A bactericidal composition containing cymoxanil and myclobutanil and its application

Abstract

The present invention discloses the application of a composition containing cymoxanil and myclobutanil, and the formulations include wettable powders, water dispersible granules and suspensions of the said composition. The weight percentage of cymoxanil to myclobutanil in the said composition is 1-80:60-1. Using the formulations containing the composition of the present invention can effectively control brown rot of fruit trees.

Description

Technical Field

[0001] The present invention relates to a composition containing cymoxanil and myclobutanil, its preparation and application, and belongs to the technical field of preparation application. Background Art

[0002] The molecular formula of cymoxanil is C 7 H 10 N 4 O 3 , and the chemical name is: 1-(2-cyano-2-methoxyimino)-3-ethylurea.

[0003] Cymoxanil is a highly effective and low-toxic fungicide, which is effective against fungi of the order Peronosporales such as Phytophthora and Peronospora. Mixing it with other protective fungicides can improve the efficacy, expand the fungicidal spectrum, and delay the generation of pathogen resistance, so as to protect plants from the invasion of pathogens.

[0004] The molecular formula of myclobutanil is C 15 H 17 ClN 4 , and the chemical name is: 2-(4-chlorophenyl)-2-(1H,1,2,4-triazol-1-ylmethyl)hexanenitrile.

[0005] Myclobutanil belongs to triazole fungicides and is an inhibitor of ergosterol biosynthesis. It has strong systemic absorption, high efficacy, safety for crops, and long residual period, and has preventive and therapeutic effects on brown rot of fruit trees.

[0006] At present, the products for controlling brown rot of fruit trees include carbendazim, mancozeb, thiophanate-methyl, etc. The long-term continuous use of the above products at high doses has led to a certain degree of resistance of pathogenic bacteria. Compared with the above products, the compound of cymoxanil and myclobutanil can better control brown rot of fruit trees according to different action mechanisms and delay the generation of resistance at the same time. Summary of the Invention

[0007] The technical problem to be solved by the present invention is: to provide a bactericidal composition containing cymoxanil and myclobutanil with reasonable components, broad fungicidal spectrum, good control effect, low use cost, safety for crops and capable of delaying the resistance of pathogenic bacteria.

[0008] The present invention solves the technical problem through the following technical solutions:

[0009] In the first aspect of the present invention, a composition containing cymoxanil and myclobutanil is provided, and the weight percentage of cymoxanil and myclobutanil in the composition is 1-80:60-1; preferably 5-50:35-5; more preferably 10-40:30-10.

[0010] In a second aspect of the present invention, there is provided a preparation comprising the composition described above, and the preparation is a wettable powder, a water dispersible granule or a suspension concentrate.

[0011] Preferably, the method for preparing the wettable powder comprises the following steps:

[0012] Step 1: Prepare raw materials, including cymoxanil, myclobutanil, a dispersant, a wetting agent and a filler;

[0013] Step 2: Mix cymoxanil, myclobutanil, the dispersant, the wetting agent and the filler uniformly, pulverize them and then mix them uniformly again to obtain the wettable powder;

[0014] Among them, the dispersant is selected from one or more of polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, calcium alkylbenzenesulfonate, sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester and glycerol fatty acid polyoxyethylene ether;

[0015] The wetting agent is selected from one or more of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, Nekal, soap powder and sodium p-methoxy fatty amide benzene sulfonate.

[0016] The filler is selected from one or more of silica white, kaolin, starch, diatomite, bentonite, attapulgite and light calcium carbonate.

[0017] Preferably, the ratio of each component in the raw materials is: cymoxanil 1-60%; myclobutanil 1-40%; dispersant 3-12%; wetting agent 2-10%; filler 8-84%.

[0018] Preferably, the mixing in Step 2 is carried out in a mixing tank, and the pulverizing method is pulverization by a jet mill.

[0019] Preferably, the method for preparing the water dispersible granule of the composition comprises the following steps:

[0020] Step 1: Prepare raw materials, including cymoxanil, myclobutanil, a dispersant, a wetting agent, a filler, and add a disintegrant as needed;

[0021] Step 2: Pulverize the cymoxanil, myclobutanil, the dispersant, the wetting agent, the disintegrant and the filler described in Step 1 to obtain a powder of 20-50 microns, which is the material for granulation;

[0022] Step 3: Granulate and dry the granulation material obtained in Step 2 to obtain the water dispersible granule.

[0023] Among them, the dispersant is selected from one or more of polycarboxylate, lignosulfonate, sodium methylene bisnaphthalenesulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, calcium alkylbenzene sulfonate, sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester, and glycerol fatty acid polyoxyethylene ether;

[0024] The wetting agent is selected from one or more of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, Nekal, and soponification powder;

[0025] The disintegrant is selected from one or more of bentonite, urea, ammonium sulfate, alumina, citric acid, and sodium bicarbonate;

[0026] The filler is selected from one or more of silica white, kaolin, starch, diatomite, bentonite, attapulgite, and light calcium carbonate.

[0027] Preferably, the ratio of each component in the raw materials is as follows: cymoxanil 1-60%; myclobutanil 1-40%; dispersant 3-15%; wetting agent 2-10%; disintegrant 0-7% and not 0; filler 8-85%.

[0028] Preferably, the crushing in step 2 is carried out by a jet mill; the granulation method in step 3 is extrusion granulation or fluidized bed granulation.

[0029] Preferably, the preparation method of the suspending agent of the composition is characterized by including the following steps:

[0030] Step 1, prepare raw materials, including cymoxanil, myclobutanil, dispersant, wetting agent, defoaming agent, and deionized water; add a thickening agent and an antifreezing agent as required;

[0031] Step 2, mix the dispersant, wetting agent, defoaming agent, thickening agent, antifreezing agent, and deionized water described in step 1 to obtain a slurry;

[0032] Step 3, add cymoxanil and myclobutanil to the slurry obtained in step 2 and mix and grind them to make the particle size of 90% of the fine particles below 5 μm to obtain a suspending agent;

[0033] Among them, the dispersant is selected from one or more of polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, calcium alkylbenzene sulfonate, sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester, and glycerol fatty acid polyoxyethylene ether;

[0034] The wetting agent is selected from one or more of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, Nekal, and soponification powder;

[0035] The defoamer selected is silicone oil and / or silicone compounds;

[0036] The thickener selected is one or more of polyvinyl alcohol, polyethylene glycol, xanthan gum, hydroxyethyl cellulose and methyl cellulose;

[0037] The antifreeze selected is one or more of glycerol, propylene glycol and ethylene glycol.

[0038] Preferably, the ratio of each component in the raw materials is as follows: cymoxanil 1-60%; myclobutanil 1-40%; dispersant 3-13%; wetting agent 2-10%; defoamer 0.1-0.5%; thickener 0-2% and not 0; antifreeze 0-10% and not 0; deionized water as the balance.

[0039] Preferably, the method of crushing in step 2 is shear crushing; the method of grinding in step 3 is grinding in a grinder, and the grinding time is 2-3 hours.

[0040] In the third aspect of the present invention, there is provided an application of the preparation in preventing and treating brown rot of fruit trees.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] 1. The effective active ingredients cymoxanil and myclobutanil provided by the present invention belong to fungicides with different action mechanisms, and there is no conflict between their mixing.

[0043] 2. The present invention has a good synergistic effect on resistant diseases within a certain range, the control effect is higher than that of single agents, and the dosage is small.

[0044] 3. The present invention does not use organic solvents, is not easy to cause phytotoxicity, and is convenient for transportation and storage.

[0045] 4. The composition of the present invention has a good treatment effect on brown rot of fruit trees. Detailed implementation mode

[0046] To make the present invention more obvious and understandable, the following is a detailed description with preferred embodiments:

[0047] Example 1 Preparation of wettable powder containing 70% cymoxanil and myclobutanil

[0048] A mixture containing 50% cymoxanil, 20% myclobutanil, 5% sodium methylenebisnaphthalenesulfonate, 3% sodium dodecyl sulfate, 2% silica and 20% kaolin is subjected to air flow crushing to obtain a wettable powder containing 70% cymoxanil and myclobutanil.

[0049] Example 2 Preparation of wettable powder containing 55% cymoxanil and myclobutanil

[0050] A mixture containing 30% cymoxanil, 25% myclobutanil, 4% lignosulfonate, 4% detergent LS (sodium p-methoxy fatty acid amide benzene sulfonate), 8% white carbon black, and 29% kaolin is subjected to air flow pulverization to obtain a wettable powder containing 55% cymoxanil and myclobutanil.

[0051] Example 3 Preparation of a Wettable Powder Containing 40% Cymoxanil and Myclobutanil

[0052] A mixture containing 20% cymoxanil, 20% myclobutanil, 2% sodium dodecyl sulfate, 5% detergent NNO (sodium methylene bisnaphthalene sulfonate), 8% white carbon black, and 45% bentonite is subjected to air flow pulverization to obtain a wettable powder containing 45% cymoxanil and myclobutanil.

[0053] Example 4 Preparation of a Wettable Powder Containing 25% Cymoxanil and Myclobutanil

[0054] A mixture containing 15% cymoxanil, 10% myclobutanil, 2% lignosulfonate, 3% sodium p-methoxy fatty acid amide benzene sulfonate, 5% white carbon black, and 75% kaolin is subjected to air flow pulverization to obtain a wettable powder containing 25% cymoxanil and myclobutanil.

[0055] Example 5 Preparation of a Water Dispersible Granule Containing 60% Cymoxanil and Myclobutanil

[0056] A mixture containing 40% cymoxanil, 20% myclobutanil, 3% polycarboxylate, 3% lignosulfonate, 4% sodium dodecyl sulfate, 2% ammonium sulfate, and 13% starch is subjected to air flow pulverization to obtain a water dispersible granule containing 60% cymoxanil and myclobutanil.

[0057] Example 6 Preparation of a Water Dispersible Granule Containing 50% Cymoxanil and Myclobutanil

[0058] A mixture containing 30% cymoxanil, 20% myclobutanil, 3% lignosulfonate, 3% sodium dodecyl sulfate, 2% polyvinyl alcohol, 3% sodium bicarbonate, 20% starch, and 12% kaolin is subjected to air flow pulverization to obtain a water dispersible granule containing 50% cymoxanil and myclobutanil.

[0059] Example 7 Preparation of a Water Dispersible Granule Containing 40% Cymoxanil and Myclobutanil

[0060] A mixture containing 25% cymoxanil, 15% myclobutanil, 5% sodium lignosulfonate, 6% ammonium sulfate, 3% polyvinyl alcohol, 1% citric acid, 20% starch, and 35% light calcium carbonate is subjected to air flow pulverization to obtain a water dispersible granule containing 40% cymoxanil and myclobutanil.

[0061] Example 8 Preparation of a Water Dispersible Granule Containing 30% Cymoxanil and Myclobutanil

[0062] A mixture containing 22% cymoxanil, 8% myclobutanil, 5% alkylphenol polyoxyethylene ether, 2% dodecylbenzenesulfonic acid, 20% starch, and 53% diatomaceous earth is subjected to air flow pulverization to obtain a 30% cymoxanil and myclobutanil water dispersible granule.

[0063] Example 9 Preparation of a 50% Cymoxanil and Myclobutanil Suspension

[0064] 35% cymoxanil, 15% myclobutanil, 4% sodium dodecyl sulfate, 3% fatty alcohol polyoxyethylene ether, 4% dodecylbenzenesulfonic acid, 0.1% silicone oil, 0.3% xanthan gum, deionized water is added to 100%, and the mixture is prepared to obtain a 50% cymoxanil and myclobutanil suspension.

[0065] Example 10 Preparation of a 35% Cymoxanil and Myclobutanil Suspension

[0066] 20% cymoxanil, 15% myclobutanil, 4% polycarboxylate, 5% sapindus powder, 0.1% silicone compound, 0.1% hydroxyethyl cellulose, 2% ethylene glycol, deionized water is added to 100%, and the mixture is prepared to obtain a 35% cymoxanil and myclobutanil suspension.

[0067] Example 11 Preparation of a 20% Cymoxanil and Myclobutanil Suspension

[0068] 10% cymoxanil, 10% myclobutanil, 4% fatty acid polyoxyethylene ester, 5% sophora powder, 0.1% silicone compound, 0.4% polyvinyl alcohol, 2% propylene glycol, deionized water is added to 100%, and the mixture is prepared to obtain a 15% cymoxanil and myclobutanil suspension.

[0069] Example 12 Preparation of a 10% Cymoxanil and Myclobutanil Suspension

[0070] 4% cymoxanil, 6% myclobutanil, 2% polycarboxylate, 2% sodium dodecylbenzenesulfonate, 0.1% silicone compound, 0.5% polyethylene glycol, 4% glycerol, deionized water is added to 100%, and the mixture is prepared to obtain a 5% cymoxanil and myclobutanil suspension.

[0071] The following performance tests are carried out on the above-mentioned examples:

[0072] I. Determination of the combined toxicity of different ratios of cymoxanil and myclobutanil against brown rot of peaches

[0073] Step 1: Cool the prepared culture medium to 60°C - 70°C, add a quantitative amount of the drug according to the set concentration to make a toxic culture medium containing different amounts of the drug. After it is fully cooled, inoculate a test pathogen disk with a diameter of 0.5 cm. In addition, set up an acetone solvent and a blank control, and place them in an incubator for cultivation (25°C ± 1°C).

[0074] Step 2: Monilinia fructicola (wint) Rehm. was cultured in an incubator for 120 hours for investigation. During the investigation, the colony growth diameter of the tested pathogenic bacteria in each treatment was measured respectively, and the inhibition rate was calculated.

[0075] Step 3: The DPS data processing system was used to calculate the virulence regression equation of each pesticide, and the EC of each tested pesticide and its formulation was obtained. 50 . According to the method of SUN-Johnson, the co-toxicity coefficient was obtained to compare the virulence effects of each pesticide, so as to screen out the best synergistic formulation.

[0076] Calculation method:

[0077] Co-toxicity coefficient CTC = actual virulence index of the mixture / theoretical virulence index of the mixture × 100

[0078] Actual virulence index of the mixture = EC of pesticide A 50 value / EC of the mixture (A + B) 50 value × 100

[0079] Theoretical virulence index of the mixture = virulence index of pesticide A × percentage of active ingredient of pesticide A in the mixture + virulence index of pesticide B × percentage of active ingredient of pesticide B in the mixture

[0080] Co-toxicity coefficient CTC: greater than 120 is synergistic, less than 80 is antagonistic, and 80 to 120 is additive.

[0081] The instruments used for measuring parameters are: constant temperature incubator, sterile room, electronic balance, ultra-clean workbench, pipette gun, etc.

[0082] The test pesticides were all provided by Yifan Biotech Group Co., Ltd.

[0083]

[0084]

[0085] II. Field efficacy of myclobutanil and cymoxanil and their mixtures against brown rot of peach

[0086] This test was carried out in Qixia District, Yantai City, Shandong Province according to the national standard of the People's Republic of China GB / T 17980.118-2004 "Pesticide field efficacy test guidelines (part 2) fungicides for controlling ring rot of apple". The test pesticides were developed and provided by Yifan Biotech Group Co., Ltd. The test was applied with pesticides 2 times, and the interval between applications was 7 days.

[0087] The test results are shown in the following table:

[0088]

[0089] III. Field Efficacy of Myclobutanil, Cymoxanil and Their Mixtures against Brown Rot of Apple

[0090] This experiment was carried out in Qixia District, Yantai City, Shandong Province according to the national standard of the People's Republic of China GB / T 17980.118-2004 "Rules for Field Efficacy Trials of Pesticides (Part 2) Fungicides for Controlling Ring Rot of Apple". The test agents were developed and provided by Yifan Biotech Group Co., Ltd. The test was applied with pesticides 2 times in total, and the interval between applications was 7 days.

[0091] The experimental results are shown in the following table:

[0092]

[0093] IV. Field Efficacy of Myclobutanil, Cymoxanil and Their Mixtures against Brown Rot of Plum

[0094] This experiment was carried out in Gaizhou City, Liaoning Province according to the national standard of the People's Republic of China GB / T 17980.118-2004 "Rules for Field Efficacy Trials of Pesticides (Part 2) Fungicides for Controlling Ring Rot of Apple". The test agents were developed and provided by Yifan Biotech Group Co., Ltd. The test was applied with pesticides 2 times in total, and the interval between applications was 7 days.

[0095] The test results are shown in the following table:

[0096]

Claims

1. A composition with cymoxanil and myclobutanil as the active ingredients, characterized in that, the weight ratio of cymoxanil to myclobutanil in the composition is 10~40:30~10.

2. A preparation containing the composition with cymoxanil and myclobutanil as the active ingredients as described in claim 1, and the preparation is a wettable powder, water dispersible granule or suspension concentrate, characterized in that, the active ingredients in the preparation are cymoxanil and myclobutanil.

3. The preparation as described in claim 2, characterized in that, the raw material components of the wettable powder include cymoxanil, myclobutanil, dispersant, wetting agent and filler; wherein, the dispersant is one or more of polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, calcium alkylbenzenesulfonate, sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester and glycerol fatty acid polyoxyethylene ether; the wetting agent is one or more of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, Nekal and soap pod powder; the filler is one or more of white carbon black, kaolin, starch, diatomite, bentonite, attapulgite and light calcium carbonate; the proportion of each component in the raw materials is: cymoxanil 1~60%; myclobutanil 1~40%; dispersant 3~12%; wetting agent 2 - 10%; filler 8~84%.

4. The preparation as described in claim 3, characterized in that, the proportion of the active ingredients is: cymoxanil 1%~50%, myclobutanil 1%~25%.

5. The preparation as described in claim 2, characterized in that, the raw material components of the water dispersible granule include cymoxanil, myclobutanil, dispersant, wetting agent, filler and disintegrant; wherein, the dispersant is one or more of polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, calcium alkylbenzenesulfonate, sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester and glycerol fatty acid polyoxyethylene ether; the wetting agent is one or more of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, Nekal and soap pod powder; the disintegrant is one or more of bentonite, urea, ammonium sulfate, alumina, citric acid and sodium bicarbonate; the filler is one or more of white carbon black, kaolin, starch, diatomite, bentonite, attapulgite and light calcium carbonate; the proportion of each component in the raw materials is: cymoxanil 1~60%, myclobutanil 1~40%, dispersant 3~15%, wetting agent 2 - 10%, disintegrant 0~7% and not 0, filler 8~85%.

6. The preparation as described in claim 5, characterized in that, the proportion of the active ingredients is: cymoxanil 1%~40%, myclobutanil 1%~20%.

7. The preparation as described in claim 2, characterized in that, the raw material components of the suspension concentrate include cymoxanil, myclobutanil, dispersant, wetting agent, defoamer, deionized water, thickener and antifreeze; Among them, the dispersant is one or more of polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, calcium alkylbenzene sulfonate, sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester, and glycerol fatty acid polyoxyethylene ether; the wetting agent is one or more of sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, Nekal, and soponification powder; the defoaming agent is silicone oil and / or silicone compounds; the thickening agent is one or more of polyvinyl alcohol, polyethylene glycol, xanthan gum, hydroxyethyl cellulose, and methyl cellulose; the antifreezing agent is one or more of glycerol, propylene glycol, and ethylene glycol; The proportion of each component in the raw materials is as follows: cymoxanil 1-60%, myclobutanil 1-40%, dispersant 3-13%, wetting agent 2-10%, defoaming agent 0.1-0.5%, thickening agent 0-2% and not 0, antifreezing agent 0-10% and not 0, with the balance being deionized water.

8. The preparation according to claim 7, wherein, the proportion of the active ingredients is: cymoxanil 1% - 35%, myclobutanil 1% - 15%.

9. Use of a preparation according to any one of claims 2 - 8 in the prevention and control of brown rot of peaches, wherein, The Latin name of the pathogen causing brown rot of peach is Monilinia fructicola (wint) Rehm.

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