A bactericidal composition comprising bifenoxam and its use

Abstract

The application belongs to the field of pesticide preparation, and particularly relates to a bactericidal composition containing bifenazate and application thereof; the bactericidal composition contains the following ingredients with the weight percentage: 3-10% of bifenazate, 5-20% of a triazole bactericide, 8-12% of Termul 5030, 1-3% of Atlox 4912, 1-5% of ethylene glycol, 13-18% of cyclohexanone, and deionized water to 100%. The triazole bactericide is tebuconazole or prothioconazole. The microemulsion prepared by the application has excellent preparation performance, and the emulsifier compound can not only form dense micelles to improve the solubilization amount, but also can reduce the emulsifier dosage, reduce the production cost, and has excellent control effect on wheat scab.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of pesticide preparation, and particularly relates to a bactericidal composition containing bifenazate and application thereof. BACKGROUND

[0002] Bifenazate is a pathogen respiration inhibitor, which inhibits the function of mitochondria by interfering with the tricarboxylic acid cycle on the complex II of the respiratory electron transport chain, prevents it from generating energy, and inhibits the growth of pathogenic bacteria, ultimately leading to its death. Bifenazate has a wide spectrum of fungicidal activity, and has both preventive and therapeutic effects, and can inhibit spore germination, mycelial growth and spore formation.

[0003] Tebuconazole is an endosmosis triazole fungicide, which is a sterol demethylation inhibitor that can inhibit the demethylation of ergosterol on the cell membrane of pathogenic bacteria, so that the pathogenic bacteria cannot form a cell membrane, thereby killing the pathogenic bacteria. Propiconazole is a triazole thio ketone fungicide, which is a sterol demethylation (biosynthesis of ergosterol) inhibitor, and has the characteristics of selectivity, protection, treatment, etc.

[0004] CN201510991965.6 discloses a bactericidal composition containing bifenazate and propiconazole, which is characterized in that the bactericidal composition takes bifenazate and propiconazole as the main effective components, and the mass ratio of bifenazate to propiconazole is 1-70:1-50. It has high synergistic effect, overcomes and delays the drug resistance of pathogenic bacteria, has fast bactericidal speed, long effective period, reduces application cost, and has obvious prevention and treatment effect, which is obviously better than the use of single agent. CN201610353890.3 discloses a bactericidal composition containing bifenazate and tebuconazole and application thereof. The bactericidal composition takes bifenazate and tebuconazole as the main effective components, and the mass ratio of bifenazate to tebuconazole is 1-70:1-50. It has high synergistic effect, overcomes and delays the drug resistance of pathogenic bacteria, has fast bactericidal speed, long effective period, reduces application cost, and has obvious prevention and treatment effect, which is obviously better than the use of single agent. The above patent documents do not study the preparation.

[0005] Pesticide microemulsion (microemulsion, ME) is a new pesticide dosage form developed in the 1970s. It is a transparent single-phase liquid preparation with water as the dispersion medium, without or with a small amount of organic solvent, containing an appropriate amount of surfactant and other additives. Microemulsion replaces a large amount of organic solvent with water, reduces the pressure on the environment during pesticide production and after application, and is an environmentally friendly pesticide dosage form. Microemulsion is a thermodynamically stable, transparent and isotropic dispersion system spontaneously formed by two immiscible liquids, which has good physical stability, long shelf life, strong diffusion and penetration ability, and high biological activity.

[0006] There is no relevant research report on the preparation of the microemulsion of bixafen and tebuconazole or prothioconazole in the prior art. The present application obtains a microemulsion formula with simple formula composition and low emulsifier dosage through systematic screening of emulsifiers, and verifies the field control effect of the microemulsion. SUMMARY

[0007] The present application provides a fungicidal composition containing bixafen and its application, and the specific technical solutions are as follows:

[0008] A fungicidal composition containing bixafen comprises the following ingredients with the weight percentage: bixafen 3-10%, triazole fungicide 5-20%, Termul 5030 8-12%, Atlox 4912 1-3%, ethylene glycol 1-5%, cyclohexanone 13-18%, and deionized water to make up 100%; the triazole fungicide is tebuconazole or prothioconazole.

[0009] The present application provides a fungicidal composition, comprising the following ingredients with the weight percentage: bixafen 4-8%, triazole fungicide 10-15%, Termul 5030 8-12%, Atlox 4912 1-3%, ethylene glycol 1-5%, cyclohexanone 13-18%, and deionized water to make up 100%.

[0010] The present application provides a fungicidal composition, comprising the following ingredients with the weight percentage: bixafen 5%, triazole fungicide 10%, Termul 5030 10%, Atlox 4912 2%, ethylene glycol 3%, cyclohexanone 15%, and deionized water to make up 100%.

[0011] The fungicidal composition described in the present application is used for preventing and treating diseases of gramineous crops. Preferably, the disease is wheat scab.

[0012] Compared with the prior art, the present application has the following beneficial effects:

[0013] Compared with a single emulsifier, the emulsifier compound can not only form a dense micelle to improve the solubilization amount, but also can reduce the emulsifier dosage and reduce the production cost.

[0014] Prothioconazole and tebuconazole both belong to triazole fungicides, and have similar physicochemical properties. The bixafen·prothioconazole microemulsion prepared by using the same microemulsion additive formula also has excellent preparation performance. DETAILED DESCRIPTION

[0015] The present application can be better understood according to the following examples. However, those skilled in the art will readily understand that the content described in the examples is only used to illustrate the present application, and should not and will not limit the present application described in detail in the claims.

[0016] Example 1: Preparation of 15% bixafen and tebuconazole microemulsion

[0017] Materials and methods:

[0018] Drugs: bixafen, tebuconazole, Termul 5030, Agrimul 600#, EL-40, Ethylan NS-500LQ, NP-10, Atlox 4912, cyclohexanone, ethanol; all purchased from the market.

[0019] Preparation method of microemulsion: dissolve the technical material with appropriate solvent cyclohexanone, then add cosolvent ethanol, fully dissolve, then add surfactant and mix evenly, add water while stirring, convert the system from water-in-oil phase to oil-in-water phase, and obtain the microemulsion. Analyze the preparation effect of different emulsifiers, and determine the best emulsifier formula.

[0020] Index performance test method:

[0021] Emulsion stability: refer to GB / T 1601-2001 "Pesticide Emulsion Stability Test Method";

[0022] pH value determination: refer to GB / T 1601-1993 "Pesticide pH Determination Method";

[0023] Transparent temperature range: take 10 mL of self-made microemulsion in a 25 mL test tube, gradually cool in a low temperature bath until turbidity or freezing occurs, and the turning point is the lower limit of transparent temperature T1. Then place the test tube in a water bath and heat at a rate of 2℃ / min, record the temperature when turbidity occurs as the upper limit of transparent temperature T2, and the transparent temperature range is T1-T2.

[0024] Thermal storage and cold storage stability test: test the indexes after storing the microemulsion at (54±2)℃ for 14d and (0±2)℃ for 7d respectively

[0025] Test results:

[0026] Emulsifier screening

[0027] Emulsifier is an important component of microemulsion, and plays a key role in the formation and stability of microemulsion. Emulsifier molecules are usually composed of hydrophilic and lipophilic groups, which assemble into micelles of different shapes in aqueous solution, thereby solubilizing hydrophobic substances in water medium. First, set the amount of emulsifier in the formula to 20%, mix well with the cosolvent and solvent containing the technical material, add water to make up the balance, observe whether the resulting solution is clear and transparent, and at the same time, test the thermal storage and cold storage stability, and record the test results after thermal storage for 14d and cold storage for 7d respectively.

[0028] As can be seen from Table 1, the microemulsions prepared using emulsifiers Termul 5030, Nonge 600# and Atlox 4912 can all form clear transparent solutions. In the transparent temperature range test, the upper limit of the transparent temperature of Termul 5030 and Atlox 4912 is higher, so Termul 5030 and Atlox 4912 are selected as the alternative emulsifiers for the microemulsion.

[0029] Table 1: Emulsifier type screening

[0030] Emulsifier Initial appearance Appearance after hot storage Appearance after cold storage Upper limit of transparency temperature Termul 5030 Clear and transparent Clear and transparent Clear and transparent 70 Agrimulse 600 Clear and transparent Clear and transparent Clear and transparent 50 EL-40 Clear and transparent White and translucent A small amount of crystal precipitated - Ethylan NS-500LQ White turbidity - - - NP-10 White turbidity - - - Atlox 4912 Clear and transparent Clear and transparent Clear and transparent 65

[0031] The alternative emulsifiers Termul 5030 and Atlox 4912 are set at 18%, 15%, 12% and 10% as gradients, and normal temperature, hot storage and cold storage stability tests are carried out respectively. As can be seen from Table 2, when the emulsifier content is the same, the performance of the microemulsion prepared by Termul 5030 is better than that of Atlox 4912, so Termul 5030 is selected as the main emulsifier for the microemulsion, and Atlox 4912 is selected as the auxiliary emulsifier for the microemulsion.

[0032] Table 2: Emulsifier content screening

[0033]

[0034]

[0035] As can be seen from Table 3, the microemulsion prepared by emulsifiers Termul 5030 + Atlox 4912 with a content of (8:1) 15%, (5:1) 15% and (5:1) 12% has better performance, and the formula with the least amount of emulsifier is selected as the emulsifier of the present application. Compared with a single emulsifier, the emulsifier complex not only can form a dense micelle to improve the solubilization amount, but also can reduce the amount of emulsifier and reduce the production cost.

[0036] Table 3: Emulsifier complex screening

[0037]

[0038] Through the screening of solvents and emulsifiers, 15% bixpyrifen and tebuconazole microemulsion is obtained, which contains the following ingredients by weight percentage: bixpyrifen 5%, tebuconazole 10%, Termul 5030 10%, Atlox 4912 2%, ethylene glycol 3%, cyclohexanone 15%, and deionized water to 100%. The performance indicators are tested and qualified.

[0039] Table 4: Performance index determination results of microemulsion

[0040] Item Test result Emulsion stability No oil and no precipitate Dispersion Fast dispersion, appearance transparent pH value 7.02 Cold storage stability Pass Hot storage stability Pass

[0041] Example 2: Test of the control effect of bifenoxime and tebuconazole or prothioconazole microemulsion on wheat scab

[0042] Test object: wheat scab.

[0043] Test agent:

[0044] Agent 1: 15% bifenoxime·tebuconazole microemulsion in Example 1;

[0045] Agent 2: 15% bifenoxime·prothioconazole microemulsion (bifenoxime 5%, prothioconazole 10%, Termul 5030 10%, Atlox 4912 2%, ethylene glycol 3%, cyclohexanone 15%, deionized water to 100%; microemulsion performance index qualified)

[0046] Test method: The test field has medium soil fertility, and the previous crop is corn. The treatment group and the control group are set, and the agents are sprayed at the heading stage of wheat (more than 50% of wheat appearing), and the control is sprayed with an equal amount of water. The specific spraying dose is shown in the table below. The test adopts random block arrangement, 4 times of repetition, and the plot area is 50m 2 .

[0047] Disease investigation method and standard: In the late filling stage of wheat, 100 plants are taken from each point according to the five-point sampling method, and the disease incidence of each ear is investigated to calculate the control effect.

[0048] Wheat scab severity grading standard:

[0049] 0 level, no disease in the whole ear;

[0050] 1 level, diseased spikelets accounting for less than 25% of the whole ear;

[0051] 3 level, diseased spikelets accounting for 26% to 50% of the whole ear;

[0052] 5 level, diseased spikelets accounting for 51% to 75% of the whole ear;

[0053] 7 level, diseased spikelets accounting for more than 75% of the whole ear.

[0054] Disease index = [Σ (number of sick ears at each level × corresponding disease level) / (total number of investigated ears × 7)] × 100

[0055] Control effect = [(disease index of the control area - disease index of the treatment area) / disease index of the control area] × 100%;

[0056] Test results

[0057] As shown in Table 5, the microemulsion of the application has excellent control effect on wheat scab.

[0058] Table 5. Test of the control effect of pydiflumetofen and triazole compound microemulsion on wheat scab

[0059] Treatment Active ingredient dosage g / acre Control effect % Pesticide 1 8 98.8 Pesticide 2 10 97.5 CK - -

[0060] The above only describes the preferred embodiments of the present application, and those skilled in the art can make appropriate improvements without departing from the raw materials of the present application, and these improvements are also within the protection scope of the present application.

Claims

1. A fungicidal composition comprising bixafen, characterized in that, The composition comprises the following ingredients with the weight percentage: bifenadime 3-10%, triazole fungicide 5-20%, Termul 5030 8-12%, Atlox 4912 1-3%, ethylene glycol 1-5%, cyclohexanone 13-18%, and deionized water to 100%.

2. The bactericidal composition according to claim 1, characterized by The composition comprises the following ingredients with the weight percentage: bifenadime 4-8%, triazole fungicide 10-15%, Termul 5030 8-12%, Atlox 4912 1-3%, ethylene glycol 1-5%, cyclohexanone 13-18%, and deionized water to 100%.

3. The germicidal composition according to claim 2, characterized in that, Bifenadime 5%, triazole fungicide 10%, Termul 5030 10%, Atlox 4912 2%, ethylene glycol 3%, cyclohexanone 15%, and deionized water to 100%.

4. The use of the fungicidal composition according to any one of claims 1-3 for controlling diseases of gramineous crops.

5. Use according to claim 4, characterized in that, The disease is wheat scab.

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