxadiazole sulfone compound (patent No. is ZL201110314246.2) " of independent intellectual property rights, and its structural formula is:
The step of preparation process of this compound and condition:
(1) preparation of different replacing acid methyl ester intermediate: with different organic acids and anhydrous methanol for raw material, back flow reaction 6-10 hour under sulphuric acid catalysis, decompression separating methanol, after saturated sodium bicarbonate aqueous solution adjusts ph=7, separatory obtains different methyl-formiates;
(2) preparation of the different formyl hydrazine intermediate replaced: be dissolved in methyl alcohol with different methyl-formiates, then slowly add 40%-80% hydrazine hydrate, till back flow reaction is complete, separates out the formyl hydrazine of different replacement after cooling;
(3) 2-sulfydryl-5-replaces the preparation of-1,3,4-oxadiazole intermediate: with the formyl hydrazine of above-mentioned preparation and KOH, dithiocarbonic anhydride for raw material, ethanol is solvent, and back flow reaction is complete, de-ethanol, adjusts PH=5 to obtain 2-and dredges base-5-and replace-1,3,4-oxadiazole;
(4) 2-thioether-5-replaces-1,3, the preparation of 4-oxadiazole intermediate: replace-1 with above-mentioned 2-sulfydryl-5-, 3,4-oxadiazole is raw material, after hydro-oxidation sodium water dissolution, be obtained by reacting corresponding sulfide compound with 1-2 by the dimethyl sulfate of molar weight (second) ester or halohydrocarbon etc.;
(5) 2-methyl (ethyl) alkylsulfonyl-5-replaces the preparation of-1,3,4-oxadiazole.
With corresponding thioether for raw material, be dissolved in Glacial acetic acid, 2%-7% potassium permanganate solution or 30% hydrogen peroxide oxidation obtain corresponding sulfone compound.
Foliage fertilizer is for the purpose of Foliage Absorption, nutrient needed for crop is directly used the fertilizer on blade face, is called foliage fertilizer.Foliage fertilizer is that nutritive element is applied to farm crop blade surface, is played a kind of fertilizer type of its function by the absorption of blade.Foliage fertilizer mainly contains humic acid, amino acid, Lalgine.
Humic acid (Humic Acids) is a kind of organic acid, it is organic important component part, it mainly comprises Ulmic acids, ulmic acid, xanthohumic acid, is a kind of mixture of complexity, usually calls humic acid except both the Ulmic acids of xanthohumic acid and ulmic acid again.Humic acid complex structure, with various active functional group, can interact with many organism, inorganics.Humic acid also because have various active functional group and larger surface-area, and becomes a kind of environment-friendly type sorbent material.
Chitin, has another name called chitin, chitin, and chemical name is (Isosorbide-5-Nitrae)-2-kharophen DDG.It is extensively present in the shell of marine organisms shrimp crab, is also present in the cell walls of the unicellular lower eukaryote such as marine alga, fungi yeast.
Amino acid is the necessary nutritive substance of plant-growth, to plant-growth particularly photosynthesis there is unique promoter action, especially glycine, it can increase chlorophyll content of plant, improve the activity of enzyme, promote the infiltration of carbonic acid gas, make photosynthesis more vigorous, to raising crop quality, increase content all important roles of Vc and sugar.
First Lalgine was produced in Great Britain Island in 1949 and is come out.It is the new-type fertilizer integrating nutritive ingredient, antibiotics, plant hormone.It is through special biochemical process process, effectively essence substance is extracted from natural seaweed, greatly remain natural radioactivity component, the various mineral element such as K, Ca, Mg, Fe, Zn, I incomparable containing a large amount of non-nitrogen containing organism, terrestrial plant and abundant VITAMIN, be rich in specific Sargassum polysaccharides, alginic acid, highly unsaturated fatty acids and multiple natural phant growth regulator in marine alga especially.
Summary of the invention
Dui Yu oxadiazole sulfone compound, applicant researches and develops further, is selected from the fluorine in halogen atom, R as Rn
2select the methyl of C1-C5 alkyl and get the structural formula of oxadiazole sulfone compound:
Its chemical name is 2-(to fluorophenyl)-5-methylsulfonyl-1,3,4-oxadiazole, is called for short methylsulfonyl bacterium azoles.
The concrete syntheti c route of compound methylsulfonyl bacterium azoles is as follows:
(1) to the synthesis of fluorobenzoyl hydrazine
(2) 2-sulfydryl-5-is to the synthesis of fluorophenyl-1,3,4-oxadiazole
(3) 2-Dimethyl sulfide-5-is to the synthesis of fluorophenyl-1,3,4-oxadiazole
(4) 2-(to fluorophenyl)-5-methylsulfonyl-1,3,4-oxadiazole target compound is prepared
Applicant studies discovery further, and methylsulfonyl bacterium azoles is the control bacterial disease medicament of novel structure, by suppressing the synthesis of pathogenic agent energy, the growth of anti-bacteria and breeding.Methylsulfonyl bacterium azoles has the feature of interior suction, conduction, and after infiltration blade epidermis, energy transporting is to other positions of same blade.A large amount of isolated tests shows, methylsulfonyl bacterium azoles has good restraining effect to causing the various pathogenetic bacterias of phytobacterial disease, and namely directly anti-bacteria is bred.Through repeatedly pot experiment and field control effectiveness test checking, show that methylsulfonyl bacterium azoles all has good prevention effect to crop bacterial disease, especially good control effect is all had to bacterial blight of rice, slice disease, tobacco bacterial wilt, bacterial wilt of tomato, citrus bacterial canker disease etc., and plant growth can be stimulated to a certain extent healthy and strong, improve the resistibility of crop.This compound has efficiently, the feature of wide spectrum, use safety, is a sterilant having much exploitation potential quality.
Find through test, methylsulfonyl bacterium azoles and foliage fertilizer rational mixture control corps diseases effect very outstanding.
In view of this, for the deficiency that prior art exists, the object of the invention is to provide a kind of complex composition and the preparation thereof that contain methylsulfonyl bacterium azoles and foliage fertilizer, this complex composition and preparation thereof have obvious synergism relative to single dose, improve fungicidal activity, Promoting plant growth is healthy and strong, strengthens via plant immunity, improve crop quality, protect and produce volume increase.
In order to realize object of the present invention, the technical scheme of employing is:
The invention provides a kind of complex composition containing methylsulfonyl bacterium azoles and foliage fertilizer, described complex composition contains two kinds of active components A and B, and described A is methylsulfonyl bacterium azoles, its chemical name is 2-(to fluorophenyl)-5-methylsulfonyl-1,3,4-oxadiazole, B is foliage fertilizer; Described foliage fertilizer is any in humic acid, chitin, amino acid, Lalgine.
The above-described complex composition containing methylsulfonyl bacterium azoles and foliage fertilizer, the weight ratio of described active components A and activeconstituents B is 100:0.01 to 0.01:100.
The above-described complex composition containing methylsulfonyl bacterium azoles and foliage fertilizer, the weight ratio of described active components A and activeconstituents B is 100:1 to 1:100.
The above-described complex composition containing methylsulfonyl bacterium azoles and foliage fertilizer, the weight ratio of described active components A and activeconstituents B is 50:1 to 1:50.
The present invention also provides a kind of preparation containing methylsulfonyl bacterium azoles and foliage fertilizer, comprises acceptable auxiliary material on above arbitrary described complex composition and agricultural chemicals, is then prepared into disinfectant use in agriculture.
The above-described preparation containing methylsulfonyl bacterium azoles and foliage fertilizer, by weight, the weight percentage that described complex composition accounts for described disinfectant use in agriculture is 0.1%-90%.
The above-described preparation containing methylsulfonyl bacterium azoles and foliage fertilizer, by weight, the weight percentage that described complex composition accounts for described disinfectant use in agriculture is 1%-60%.
Arbitrary described preparation containing methylsulfonyl bacterium azoles and foliage fertilizer above, on described agricultural chemicals, acceptable auxiliary material is the mixture of a kind of and auxiliary agent in solvent and filler.
Above-described humic acid is xanthohumic acid.
Described amino acid is one or more in Threonine, aspartic acid, tyrosine, phenylalanine, Serine, Methionin, L-glutamic acid, proline(Pro), glycine, arginine, L-Ala, Histidine, Gelucystine, Isoleucine, α-amino-isovaleric acid, leucine, methionine(Met).
Auxiliary agent of the present invention comprises emulsifying agent, wetting agent, dispersion agent.Add other conventional functionality auxiliary agents such as antifreezing agent, thickening material, stablizer, defoamer, disintegrating agent if desired.
Emulsifying agent is calcium dodecylbenzene sulphonate, thermally coupled distillation columns, alkylaryl polyoxyethylene polyoxypropylene ether.
Dispersion agent is naphthalene sulfonic acidformaldehyde condensation product, naphthalene sulfonic acid formaldehyde polymer sodium salt (hereinafter referred to as NNO), sodium methylene bis-naphthalene sulfonate, calcium lignin sulphonate, succinate sodium sulfonate, sodium laurylsulfate, sodium lignosulfonate, alkylphenol polyoxyethylene formaldehyde condensation products vitriol, pull open in powder, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acidformaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, aliphatic amine polyoxyethylene ether one or more.
Wetting agent is sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, calcium dodecylbenzene sulphonate, pull open in powder copper rosinate X, sulfonated alkyl naphathalene, polyoxyethylene tri-styryl phosphenylic acid salt, alkylbenzene sulfonate, wetting and penetrating agent F, wetting agent T, spaonin powder, the withered powder of tea, silkworm excrement and Seed of Chinese Soapberry powder one or more.
Disintegrating agent is one or more in urea, volatile salt, aluminum chloride.
Solvent is water, soybean oil, pimelinketone, Witconol 2301, methylnaphthalene, N-Methyl pyrrolidone.
Solid carrier is clay, polynite, silicon-dioxide, diatomite, terra alba, kaolin, attapulgite, talcum powder, light calcium carbonate, aluminum oxide, urea, river sand, nitrogenous fertilizer, phosphate fertilizer, potash fertilizer, moderate-element fertilizer, trace element fertilizer.
Wherein nitrogenous fertilizer is selected from urea, volatile salt, one or more in ammonium nitrate and ammonium phosphate, phosphate fertilizer is selected from calcium superphosphate, monoammonium phosphate, one or more in diammonium phosphate and fused(calcium magnesium)phosphate, potash fertilizer is preferably from potassium sulfate and potassium primary phosphate, moderate-element fertilizer is selected from nitrocalcite, calcium chloride, one or more in magnesium sulfate and magnesium nitrate, trace element fertilizer is selected from zinc sulfate, zinc nitrate, EDTA zinc, boric acid, eight Sodium Tetraboratees, potassium tetraborate, manganous sulfate, manganous nitrate, EDTA manganese, cupric nitrate, ferric sulfate, NaFeEDTA, one or more in ammonium molybdate and Sodium orthomolybdate.These fertilizer components also have disintegration at solid preparation.
Complex composition provided by the invention, after adding auxiliary agent, solvent or filler, the preparation of wettable powder, suspension agent, microemulsion, aqueous emulsion, water dispersible granules, granule, seed coat agent, soluble powder, soluble liquid, suspended emulsion agent, dry suspension, ultra low volume liquids or other formulation can be mixed with.
In embodiments more provided by the invention, the formulation of described sterilant is wettable powder, aqueous emulsion, water dispersible granules, suspended emulsion agent.
Sterilant of the present invention can be used by usual way, as spraying cauline leaf process, also can soil treatment, and such as solid root spreads fertilizer over the fields or liquid fills with root, can also dress seed, to soak seed or seed pelleting uses.
Above-mentioned complex composition can be used for control crop bacterial disease.
Described bacterial disease can be spotted type Micobial Disease, leaf withered type Micobial Disease, blue or green withered type Micobial Disease, withered type Micobial Disease, ulcer type Micobial Disease, type Micobial Disease of rotting or deformity Micobial Disease.
Above-mentioned spotted type Micobial Disease is paddy bacterial brown spot, bacterial leaf streak of rice, cucumber bacterial angular leaf spot, cotton bacterial angular leaf spot, tomato macula disease, Chinese cabbage leaf spot, watermelon bacterial angular leaf spot, cucumber bacterial angular leaf spot, pepper bacterial leaf spot, Chinese cabbage bacterial angular leaf spot, mango bacterial black spot, common bacterial blight of bean or corn bacterial leaf blight;
The withered type Micobial Disease of above-mentioned leaf is bacterial blight of rice, cucumber Bacterial Leaf Blight, konjaku Bacterial Leaf Blight or Folium Cucumidis sativi rot;
The withered type Micobial Disease of above-mentioned green grass or young crops is tobacco bacterial wilt, bacterial wilt of tomato, potato bacterial wilt, leather certain kind of berries bacterial wilt, pepper ralstonia solanacearum or eggplant bacterial wilt;
Above-mentioned withered type Micobial Disease is potato wilt;
Above-mentioned ulcer type Micobial Disease is citrus ulcer, bacterial pustule of soybean, canker of tomato, tomato shot hole, bacterial speck or bacterial spot of pepper;
Above-mentioned rotten type Micobial Disease is the bacterial soft rot of Solanaceae and ground family crop, paddy rice basal stem rot, soft rot of cabbage, capsicum soft rot, wild cabbage soft rot, cabbage black rot, bacterial ring rot o potato or bacterial soft rot of potato.
In embodiments more provided by the invention, described complex composition can be used for high-efficiency prevention and control cucumber bacterial angular leaf spot, citrus bacterial canker disease, paddy bacterial angular leaf spot, bacterial wilt of tomato.
Complex composition of the present invention and sterilant thereof have the following advantages relative to prior art tool:
Complex composition of the present invention and sterilant thereof have obvious synergism relative to single dose, improve protection effect, can also promote that plant growth is healthy and strong, improve crop immunizing power, reach the object of protecting and producing volume increase oil recovery enhancement.
Embodiment
Below by embodiment, the present invention is further elaborated.It should be noted that, the embodiment of the present invention is only used for the present invention is described, instead of limitation of the present invention.The former medicine of methylsulfonyl bacterium azoles used in the present invention is provided by Guizhou University, and other former medicines used and preparation are commercial.
Embodiment prepared by preparation:
Application Example one
The preparation technology of wettable powder: by methylsulfonyl bacterium azoles, foliage fertilizer, dispersion agent, wetting agent, filler mixing, mix in mixed cylinder, remix is even after micronizer mill is pulverized, and can obtain the wettable powder of sterilant of the present invention.
Embodiment 1 50.005% methylsulfonyl bacterium azoles humic acid wettable powder
Methylsulfonyl bacterium azoles 50g, humic acid 0.005g, sodium methylene bis-naphthalene sulfonate 3g, sodium lauryl sulphate 2.5g, kaolin supplies 100g.
Contrast medicament 1 20% methylsulfonyl bacterium azoles wettable powder
Methylsulfonyl bacterium azoles 20g, sodium methylene bis-naphthalene sulfonate 3g, sodium lauryl sulphate 2.5g, kaolin supplies 100g.
Embodiment 2 10.1% methylsulfonyl bacterium azoles humic acid wettable powder
Methylsulfonyl bacterium azoles 10g, humic acid 0.1g, sodium lignosulfonate 5g, calcium dodecylbenzene sulphonate 2g, ammonium nitrate 4g, silicon-dioxide supplies 100g.
Embodiment 3 80% methylsulfonyl bacterium azoles humic acid wettable powder
Methylsulfonyl bacterium azoles 70g, humic acid 10g, calcium lignin sulphonate 6g, calcium dodecylbenzene sulphonate 1g, ammonium phosphate 3g, clay supplies 100g.
Embodiment 4 1% methylsulfonyl bacterium azoles humic acid wettable powder
Methylsulfonyl bacterium azoles 0.5g, humic acid 0.5g, alkylphenol polyoxyethylene formaldehyde condensation products vitriol 5g, wetting agent T 2g, diatomite supplies 100g.
Embodiment 5 20.2% methylsulfonyl bacterium azoles humic acid wettable powder
Methylsulfonyl bacterium azoles 0.2g, humic acid 20g, NNO 3g, alkylbenzene sulfonate 7g, diammonium phosphate 5g, kaolin supplies 100g.
Contrast medicament 2 10% humic acid wettable powder
Humic acid 10g, alkyl benzene sulfonate calcium salt 3g, alkylbenzene sulfonate 7g, kaolin supplies 100g.
Embodiment 6 10.001% methylsulfonyl bacterium azoles humic acid wettable powder
Methylsulfonyl bacterium azoles 0.001g, humic acid 10g, naphthalene sulfonic acidformaldehyde condensation product sodium salt 4g, the withered powder 6g of tea, 100g supplied by terra alba.
Embodiment 7 30.003% methylsulfonyl bacterium azoles amino acid wettable powder
Methylsulfonyl bacterium azoles 30g, amino acid 0.003g, alkylphenol polyoxyethylene 5.4g, sulfonated alkyl naphathalene 2.6g, 100g supplied by aluminum oxide.
Embodiment 8 20.2% methylsulfonyl bacterium azoles amino acid wettable powder
Methylsulfonyl bacterium azoles 20g, amino acid 0.2g, aliphatic amine polyoxyethylene ether 6g, polyoxyethylene tri-styryl phosphenylic acid salt 2g, manganous nitrate 5g, kaolin supplies 100g.
Embodiment 9 80% methylsulfonyl bacterium azoles amino acid wettable powder
Methylsulfonyl bacterium azoles 60g, amino acid 20g, polyoxyethylene carboxylate 6g, sulfonated alkyl naphathalene 3g, light calcium carbonate supplies 100g
Embodiment 10 1% methylsulfonyl bacterium azoles amino acid wettable powder
Methylsulfonyl bacterium azoles 0.5g, amino acid 0.5g, ester Soxylat A 25-7 5g, sodium lauryl sulphate 3g, magnesium nitrate 6g, 100g is supplied in polynite
Embodiment 11 30.3% methylsulfonyl bacterium azoles amino acid wettable powder
Methylsulfonyl bacterium azoles 0.3g, amino acid 30g, polyoxyethylene carboxylate 4g, Seed of Chinese Soapberry powder 4g, cupric nitrate 5g, light calcium carbonate supplies 100g
Embodiment 12 20.002% methylsulfonyl bacterium azoles amino acid wettable powder
Methylsulfonyl bacterium azoles 0.002g, amino acid 20g, calcium lignin sulphonate 7g, spaonin powder 2g, nitrocalcite 2g, clay supplies 100g
Embodiment 13 40.004% methylsulfonyl bacterium azoles Lalgine wettable powder
Methylsulfonyl bacterium azoles 40g, Lalgine 0.004g, succinate sodium sulfonate 4g, alkylbenzene sulfonate 5g, kaolin supplies 100g
Embodiment 14 50.5% methylsulfonyl bacterium azoles Lalgine wettable powder
Methylsulfonyl bacterium azoles 50g, Lalgine 0.5g, sodium laurylsulfate 6g, the withered powder 5g of tea, ammonium molybdate 8g, light calcium carbonate supplies 100g
Embodiment 15 90% methylsulfonyl bacterium azoles Lalgine wettable powder
Methylsulfonyl bacterium azoles 50g, Lalgine 40g, calcium lignin sulphonate 2g, silkworm excrement 6g, zinc nitrate 1g, clay supplies 100g
Embodiment 16 1% methylsulfonyl bacterium azoles Lalgine wettable powder
Methylsulfonyl bacterium azoles 0.5g, Lalgine 0.5g, succinate sodium sulfonate 6g, Seed of Chinese Soapberry powder 6g, Sodium orthomolybdate 7g, kaolin supplies 100g
Embodiment 17 10.1% methylsulfonyl bacterium azoles Lalgine wettable powder
Methylsulfonyl bacterium azoles 0.1g, Lalgine 10g, succinate sodium sulfonate 6g, Sodium dodecylbenzene sulfonate 3g, EDTA zinc 4g, attapulgite 5g, kaolin supplies 100g
Contrast medicament 3 10% Lalgine wettable powder
Lalgine 10g, succinate sodium sulfonate 6g, Sodium dodecylbenzene sulfonate 3g, EDTA zinc 4g, attapulgite 5g, kaolin supplies 100g
Embodiment 18 60.006% methylsulfonyl bacterium azoles Lalgine wettable powder
Methylsulfonyl bacterium azoles 0.006g, Lalgine 60g, succinate sodium sulfonate 4g, pull open powder copper rosinate X 4g, potassium tetraborate 4g, 100g is supplied in polynite
Embodiment 19 20.2% methylsulfonyl bacterium azoles chitin wettable powder
Methylsulfonyl bacterium azoles 20g, chitin 0.2g, wetting and penetrating agent F 2g, pull open powder 9g, attapulgite 10g, NaFeEDTA 4g, kaolin supplies 100g
Embodiment 20 51% methylsulfonyl bacterium azoles chitin wettable powder
Methylsulfonyl bacterium azoles 1g, chitin 50g, sodium laurylsulfate 2g, spaonin powder 8g, white carbon black 10g, polynite is supplied 100g and is contrasted medicament 4 10% chitin wettable powder
Chitin 10g, sodium laurylsulfate 2g, spaonin powder 8g, white carbon black 10g, EDTA manganese 5g, 100g is supplied in polynite
Application Example two
The preparation technology of water dispersible granules: methylsulfonyl bacterium azoles, foliage fertilizer, auxiliary agent, disintegrating agent, filler are mixed; pulverize, stir after adding water-wet, then use screw extruder pelletizer granulation; sieve after drying, obtain the water dispersible granules of sterilant of the present invention.
Embodiment 21 51% methylsulfonyl bacterium azoles humic acid water dispersible granules
Methylsulfonyl bacterium azoles 50g, humic acid 1g, pulls open powder 5g, and the withered powder 5g of tea, urea 8g, attapulgite 10g, kaolin supplies 100g.
Embodiment 22 24% methylsulfonyl bacterium azoles amino acid water dispersible granules
Methylsulfonyl bacterium azoles 3g, amino acid 21g, sodium laurylsulfate 3g, spaonin powder 7g, volatile salt 5g, clay supplies 100g.
Embodiment 23 20% methylsulfonyl bacterium azoles Lalgine water dispersible granules
Methylsulfonyl bacterium azoles 10g, X.6g Lalgine 10g, sodium methylene bis-naphthalene sulfonate 3g, pull open powder copper rosinate, aluminum chloride 6.5g, and aluminum oxide 5g, kaolin supplies 100g.
Embodiment 24 30.003% methylsulfonyl bacterium azoles chitin water dispersible granules
Methylsulfonyl bacterium azoles 30g, chitin 0.003g, sodium laurylsulfate 2g, spaonin powder 5g, urea 3g, 100g supplied by talcum powder.
Application Example three
The preparation technology of suspension agent: by frostproofer, thickening material, auxiliary agent, water mixing, mix through high speed shear, add methylsulfonyl bacterium azoles, foliage fertilizer successively, abrading-ball 2 ~ 3 hours in ball crusher, the suspension agent of obtained sterilant of the present invention.
Embodiment 25 14% methylsulfonyl bacterium azoles humic acid suspension agent
Methylsulfonyl bacterium azoles 7g, humic acid 7g, succinate sodium sulfonate 6g, pull open powder copper rosinate X 6g, propylene glycol 5g, polyvinyl alcohol 0.3g, water supplies 100g
Embodiment 26 10.2% methylsulfonyl bacterium azoles amino acid suspension agent
Methylsulfonyl bacterium azoles 10g, amino acid 0.2g, sodium laurylsulfate 2g, pull open powder 7g, and ethylene glycol 3g, xanthan gum 0.2g, water supplies 100g.
Embodiment 27 25.5% methylsulfonyl bacterium azoles Lalgine suspension agent
Methylsulfonyl bacterium azoles 25g, Lalgine 0.5g, pulls open powder 9g, and wetting and penetrating agent F 2g, glycerol 3g, xanthan gum 0.4g, water supplies 100g
Application Example four
The preparation technology of aqueous emulsion: methylsulfonyl bacterium azoles, foliage fertilizer, solvent, emulsifying agent are added together, make to be dissolved into homogeneous oil phase; Water, frostproofer are mixed, becomes homogeneous aqueous phase.Under high velocity agitation, aqueous phase is added oil phase, the aqueous emulsion of obtained sterilant of the present invention.
Embodiment 28 0.1% methylsulfonyl bacterium azoles humic acid aqueous emulsion
Methylsulfonyl bacterium azoles 0.08g, humic acid 0.02g, soybean oil 6g, pimelinketone 5g, alkylaryl polyoxyethylene polyoxypropylene ether 6g, calcium dodecylbenzene sulphonate 3g, ethylene glycol 3g, water supplies 100g
Embodiment 29 7% methylsulfonyl bacterium azoles amino acid aqueous emulsion
Methylsulfonyl bacterium azoles 5g, amino acid 2g, Witconol 2301 8g, pimelinketone 5g, thermally coupled distillation columns 7g, calcium dodecylbenzene sulphonate 3g, glycerol 3g, water supplies 100g
Embodiment 30 3.2% methylsulfonyl bacterium azoles Lalgine aqueous emulsion
Methylsulfonyl bacterium azoles 3g, Lalgine 0.2g, methylnaphthalene 10g, N-Methyl pyrrolidone 5g, 7g, calcium dodecylbenzene sulphonate 3g, glycerol 3g, water supplies 100g
Application Example five
The preparation technology of granule: methylsulfonyl bacterium azoles, foliage fertilizer, auxiliary agent, disintegrating agent, filler are mixed, pulverizes, stirs, then use screw extruder pelletizer granulation, sieve after drying, obtain the granule of sterilant of the present invention after adding water-wet.
Embodiment 31 9% methylsulfonyl bacterium azoles humic acid granule
Methylsulfonyl bacterium azoles 8g, humic acid 1g, sodium methylene bis-naphthalene sulfonate 4g, calcium dodecylbenzene sulphonate 2g, calcium chloride 0.5g, potassium sulfate 5g, urea 10g, river sand supplies 100g.
Embodiment 32 5.1% methylsulfonyl bacterium azoles humic acid granule
Methylsulfonyl bacterium azoles 0.1g, humic acid 5g, sodium methylene bis-naphthalene sulfonate 4g, calcium dodecylbenzene sulphonate 2g, potassium sulfate 5g, urea 10g, 100g supplied by urea.
Embodiment 33 0.4% methylsulfonyl bacterium azoles chitin granule
Methylsulfonyl bacterium azoles 0.3g, chitin 0.1g, sodium lauryl sulphate 3g, NNO 3.5g, fused(calcium magnesium)phosphate 5g, potassium sulfate 2g, 100g supplied by urea
Contrast medicament 5 0.2% methylsulfonyl bacterium azoles granule
Methylsulfonyl bacterium azoles 0.2g, sodium lauryl sulphate 3g, NNO 3.5g, fused(calcium magnesium)phosphate 5g, potassium sulfate 2g, 100g supplied by urea
Embodiment 34 10.1% methylsulfonyl bacterium azoles chitin granule
Methylsulfonyl bacterium azoles 0.1g, chitin 10g, sodium methylene bis-naphthalene sulfonate 2g, NNO 3g, calcium superphosphate 3g, monoammonium phosphate 4g, ferric sulfate 0.3g, potassium sulfate 1g, 100g supplied by urea
Embodiment 35 4.2% methylsulfonyl bacterium azoles chitin granule
Methylsulfonyl bacterium azoles 4g, chitin 0.2g, sodium methylene bis-naphthalene sulfonate 2.5g, NNO 3g, calcium superphosphate 5g, magnesium sulfate 0.6g, eight Sodium Tetraborate 0.4g, river sand supplies 100g
The agent of embodiment 36 0.14% methylsulfonyl bacterium azoles amino acid granular
Methylsulfonyl bacterium azoles 0.04g, amino acid 0.1g, NNO 4g, pulls open powder 2g, calcium superphosphate 5g, zinc sulfate 0.5g, manganous sulfate 0.3g, and potassium primary phosphate 3g, 100g supplied by urea
BIOLOGICAL ACTIVITY EXAMPLES
In order to how whether clear and definite methylsulfonyl bacterium azoles and the composite use of foliage fertilizer have synergism and synergy degree, and field result of use, We conducted Toxicity Determination and field control effectiveness test.
Toxicity Determination:
Following indoor biometrics test adopts the abundant method of Sun Yun to calculate cotoxicity coefficient (CTC) and evaluates mixed effect.
Toxicity index TI (B)=(EC of standard agent A
50the EC of ÷ B agent
50) × 100
Actual toxicity index ATI (AB)=(EC of A
50the EC of ÷ AB
50) × 100
Theoretical toxicity index TTI (AB)=TI (the A) × A percentage ratio+TI (B) in the mixture × percentage ratio of B in mixture
Actual measurement toxicity index (ATI)=(standard agent EC
50÷ reagent agent EC
50) × 100
In theoretical toxicity index (TTI)=A medicament toxicity index × mixture A percentage composition+B medicament toxicity index × mixture in the percentage composition of B
Cotoxicity coefficient (CTC)=[the theoretical toxicity index (TTI) of mixture actual measurement toxicity index (ATI) ÷ mixture] × 100
Judgement criteria is: cotoxicity coefficient >=120 show as synergism; Cotoxicity coefficient≤80 show as antagonistic action; 80< cotoxicity coefficient <120 shows as summation action.
Toxicity Determination embodiment one: (Toxicity Determination of control cucumber bacterial angular leaf spot)
Below that methylsulfonyl bacterium azoles is tested with the Toxicity Determination of humic acid, the composite control cucumber bacterial angular leaf spot of chitin respectively.
Test method: be that 108cfumL-1 pathogenic bacteria adds 0.5mL in each diameter 9cm sterilizing culture dish by bacteria suspension concentration, then pour 15mL into and be cooled in 45 DEG C of gravy peptone substratum, fully mix, solidify.At the equidistant Angle Position of 3 Ge Ju center 2.5cm of culture dish bottom marker equilateral triangle, prevent Oxford cup (high 10mm, internal diameter 6mm), drip the medicament diluent of equivalent different concns, 7d is cultivated under 28 DEG C of constant temperature aseptic conditions, measure antibacterial circle diameter, and calculate mean value, the inhibiting rate of antibacterial circle diameter.Carry out statistical study with DPS data processing software, calculate the EC of each medicament
50, then press the abundant method of Sun Yun and calculate cotoxicity coefficient (CTC).The results are shown in Table 1 ~ table 2.
The Toxicity Determination result of the composite control cucumber bacterial angular leaf spot of xanthohumic acid in table 1 methylsulfonyl bacterium azoles and humic acid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (hereinafter referred to as A) | 7.41 | 100.00 | / | / |
| Xanthohumic acid (hereinafter referred to as B) | 77.23 | 9.59 | / | / |
| A:B＝1000:1 | 6.05 | 122.48 | 99.91 | 122.59 |
| A:B＝750:1 | 5.21 | 142.23 | 99.88 | 142.40 |
| A:B＝500:1 | 5.12 | 144.73 | 99.82 | 144.99 |
| A:B＝250:1 | 5.06 | 146.44 | 99.64 | 146.97 |
| A:B＝100:1 | 4.61 | 160.74 | 99.10 | 162.19 |
| A:B＝50:1 | 4.65 | 159.35 | 98.23 | 162.23 |
| A:B＝20:1 | 4.75 | 156.00 | 95.69 | 163.02 |
| A:B＝8:1 | 4.93 | 150.30 | 89.95 | 167.09 |
| A:B＝3:1 | 5.39 | 137.48 | 77.40 | 177.62 |
| A:B＝1:1 | 7.22 | 102.63 | 54.80 | 187.29 |
| A:B＝1:3 | 12.65 | 58.58 | 32.20 | 181.94 |
| A:B＝1:8 | 21.98 | 33.71 | 19.64 | 171.65 |
| A:B＝1:20 | 31.44 | 23.57 | 13.90 | 169.56 |
| A:B＝1:50 | 39.48 | 18.77 | 11.37 | 165.11 |
| A:B＝1:100 | 43.63 | 16.98 | 10.49 | 161.91 |
| A:B＝1:250 | 55.47 | 13.36 | 9.95 | 134.19 |
| A:B＝1:500 | 58.34 | 12.70 | 9.78 | 129.94 |
| A:B＝1:750 | 60.39 | 12.27 | 9.72 | 126.30 |
| A:B＝1:1000 | 62.48 | 11.86 | 9.69 | 122.45 |
The Toxicity Determination result of table 2 methylsulfonyl bacterium azoles and the composite control cucumber bacterial angular leaf spot of chitin
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (hereinafter referred to as A) | 7.63 | 100.00 | / | / |
| Chitin (hereinafter referred to as C) | 94.68 | 8.06 | / | / |
| A:C＝1000:1 | 6.31 | 120.92 | 99.91 | 121.03 |
| A:C＝750:1 | 5.85 | 130.43 | 99.88 | 130.59 |
| A:C＝500:1 | 5.24 | 145.61 | 99.82 | 145.88 |
| A:C＝250:1 | 5.03 | 151.69 | 99.63 | 152.25 |
| A:C＝100:1 | 4.75 | 160.63 | 99.09 | 162.11 |
| A:C＝50:1 | 4.79 | 159.29 | 98.20 | 162.21 |
| A:C＝20:1 | 4.91 | 155.40 | 95.62 | 162.51 |
| A:C＝8:1 | 5.03 | 151.69 | 89.78 | 168.95 |
| A:C＝3:1 | 5.39 | 141.56 | 77.01 | 183.81 |
| A:C＝1:1 | 7.36 | 103.67 | 54.03 | 191.87 |
| A:C＝1:3 | 13.78 | 55.37 | 31.04 | 178.36 |
| A:C＝1:8 | 23.52 | 32.44 | 18.27 | 177.52 |
| A:C＝1:20 | 35.14 | 21.71 | 12.44 | 174.59 |
| A:C＝1:50 | 45.76 | 16.67 | 9.86 | 169.08 |
| A:C＝1:100 | 53.13 | 14.36 | 8.97 | 160.12 |
| A:C＝1:250 | 62.41 | 12.23 | 8.43 | 145.11 |
| A:C＝1:500 | 71.35 | 10.69 | 8.24 | 129.74 |
| A:C＝1:750 | 75.18 | 10.15 | 8.18 | 124.05 |
| A:C＝1:1000 | 77.98 | 9.78 | 8.15 | 120.05 |
From toxicity test result table 1, table 2, methylsulfonyl bacterium azoles respectively with humic acid, chitin in (100 ~ 0.01): composite in (0.01 ~ 100) scope, the CTC value of control cucumber bacterial angular leaf spot is all greater than 120, and composite both showing have obvious synergistic function.Especially in (100 ~ 1): time composite in (1 ~ 100) scope, the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Toxicity Determination embodiment two: (Toxicity Determination of control citrus bacterial canker disease)
Below that the Toxicity Determination of the composite control citrus bacterial canker disease of methylsulfonyl bacterium azoles and amino acid is tested.
Test is with reference to " pesticide bioassay technology " (old spring chief editor, press of Beijing Agricultural University publishes) and " farm-chemical indoor determination test rule NY/T1156.2-2006 ".This test adopts inhibition zone method.On aseptic operating platform, poured into by NA substratum on NA flat board, after drying, the citrus processing bacteria suspension spreading rod getting 0.1ml is applied on NA flat board equably.After drying, punch in dull and stereotyped central authorities with the punch tool of diameter 7mm, then get 100 μ l liquids in aperture.Each concentration 5 repetition.To add the process of sterilized water in aperture for blank.Be placed on the thermostat container sterile culture of 28 ± 0.5 DEG C after process, take out after 2d.Adopt right-angled intersection method to measure the antibacterial circle diameter (in units of millimeter) of each process respectively, and calculate mean value, the inhibiting rate of antibacterial circle diameter.Carry out statistical study with DPS data processing software, calculate the EC of each medicament
50, then press the abundant method of Sun Yun and calculate cotoxicity coefficient (CTC), the results are shown in Table 3.
The Toxicity Determination result of table 3 methylsulfonyl bacterium azoles and the composite control citrus bacterial canker disease of amino acid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (hereinafter referred to as A) | 9.41 | 100.00 | / | / |
| Amino acid (hereinafter referred to as D) | 79.44 | 11.85 | / | / |
| A:D＝1000:1 | 7.65 | 123.01 | 99.91 | 123.11 |
| A:D＝700:1 | 7.17 | 131.24 | 99.87 | 131.41 |
| A:D＝450:1 | 6.94 | 135.59 | 99.80 | 135.86 |
| A:D＝200:1 | 6.17 | 152.51 | 99.56 | 153.18 |
| A:D＝100:1 | 5.92 | 158.95 | 99.13 | 160.35 |
| A:D＝50:1 | 5.95 | 158.15 | 98.27 | 160.93 |
| A:D＝21:1 | 6.03 | 156.05 | 95.99 | 162.57 |
| A:D＝7:1 | 6.39 | 147.26 | 88.98 | 165.50 |
| A:D＝2.5:1 | 7.36 | 127.85 | 74.81 | 170.90 |
| A:D＝1:1 | 8.61 | 109.29 | 55.92 | 195.43 |
| A:D＝1:2.5 | 12.05 | 78.09 | 37.03 | 210.87 |
| A:D＝1:7 | 20.91 | 45.00 | 22.86 | 196.82 |
| A:D＝1:21 | 33.38 | 28.19 | 15.85 | 177.83 |
| A:D＝1:50 | 42.90 | 21.93 | 13.57 | 161.59 |
| A:D＝1:100 | 45.94 | 20.48 | 12.72 | 161.05 |
| A:D＝1:200 | 52.76 | 17.84 | 12.28 | 145.19 |
| A:D＝1:450 | 55.51 | 16.95 | 12.04 | 140.79 |
| A:D＝1:700 | 60.04 | 15.67 | 11.97 | 130.92 |
| A:D＝1:1000 | 65.24 | 14.42 | 11.93 | 120.87 |
From toxicity test result table 3, methylsulfonyl bacterium azoles and amino acid are in (100 ~ 0.01): composite in (0.01 ~ 100) scope, the CTC value of control citrus bacterial canker disease is all greater than 120, and composite both showing have obvious synergistic function.Especially in (100 ~ 1): time composite in (1 ~ 100) scope, the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Toxicity Determination embodiment three: (Toxicity Determination of control bacterial leaf streak of rice)
Below that the Toxicity Determination of the composite control bacterial leaf streak of rice of methylsulfonyl bacterium azoles and xanthohumic acid is tested.
Test method: adopt in vitro Nephelometric Determination, design concentration on the basis of pilot study, each medicament is joined respectively in NA liquid nutrient medium, gradient dilution makes pastille substratum, Inoculated Rice Xanthomonas campestris PV.oryzicola is placed on 28 DEG C of about shaking culture 24h, its turbidity (turbidity and bacterium amount be changing into positive correlation) is measured with turbidimeter, the inhibiting rate that each chemicals treatment breeds bacterial growth is calculated according to the turbidity of blank and the turbidity of process, by the linear regression analysis between the probit value of inhibiting rate and the logarithmic value of serial drug concentration, obtain the EC of each medicament
50value, CTC value.The results are shown in Table 4.
The Toxicity Determination result of the composite control bacterial leaf streak of rice of xanthohumic acid in table 4 methylsulfonyl bacterium azoles and humic acids
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (hereinafter referred to as A) | 6.26 | 100.00 | / | / |
| Xanthohumic acid (hereinafter referred to as B) | 97.33 | 6.43 | / | / |
| A:B＝1000:1 | 5.16 | 121.32 | 99.91 | 121.43 |
| A:B＝730:1 | 4.50 | 139.11 | 99.87 | 139.29 |
| A:B＝470:1 | 4.30 | 145.58 | 99.80 | 145.87 |
| A:B＝230:1 | 4.19 | 149.40 | 99.59 | 150.01 |
| A:B＝100:1 | 3.93 | 159.29 | 99.07 | 160.78 |
| A:B＝60:1 | 3.95 | 158.48 | 98.47 | 160.95 |
| A:B＝50:1 | 3.96 | 158.08 | 98.17 | 161.04 |
| A:B＝25:1 | 4.04 | 154.95 | 96.40 | 160.73 |
| A:B＝9:1 | 4.11 | 152.31 | 90.64 | 168.03 |
| A:B＝3:1 | 4.72 | 132.63 | 76.61 | 173.12 |
| A:B＝1:1 | 5.45 | 114.86 | 53.22 | 215.84 |
| A:B＝1:3 | 10.50 | 59.62 | 29.82 | 199.90 |
| A:B＝1:9 | 20.78 | 30.13 | 15.79 | 190.80 |
| A:B＝1:25 | 35.88 | 17.45 | 10.03 | 173.94 |
| A:B＝1:50 | 45.04 | 13.90 | 8.27 | 168.14 |
| A:B＝1:60 | 48.31 | 12.96 | 7.97 | 162.67 |
| A:B＝1:100 | 53.11 | 11.79 | 7.36 | 160.19 |
| A:B＝1:230 | 59.20 | 10.57 | 6.84 | 154.67 |
| A:B＝1:470 | 65.36 | 9.58 | 6.63 | 144.45 |
| A:B＝1:730 | 71.35 | 8.77 | 6.56 | 133.75 |
| A:B＝1:1000 | 78.16 | 8.01 | 6.53 | 122.74 |
From toxicity test result table 4, methylsulfonyl bacterium azoles and xanthohumic acid are in (100 ~ 0.01): composite in (0.01 ~ 100) scope, the CTC value of control bacterial leaf streak of rice is all greater than 120, and composite both showing have obvious synergistic function.Especially in (100 ~ 1): time composite in (1 ~ 100) scope, the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Toxicity Determination embodiment four: (Toxicity Determination of control of plant bacterial wilt)
Below that methylsulfonyl bacterium azoles and Lalgine are tested the Toxicity Determination of bacterial wilt of tomato.
Test method: with reference to the method for tobacco bacterial wilt Toxicity Determination, after bacterial wilt of tomato pathogenic bacteria is activated on NA substratum, be made into bacterium stoste with sterilized water, the colony number grown after bacterium stoste is diluted to coated plate 100ul is the bacteria suspension of about 100, for subsequent use.
Get 400ul bacteria suspension and equivalent agricultural chemicals single dose mixes, 100ul is got with liquid-transfering gun, be placed on ready-made NA flat board, with sterilized " L " shape glass stick by even for bacteria suspension coating, cultivate 48h for 28 DEG C, counting colony number, and press formulae discovery bacteriostasis rate, bacterium colony inhibiting rate (%)=(contrast colony number-process colony number)/contrast colony number × 100, often process repetition 4 times, replace pesticide-treated for contrast with sterilized water, the result of gained adopts Excel software analysis, calculates the EC of each medicament
50, and calculate cotoxicity coefficient according to the abundant method of Sun Yun.The results are shown in Table 5.
The Toxicity Determination result of table 5 methylsulfonyl bacterium azoles and the composite control of plant bacterial wilt of Lalgine
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (hereinafter referred to as A) | 14.37 | 100.00 | / | / |
| Lalgine (hereinafter referred to as B) | 87.36 | 16.45 | / | / |
| A:B＝1000:1 | 11.88 | 120.96 | 99.92 | 121.06 |
| A:B＝800:1 | 10.90 | 131.83 | 99.90 | 131.97 |
| A:B＝600:1 | 9.89 | 145.30 | 99.86 | 145.50 |
| A:B＝400:1 | 9.50 | 151.26 | 99.79 | 151.58 |
| A:B＝200:1 | 9.28 | 154.85 | 99.58 | 155.50 |
| A:B＝100:1 | 8.99 | 159.84 | 99.17 | 161.18 |
| A:B＝50:1 | 9.03 | 159.14 | 98.36 | 161.79 |
| A:B＝15:1 | 9.25 | 155.35 | 94.78 | 163.91 |
| A:B＝4:1 | 9.56 | 150.31 | 83.29 | 180.47 |
| A:B＝1:1 | 12.05 | 119.25 | 58.22 | 204.82 |
| A:B＝1:4 | 24.06 | 59.73 | 33.16 | 180.12 |
| A:B＝1:15 | 38.02 | 37.80 | 21.67 | 174.41 |
| A:B＝1:50 | 48.21 | 29.81 | 18.09 | 164.79 |
| A:B＝1:100 | 51.82 | 27.73 | 17.28 | 160.51 |
| A:B＝1:200 | 56.87 | 25.27 | 16.86 | 149.83 |
| A:B＝1:400 | 62.17 | 23.11 | 16.66 | 138.76 |
| A:B＝1:600 | 65.41 | 21.97 | 16.59 | 132.44 |
| A:B＝1:800 | 70.34 | 20.43 | 16.55 | 123.41 |
| A:B＝1:1000 | 72.37 | 19.86 | 16.53 | 120.10 |
From toxicity test result table 5, methylsulfonyl bacterium azoles and Lalgine are in (100 ~ 0.01): composite in (0.01 ~ 100) scope, the CTC value of control of plant bacterial wilt is all greater than 120, and composite both showing have obvious synergistic function.Especially in (100 ~ 1): time composite in (1 ~ 100) scope, the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Land for growing field crops test examples
Complex composition provided by the invention, have efficient, the lasting period is long, medication is low, safety, environmental protection feature, illustrate with several embodiment below.Following methylsulfonyl bacterium azoles is referred to as first sulphur.
Contrast medicament 1:20% methylsulfonyl bacterium azoles wettable powder, self-control;
Contrast medicament 2:10% humic acids wettable powder, self-control;
Contrast medicament 3:10% Lalgine wettable powder, self-control;
Contrast medicament 4:10% chitin wettable powder, self-control;
Contrast medicament 5:0.2% methylsulfonyl bacterium azoles granule, self-control;
Contrast medicament 6: containing humic acid water-soluble fertilizer, aqua, register technique index: humic acids >=30g/L; N+P2O5+K2O >=200g/L.Registration card number: agriculture fertilizer (2014) faces No. 8291, word, Shanghai You Ma Bioisystech Co., Ltd, commercial;
Contrast medicament 7: containing amino acid water-soluble fertilizer, aqua, register technique index: amino acid >=100g/L, Mn+Zn+B >=20g/L.Registration card number: agriculture fertilizer (2014) faces No. 8310, word, the large plump industry Science and Technology Ltd. in Weifang, commercial.
Field efficacy embodiment one: the field control effectiveness test of control cucumber bacterial angular leaf spot
Test method: the test method of recommending with reference to " GB/T17980.110-2004 pesticide field efficacy medicine test criterion (two) the 110th part: bactericidal agent for preventing and treating cucumber bacterial angular leaf spot ".When beginning to see scab first time spray pesticide, second time spray pesticide after 7d.Dispenser twice altogether, each process plot area is 25m
2, multiplicity 4 times.The incidence of each community of 7d, 14d sample survey after second time dispenser, record investigation number, disease progression, calculate disease index and preventive effect.The results are shown in Table 6:
Table 6 methylsulfonyl bacterium azoles is the field control effectiveness test result of composite control cucumber bacterial angular leaf spot with humic acid, amino acid etc. respectively
Known according to test of pesticide effectiveness result table 6, when preventing and treating cucumber bacterial angular leaf spot, methylsulfonyl bacterium azoles respectively with humic acid, amino acid, Lalgine, chitin composite when consumption no more than preventive effect when single dose consumption higher than single dose, higher than the preventive effect of single dose by more than 21.35%, synergy is obvious.And the preventive effect of 14 days can also reach more than 77% after second time medicine, the lasting period is long.
Field efficacy embodiment two: the field control effectiveness test of control of plant bacterial wilt
Test method and method of calculation reference " NY/T1464.32-2010 pesticide field efficacy medicine test criterion the 32nd part: bactericidal agent for preventing and treating bacterial wilt of tomato ", every plot area 30m
2, often process and repeat for 4 times, carry out root granule and spread fertilizer over the fields dispenser when first meeting morbidity strain, or wettable powder is mixed soil and is spread fertilizer over the fields dispenser, if spread soil to be treated to blank.15 days, 30 days investigation results after medicine before medicine, after medicine, in units of strain, classification investigation incidence, calculates disease index, preventive effect.The results are shown in Table 7:
Table 7 methylsulfonyl bacterium azoles is the composite control of plant bacterial wilt field control effectiveness test result with humic acid, amino acid etc. respectively
Known according to test of pesticide effectiveness result table 7, methylsulfonyl bacterium azoles respectively with humic acid, chitin, amino acid during composite control of plant bacterial wilt when consumption is no more than single dose consumption, the prevention effect of each process is higher than single dose, after medicine, the preventive effect of 15 days is higher than single dose by more than 23.70%, and synergy is obvious; After medicine, the preventive effect of 30 days can also reach more than 78%, and the lasting period is long.
Claims (9)
1. contain a complex composition for methylsulfonyl bacterium azoles and foliage fertilizer, it is characterized in that, described complex composition contains two kinds of active components A and B, described A is methylsulfonyl bacterium azoles, and its chemical name is 2-(to fluorophenyl)-5-methylsulfonyl-1,3,4-oxadiazole, B is foliage fertilizer; Described foliage fertilizer is any in humic acid, chitin, amino acid, Lalgine.
2. the complex composition containing methylsulfonyl bacterium azoles and foliage fertilizer according to claim 1, is characterized in that: the weight ratio of described active components A and activeconstituents B is 100:0.01 to 0.01:100.
3. the complex composition containing methylsulfonyl bacterium azoles and foliage fertilizer according to claim 2, is characterized in that: the weight ratio of described active components A and activeconstituents B is 100:1 to 1:100.
4. the complex composition containing methylsulfonyl bacterium azoles and foliage fertilizer again according to claim 3, is characterized in that: the weight ratio of described active components A and activeconstituents B is 50:1 to 1:50.
5. contain a preparation for methylsulfonyl bacterium azoles and foliage fertilizer, it is characterized in that, comprise acceptable auxiliary material on the arbitrary described complex composition of claim 1-4 and agricultural chemicals, be then prepared into disinfectant use in agriculture.
6. the preparation containing methylsulfonyl bacterium azoles and foliage fertilizer according to claim 5, it is characterized in that, by weight, the weight percentage that described complex composition accounts for described disinfectant use in agriculture is 0.1%-90%.
7. the preparation containing methylsulfonyl bacterium azoles and foliage fertilizer according to claim 6, it is characterized in that, by weight, the weight percentage that described complex composition accounts for described disinfectant use in agriculture is 1%-60%.
8. according to the arbitrary described preparation containing methylsulfonyl bacterium azoles and foliage fertilizer of claim 5-7, it is characterized in that, on described agricultural chemicals, acceptable auxiliary material is the mixture of a kind of and auxiliary agent in solvent and filler.
9. the purposes of arbitrary described complex composition in control crop bacterial disease in claim 1-4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN105085075A (en) * | 2015-09-12 | 2015-11-25 | 顾伟 | Agricultural composition containing propamidine and foliage fertilizer |
| CN107258332A (en) * | 2017-05-28 | 2017-10-20 | 陈俊豪 | The engrafting method of emperor's mandarin orange high yield |
| CN107258426A (en) * | 2017-05-28 | 2017-10-20 | 陈俊豪 | Improve the cultural method of emperor's mandarin orange pulp quality |
| CN107347547A (en) * | 2017-05-28 | 2017-11-17 | 陈俊豪 | The implantation methods of emperor mandarin orange |
| CN107586195A (en) * | 2017-09-22 | 2018-01-16 | 无为县姚沟镇太白瓜蒌种植专业合作社 | A kind of Snakegourd Fruit best fruiting period foliar fertilizer |
| CN108794140A (en) * | 2017-05-04 | 2018-11-13 | 江苏龙灯化学有限公司 | A kind of solid pharmaceutical preparation and its preparation method and application containing alginic acid and trace element built |
| CN113429239A (en) * | 2021-07-28 | 2021-09-24 | 齐齐哈尔盛泽农药有限公司 | Oil suspending agent fertilizer and application |
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| CN107258426A (en) * | 2017-05-28 | 2017-10-20 | 陈俊豪 | Improve the cultural method of emperor's mandarin orange pulp quality |
| CN107347547A (en) * | 2017-05-28 | 2017-11-17 | 陈俊豪 | The implantation methods of emperor mandarin orange |
| CN107586195A (en) * | 2017-09-22 | 2018-01-16 | 无为县姚沟镇太白瓜蒌种植专业合作社 | A kind of Snakegourd Fruit best fruiting period foliar fertilizer |
| CN113429239A (en) * | 2021-07-28 | 2021-09-24 | 齐齐哈尔盛泽农药有限公司 | Oil suspending agent fertilizer and application |
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