A microemulsion of pyraclostrobin and pyrimethanil, its preparation method and application
By using a specific formulation of pyraclostrobin and prochloraz microemulsion, the problems of poor penetration and flocculation have been solved, achieving efficient and stable pesticide application, adapting to various environmental conditions, and expanding the scope of application.
Patent Information
- Application Number
- CN202211720930.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-30
- Publication Date
- 2025-12-19
- Estimated Expiration
- 2042-12-30
AI Technical Summary
Existing pesticide formulations combining pyraclostrobin and prochloraz have problems such as poor penetration, short duration of action, and easy formation of flocculation and precipitation. Furthermore, their effectiveness is poor when diluted at high concentrations, which affects the efficacy of the pesticide.
By using pyraclostrobin and imazalil microemulsions, and combining anionic and nonionic emulsifiers in a specific ratio, along with fertilizer compatibility agents and solubilizers, a stable microemulsion system is formed, which improves permeability and duration of action, inhibits flocculation, and expands the scope of application.
It significantly improves pesticide utilization and bactericidal effect, reduces the number of applications, adapts to various environmental conditions, is suitable for tank mixing and aerial spraying scenarios, and enhances pesticide stability and penetration.
Smart Images

Figure BDA0004029704040000091 
Figure BDA0004029704040000101 
Figure HDA0004029704050000011
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of pesticides, in particular to a microemulsion of flusilazole and prochloraz, a preparation method and application thereof. BACKGROUND
[0002] Traditional pesticide formulations are mainly emulsifiable concentrate and wettable powder, about half of which is emulsifiable concentrate. A large amount of aromatic hydrocarbon organic solvents such as toluene and xylene in the product can easily cause environmental pollution and resource waste. With people paying more and more attention to environmental safety, more stringent requirements for the safety of pesticides have been put forward. Therefore, the development of new pesticide formulations with high efficiency, low toxicity, low residue and environmental friendliness, which replace the organic solvents in emulsifiable concentrate with water phase or all water-based formulations, has become a hot spot in the research of new pesticide formulations at home and abroad.
[0003] Chinese patent application (publication number CN106106491A) discloses a flusilazole and prochloraz compound emulsion in water, which specifically uses flusilazole and prochloraz as the main active ingredients to prepare a compound emulsion in water in the presence of other additives, and has a high prevention effect on citrus anthracnose. However, the research focuses on the synergistic effect, and ignores the further in-depth research on the penetration and persistence of pesticides; Chinese patent application (grant number CN107306947B) provides a mixture of an agricultural synergist and a flusilazole and prochloraz compound, and its preparation and application, which specifically uses a mixture of a pesticide synergist N-380 and a flusilazole and prochloraz compound to prevent and control agricultural diseases, effectively increasing the leaf penetration of flusilazole and prochloraz. However, the synergistic effect is not significant, and the highest prevention effect of 12g / mu of active ingredient content on cucumber downy mildew is 84.5%, and the best prevention effect on cucumber powdery mildew is 90.2%. In addition, traditional formulations can achieve good use effect after being diluted by hundreds of times, but in the actual application of aerial spraying, they need to be diluted at a high concentration of 10 to 50 times, and when used with leaf fertilizer and other compounds, they can produce creaming, flocculation, precipitation, and layering, which seriously affect the drug efficacy. SUMMARY
[0004] The present application relates to the technical field of pesticides, in particular to a microemulsion of flusilazole and prochloraz, a preparation method and application thereof.
[0005] As a preferred technical solution, the mass ratio of the fluoxastrobin and prochloraz is 1:(1-5); preferably, the mass ratio of the fluoxastrobin and prochloraz is 1:3; based on the system, the fluoxastrobin and prochloraz are used as effective active ingredients, under the action of specific emulsifiers, solvents and cosolvents, the combination of the two can not only not produce cross resistance, but also can synergistically act on bacteria through different bactericidal mechanisms, improve the bactericidal efficacy and range of action, and reduce the use frequency of pesticides. The inventor analyzes the reason that the fluoxastrobin is a quinone outside inhibitor, which can inhibit the electron transfer of cytochrome bc1 complex, thereby inhibiting mitochondrial respiration, and achieving the bactericidal effect, while the prochloraz can cause the effect by inhibiting the biosynthesis of sterols, and the two can produce synergistic effect through different ways and jointly play the bactericidal effect. The inventor found that, especially when the mass ratio of the fluoxastrobin and prochloraz introduced into the system is 1:3, the synergistic effect of the fluoxastrobin and prochloraz is most significant, and the fluoxastrobin and prochloraz can have the highest co-toxicity coefficient when used for preventing and treating wheat scab, banana leaf spot, citrus anthracnose and mango anthracnose.
[0006] As a preferred technical solution, the emulsifier is at least one of anionic emulsifier, anionic-nonionic mixed emulsifier and nonionic emulsifier;
[0007] As a preferred technical solution, the anionic-nonionic mixed emulsifier is mixed from alkylphenol polyoxyalkylated, 4-C10-14-alkyl derivative benzene sulfonate;
[0008] As a preferred technical solution, the anionic emulsifier is at least one of 2-naphthalenesulfonic acid formaldehyde polycondensate sodium salt, sodium lignosulfonate and calcium dodecylbenzenesulfonate;
[0009] As a preferred technical solution, the nonionic emulsifier is at least one of isooctylphenyl polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, diphenylstyryl phenol polyoxyethylene ether, phenyl phenol polyoxyethylene ether and castor oil polyoxyethylene ether;
[0010] Preferably, the emulsifier is a combination of anionic-nonionic mixed emulsifier and non-ionic emulsifier, and the mass ratio of the anionic-nonionic mixed emulsifier and the non-ionic emulsifier is (8-15):(15-25). In the pesticide preparation, although the active ingredient is the key factor for determining the final disease control, the effect of the active ingredient is closely related to the cooperation of the adjuvant, and the cooperation of the adjuvant may also affect the overall control effect and application range of the pesticide preparation. Based on the active ingredients pyraclostrobin and prochloraz adopted in the system, the combination of anionic-nonionic mixed emulsifier and non-ionic emulsifier is adopted, specifically, the combination of phenyl phenol polyoxyethylene ether and anionic-nonionic mixed emulsifier is adopted as the emulsifier, so as to ensure the synergistic effect of pyraclostrobin and prochloraz, improve the penetration and persistence of the microemulsion product, and greatly improve the utilization rate of pyraclostrobin and prochloraz. The inventor analyzes the reason: the phenyl phenol polyoxyethylene ether and the anionic-nonionic mixed emulsifier in the system have strong mutual interaction, can produce certain additive and synergistic effect, effectively improve the wetting property and emulsifying property, ensure the stability of the microemulsion system, promote the penetration of pyraclostrobin and prochloraz on the surface of the action matrix, and make the provided microemulsion can effectively and durably control. If the introduction amount of the emulsifier or the mass ratio of the anionic-nonionic mixed emulsifier and the non-ionic emulsifier is changed, the microemulsion prepared may become turbid or quickly crystallize.
[0011] Preferably, the emulsifier is a combination of phenyl phenol polyoxyethylene ether and anionic-nonionic mixed emulsifier; preferably, the HLB value of the anionic-nonionic mixed emulsifier is 9-14, preferably 13.6, TERMUL 5030, from Nanjing Hensmann Chemical Co., Ltd.; preferably, the mass ratio of the phenyl phenol polyoxyethylene ether and the anionic-nonionic mixed emulsifier is (10-14):(16-20). The model of the phenyl phenol polyoxyethylene ether is Emulsogen TS 200, from Clariant Chemicals (China) Co., Ltd. The inventors found in the exploration process that in the compounding process of anionic-nonionic mixed emulsifier and nonionic emulsifier, there is a phenomenon that only the emulsifier with a specific structure can produce additive effect after compounding, and the ratio between the emulsifiers will affect the overall compounding effect and system stability, which will lead to the failure of the synergistic effect of the pyraclostrobin and prochloraz. Based on the system of the application, by using anionic-nonionic mixed emulsifier mixed by alkyl phenol and 4-C10-14-alkyl derivative benzene sulfonate, and controlling the mass ratio of the phenyl phenol polyoxyethylene ether and the anionic-nonionic mixed emulsifier to be (10-14):(16-20), mixed micelles are formed in the system, the emulsification effect and the foam stabilization effect are maximized, the stability of the microemulsion system is ensured, the pyraclostrobin and prochloraz in the provided microemulsion can quickly wet, spread and penetrate on the surface of the target plant, and the utilization efficiency of the pesticide is significantly improved. The applicant unexpectedly found that when the HLB value of the anionic-nonionic mixed emulsifier is 9-14, especially when the HLB value of the anionic-nonionic mixed emulsifier is 13.6, the phenyl phenol polyoxyethylene ether in the system is well matched, the provided microemulsion is not easily affected by environmental humidity and temperature, and the storage stability is improved.
[0012] As a preferred technical solution, the fertilizer compatibility agent is selected from at least one of alkyl ethyl sulfonate; preferably, the model of the alkyl ethyl sulfonate is SYNERM280, which is from Nanjing Deyi Chemical Co., Ltd. In the actual production and research process, the applicant found that when the same type of product on the market was applied to tank mixing and aerial spraying, there were flocculation and crystallization phenomena, which seriously affected the efficacy of the pesticide. The inventor found that by introducing 6wt%-10wt% of the fertilizer compatibility agent, especially introducing the model of the alkyl ethyl sulfonate SYNERM280, the prepared microemulsion has good matching compatibility with other raw materials in the system, so that the prepared microemulsion has significantly improved electrolyte resistance, effectively inhibits the flocculation problem under high concentration use conditions, improves the hard water resistance and water stability of the microemulsion, can be effectively applied to tank mixing and aerial spraying scenes, expands the use range of the microemulsion product, and further improves the wetting and penetration of the pyraclostrobin and prochloraz on the surface of the target plant, and synergistically improves the utilization rate of the pesticide.
[0013] As a preferred technical solution, the solvent is at least one of dimethylformamide and dimethylacetamide; preferably, the solvent is dimethylacetamide or dimethylformamide.
[0014] As a preferred technical solution, the cosolvent is at least one of cyclohexanone, N-methyl pyrrolidone and acetone.
[0015] Another aspect of the present application provides a preparation method of a pyraclostrobin and prochloraz microemulsion, which at least comprises the following steps:
[0016] (1) The cosolvent and the solvent are added to the preparation kettle, the stirrer is turned on, pyraclostrobin is first added and stirred until dissolved, and then the prochloraz heated into a liquid state is added to the preparation kettle for dissolution and mixing;
[0017] (2) The emulsifier and the fertilizer compatibility agent are accurately weighed according to the feeding ratio and then added to the preparation kettle in sequence, and the stirrer is turned on for mixing;
[0018] (3) The deionized water is added to the preparation kettle and mixed for 30-60min to obtain the product.
[0019] As a preferred technical solution, the dissolution and mixing time in step (1) is 30-60min.
[0020] As a preferred technical solution, the mixing time in step (2) is 30-60min.
[0021] The specific process is designed in the application, the cosolvent and the solvent are mixed first, then pyraclostrobin is added and stirred until completely dissolved, then the treated pyrimethanil is added for mixing, then the emulsifier is added for emulsification, finally water is added for dispersion, the mixing time of the raw materials is controlled to be 30-60 min, a stable dispersion system which is fully dissolved, mixed and emulsified is obtained, and the method is simple and efficient.
[0022] Application of the pyraclostrobin and pyrimethanil microemulsion: for the prevention and treatment of wheat scab, banana leaf spot, citrus anthracnose and mango anthracnose.
[0023] Beneficial effects
[0024] 1. The pyraclostrobin and pyrimethanil microemulsion provided by the application adopts pyraclostrobin and pyrimethanil as effective active ingredients, and under the action of specific emulsifiers, fertilizer compatibility agents, solvents and cosolvents, a microemulsion product with good pharmaceutical properties is obtained, which can cope with high-temperature and low-temperature environments, adapt to various regional environments, transportation conditions and storage conditions, and is environmentally friendly to raw materials, effectively reduces soil pollution, and has important significance in application.
[0025] 2. By introducing 6wt%-10wt% of the fertilizer compatibility agent, especially introducing the alkyl ethyl sulfonate with the model number of SYNERM280, the microemulsion prepared has good matching compatibility with other raw materials in the system, the anti-electrolyte capacity of the microemulsion is significantly improved, the flocculation problem under high-concentration use conditions is effectively inhibited, the hard water resistance and water entry stability of the microemulsion are improved, the microemulsion can be effectively applied to the scenarios of barrel mixing and aerial spraying, the use range of the microemulsion product is expanded, and the wetting and penetration of pyraclostrobin and pyrimethanil in the microemulsion on the surface of target plants are further improved, and the utilization rate of pesticides is improved.
[0026] 3. Based on the system of the application, by adopting the anionic-nonionic mixed emulsifier which is mixed by an alkoxylated alkyl phenol and a 4-C10-14-alkyl derivative benzene sulfonate, and controlling the mass ratio of the phenol polyoxyethylene ether and the anionic-nonionic mixed emulsifier to be (10-14):(16-20), a mixed micelle is formed in the system, after water entry, a transparent homogeneous diluent can be formed, the liquid particles are in a nano state, the particle size is between 0.01-0.1 microns, the stability of the microemulsion system is ensured, the rapid wetting, spreading and penetration of pyraclostrobin and pyrimethanil in the microemulsion on the surface of target plants are ensured, and the utilization efficiency of pesticides is significantly improved.
[0027] 4. Based on the system of the present application, pyraclostrobin and prochloraz are used as effective active ingredients, and especially when the mass ratio of pyraclostrobin and prochloraz introduced into the system is 1:3, the synergistic effect of pyraclostrobin and prochloraz is most significant. Under the action of specific emulsifiers, solvents and cosolvents, the combination of pyraclostrobin and prochloraz not only does not produce cross resistance, but also can synergistically act on bacteria through different bactericidal mechanisms, thereby improving the bactericidal efficacy and range and reducing the use frequency of pesticides. BRIEF DESCRIPTION OF DRAWINGS
[0028] Figure 1 Table 1 is the toxicity test results of pyraclostrobin and prochloraz and their mixed proportions of 1:1, 1:2, 1:3, 1:4 and 1:5 on citrus anthracnose.
[0029] Figure 2 Table 2 is the toxicity test results of pyraclostrobin and prochloraz and their mixed proportions of 1:1, 1:2, 1:3, 1:4 and 1:5 on mango anthracnose.
[0030] Figure 3 Table 3 is the field efficacy test report of pyraclostrobin and prochloraz microemulsion prepared by Example 1 for preventing and treating wheat scab.
[0031] Figure 4 Figure 1 is a test result graph of 200-fold dilution of Example 1 in water, wherein (a)-(g) respectively correspond to well water, tap water, potassium dihydrogen phosphate solution, standard hard water (hardness is 342 ppm), 2-fold hard water, 5-fold hard water and 10-fold hard water.
[0032] Figure 5 Figure 2 is a test result graph of 20-fold dilution of Example 1 in water, wherein (a)-(g) respectively correspond to well water, tap water, potassium dihydrogen phosphate solution, standard hard water (hardness is 342 ppm), 2-fold hard water, 5-fold hard water and 10-fold hard water.
[0033] Figure 6 Figure 3 is a comparison graph of 20-fold dilution stability test results of Example 1 and Comparative Example 1 in water, wherein (a1) is Example 1 just after entering water, (b1) is Comparative Example 1 just after entering water; (a2) is Example 1 after entering water for 1 h, and (b2) is Comparative Example 1 after entering water for 1 h.
[0034] Figure 7 Figure 4 is a comparison graph of 20-fold dilution stability test results of Example 1 and Comparative Example 2 in potassium dihydrogen phosphate aqueous solution, wherein (a) is Example 1, and (b) is Comparative Example 2. DETAILED DESCRIPTION
[0035] Example 1
[0036] The embodiment 1 of the present application provides a pyraclostrobin and prochloraz microemulsion, comprising, in percentage by weight: pyraclostrobin 10%, prochloraz 30%, emulsifier 30%, fertilizer compatible agent 8%, solvent 8%, cosolvent 10%, and deionized water, the balance to 100%.
[0037] The emulsifier is a combination of anionic-nonionic mixed emulsifier and nonionic emulsifier; the nonionic emulsifier is phenyl phenol polyoxyethylene ether. The anionic-nonionic mixed emulsifier is mixed by alkylphenol polyethoxylate and 4-C10-14-alkyl derivative benzene sulfonate; the HLB value of the anionic-nonionic mixed emulsifier is 13.6, TERMUL 5030, from Nanjing Hensmann Chemical Co., Ltd.; the mass ratio of the phenyl phenol polyoxyethylene ether and the anionic-nonionic mixed emulsifier is 12:18. The model of the phenyl phenol polyoxyethylene ether is Emulsogen TS 200, from Clariant Chemicals (China) Co., Ltd.
[0038] The fertilizer compatible agent is alkyl ethyl sulfonate, and the model of the alkyl ethyl sulfonate is SYNERM280, from Nanjing Deyi Chemical Co., Ltd.
[0039] The solvent is dimethylacetamide.
[0040] The cosolvent is cyclohexanone.
[0041] The embodiment 1 of the present application further provides a preparation method of the pyraclostrobin and prochloraz microemulsion, comprising the following steps.
[0042] (1) adding the cosolvent and the solvent into a preparation kettle, opening a stirrer, first adding pyraclostrobin, stirring until completely dissolved, and then adding prochloraz heated into a liquid into the preparation kettle for dissolving and mixing;
[0043] (2) accurately weighing the emulsifier and the fertilizer compatible agent according to the feeding ratio, and then adding them into the preparation kettle in sequence, and opening the stirrer for mixing;
[0044] (3) adding deionized water into the preparation kettle, and mixing for 50 min to obtain the pyraclostrobin and prochloraz microemulsion.
[0045] The dissolving and mixing time in the step (1) is 60 min.
[0046] The mixing time in the step (2) is 60 min.
[0047] Embodiment 2
[0048] The embodiment 2 of the present application provides a pyraclostrobin and prochloraz microemulsion in one aspect, comprising, in percentage by weight: pyraclostrobin 20%, prochloraz 20%, emulsifier 30%, fertilizer compatible agent 8%, solvent 8%, cosolvent 10%, deionized water, and the balance.
[0049] The emulsifier is a combination of anionic-nonionic mixed emulsifier and nonionic emulsifier; the nonionic emulsifier is phenyl phenol polyoxyethylene ether. The anionic-nonionic mixed emulsifier is mixed by alkylphenol polyethoxylate and 4-C10-14-alkyl derivative benzene sulfonate; the HLB value of the anionic-nonionic mixed emulsifier is 13.6, TERMUL 5030, from Nanjing Hensmann Chemical Co., Ltd.; the mass ratio of the phenyl phenol polyoxyethylene ether and the anionic-nonionic mixed emulsifier is 10:20. The model of the phenyl phenol polyoxyethylene ether is Emulsogen TS 200, from Clariant Chemicals (China) Co., Ltd.
[0050] The fertilizer compatible agent is alkyl ethyl sulfonate, and the model of the alkyl ethyl sulfonate is SYNERM280, from Nanjing Deyi Chemical Co., Ltd.
[0051] The solvent is dimethylformamide.
[0052] The cosolvent is cyclohexanone.
[0053] The embodiment 2 of the present application provides a preparation method of pyraclostrobin and prochloraz microemulsion in another aspect, comprising the following steps:
[0054] (1) The cosolvent and the solvent are added to a preparation kettle, a stirrer is turned on, pyraclostrobin is first added, and stirring is performed until complete dissolution, and then prochloraz heated into a liquid state is added to the preparation kettle for dissolution and mixing;
[0055] (2) The emulsifier and the fertilizer compatible agent are accurately weighed according to the feeding ratio, and then sequentially added to the preparation kettle, and a stirrer is turned on for mixing;
[0056] (3) Deionized water is added to the preparation kettle for mixing for 50 min, and then the pyraclostrobin and prochloraz microemulsion is obtained.
[0057] The time for dissolution and mixing in the step (1) is 60 min.
[0058] The time for mixing in the step (2) is 60 min.
[0059] Embodiment 3
[0060] Embodiment 3 of the present application provides a pyraclostrobin and prochloraz microemulsion, comprising, in percentage by weight: pyraclostrobin 8%, prochloraz 32%, emulsifier 30%, fertilizer compatible agent 8%, solvent 8%, cosolvent 10%, deionized water, and the balance.
[0061] The emulsifier is a combination of anionic-nonionic mixed emulsifier and nonionic emulsifier; the nonionic emulsifier is phenyl phenol polyoxyethylene ether. The anionic-nonionic mixed emulsifier is mixed from alkyl phenol and 4-C10-14-alkyl derivative benzene sulfonate; the HLB value of the anionic-nonionic mixed emulsifier is 13.6, TERMUL 5030, from Nanjing Hensman Chemical Co., Ltd.; the mass ratio of the phenyl phenol polyoxyethylene ether and the anionic-nonionic mixed emulsifier is 14:16. The phenyl phenol polyoxyethylene ether is of the type Emulsogen TS 200, from Clariant Chemicals (China) Co., Ltd.
[0062] The fertilizer compatible agent is alkyl ethyl sulfonate, and the alkyl ethyl sulfonate is of the type SYNERM280, from Nanjing Deyi Chemical Co., Ltd.
[0063] The solvent is dimethylformamide.
[0064] The cosolvent is cyclohexanone.
[0065] Embodiment 3 of the present application provides a preparation method of a pyraclostrobin and prochloraz microemulsion, comprising the following steps:
[0066] (1) adding the cosolvent and the solvent into a preparation kettle, turning on a stirrer, first adding pyraclostrobin, stirring until completely dissolved, and then adding prochloraz heated into a liquid into the preparation kettle for dissolving and mixing;
[0067] (2) accurately weighing the emulsifier and the fertilizer compatible agent according to the feeding ratio, and then adding them into the preparation kettle in sequence, and mixing by turning on the stirrer;
[0068] (3) adding deionized water into the preparation kettle, and mixing for 50 min to obtain the product.
[0069] The dissolving and mixing time in step (1) is 60 min.
[0070] The mixing time in step (2) is 60 min.
[0071] Comparative Example 1
[0072] Comparative Example 1 of the present application provides a pyraclostrobin and prochloraz microemulsion and a preparation method thereof, and the specific implementation manner is the same as that of Embodiment 1, except that the emulsifier is a nonionic emulsifier.
[0073] Comparative Example 2
[0074] Comparative Example 2 of the present application provides a pyraclostrobin and prochloraz microemulsion and a preparation method thereof, the specific embodiment of which is the same as that of Example 1, except that it comprises, by weight percentage: pyraclostrobin 10%, prochloraz 30%, emulsifier 38%, solvent 8%, cosolvent 10%, and deionized water to make up to 100%.
[0075] Performance test method
[0076] (1) According to the standards of GB / T1601-93 "Determination of pH value of pesticides", GB / T28137-2011 "Determination method of persistent foaming property of pesticides", GB / T1603-2001 "Determination method of emulsion stability of pesticides", GB / T19137-2003 "Determination method of low temperature stability of pesticides", GB / T19136-2003 "Determination method of thermal storage stability of pesticides", the appearance, pyraclostrobin mass fraction, prochloraz mass fraction, pH value, emulsion stability, persistent foaming property, low temperature stability and thermal storage stability of the pyraclostrobin and prochloraz microemulsion provided by Example 1 were detected, and the test results all met the requirements, see Table 1.
[0077] Table 1,
[0078]
[0079]
[0080] (2) According to the standards of NY / T1156.2-2006 and NY / T1156.6-2006, the toxicity of pyraclostrobin and prochloraz and their mass ratios of 1:1, 1:2, 1:3, 1:4 and 1:5 to citrus anthracnose was determined by using drug-containing medium method, and the results showed that pyraclostrobin and prochloraz mixed in the above five ratios showed synergistic effect on citrus anthracnose, and the EC 50 values were 1.09 mg / L, 0.85 mg / L, 0.66 mg / L, 0.71 mg / L and 0.68 mg / L, respectively, and the co-toxicity coefficients were 132.38, 147.30, 177.93, 159.46 and 162.60, respectively. Among them, the synergistic effect of the mixture of the two at a ratio of 1:3 was more obvious, and the results are shown in Figure 1 .
[0081] (3) According to the standards of NY / T1156.2-2006 and NY / T1156.6-2006, the toxicity of the mixture of the pyraclostrobin and prochloraz at the mass ratio of 1:1, 1:2, 1:3, 1:4 and 1:5 to Colletotrichum gloeosporioides was determined by the method of culture medium containing drug. The results showed that the mixture of the pyraclostrobin and prochloraz at the above-mentioned five ratios had synergistic effect on the C. gloeosporioides, and the EC50 values were 0.93 mg / L, 0.75 mg / L, 0.61 mg / L, 0.64 mg / L and 0.60 mg / L, respectively, and the co-toxicity coefficients were 132.93, 142.43, 163.98, 150.55 and 156.75, respectively. The synergistic effect of the mixture of the pyraclostrobin and prochloraz at the ratio of 1:3 was more obvious, and the results were shown in Table 2. 50 . Figure 2 .
[0082] (4) The pyraclostrobin and prochloraz microemulsion prepared in Example 1 was used for the field efficacy test for the wheat scab, and the method and results were shown in Table 3. Figure 3 .
[0083] (5) The 200-fold dilution stability and 20-fold dilution stability of the pyraclostrobin and prochloraz microemulsion prepared in Example 1 were tested under the conditions of well water, tap water, potassium dihydrogen phosphate solution, standard hard water (hardness of 342 ppm), 2 times hard water, 5 times hard water and 10 times hard water, and the results were shown in Table 4a-g and Table 4a-g. Figure 4 . Figure 5 The results showed that the 200-fold dilution stability and 20-fold dilution stability of the pyraclostrobin and prochloraz microemulsion prepared in Example 1 were qualified under the conditions of well water, tap water, potassium dihydrogen phosphate solution, standard hard water (hardness of 342 ppm), 2 times hard water, 5 times hard water and 10 times hard water, and no crystal was precipitated.
[0084] (6) The pyraclostrobin and prochloraz microemulsion prepared in Example 1 and Comparative Example 1 was diluted 20 times with standard hard water, and the results were shown in Table 5. Figure 6 .
[0085] (7) The pyraclostrobin and prochloraz microemulsion prepared in Example 1 and Comparative Example 2 was diluted 20 times with potassium dihydrogen phosphate aqueous solution (solute:solvent = 1:20), and the results were shown in Table 6. The pyraclostrobin and prochloraz microemulsion prepared in Example 1 showed homogeneous phase after being diluted with high-concentration potassium dihydrogen phosphate aqueous solution, while the pyraclostrobin and prochloraz microemulsion prepared in Comparative Example 2 showed flocculation after being diluted with high-concentration potassium dihydrogen phosphate aqueous solution. Figure 7 .
Claims
1. A microemulsion of pyraclostrobin and pyrimethanil, characterized in that, By weight percentage, including: pyraclostrobin 5-20%, prochloraz 20-40%, emulsifier 10%-34%, fertilizer compatible agent 6%-10%, solvent 5%-12%, cosolvent 8-15%, deionized water to 100%; The mass ratio of pyraclostrobin and prochloraz is 1:(1-5); The emulsifier is a combination of phenolic polyoxyethylene ether and anionic-nonionic mixed emulsifier, and the mass ratio of the phenolic polyoxyethylene ether and the anionic-nonionic mixed emulsifier is (10-14):(16-20), the HLB value of the anionic-nonionic mixed emulsifier is 13.6, and the model is TERMUL 5030; The model of the phenolic polyoxyethylene ether is Emulsogen TS200; The solvent is dimethylacetamide or dimethylformamide; The cosolvent is at least one of cyclohexanone, N-methyl pyrrolidone and acetone; The fertilizer compatible agent is alkyl ethyl sulfonate, and the model of the alkyl ethyl sulfonate is SYNERM 280.
2. A process for the preparation of a microemulsion of fluazinam and pyraclostrobin according to claim 1, characterized in that, At least the following steps are included: (1) The cosolvent and the solvent are added to the preparation kettle, the stirrer is opened, pyraclostrobin is first added, and then stirred until completely dissolved, and then prochloraz heated into a liquid state is added to the preparation kettle for dissolution and mixing; (2) The emulsifier and the fertilizer compatible agent are accurately weighed according to the feeding ratio and then added to the preparation kettle in sequence, and the stirrer is opened for mixing; (3) The deionized water is added to the preparation kettle and mixed for 30-60 min to obtain the product.
3. Use of a microemulsion of fluazinam and pyraclostrobin according to claim 1, characterized in that, It is used for the prevention and treatment of wheat scab, banana leaf spot, citrus anthracnose, and mango anthracnose.
Citation Information
Patent Citations
Pyraclostrobin and prochloraz compound emulsion in water and preparation method thereof
CN106106491A
A mixture of an agricultural synergist with pyraclostrobin and prochloraz, its preparation and application.
CN107306947B
Pyraclostrobin and prochloraz pesticide mixture
CN101524082A
Composite bactericide comprising prochloraz and use thereof
CN102783496A