Metalaxyl-M and fluazinam compounded granules and preparation method thereof

Abstract

The invention discloses granules compounded by metalaxyl-M and fluazinam and a preparation method of the granules. The metalaxyl-M and fluazinam granule is prepared from the following raw material components in percentage by weight: 0.1 to 10 percent of metalaxyl-M, 0.1 to 10 percent of fluazinam, 1 to 5 percent of synergist, 5 to 10 percent of solvent, 1 to 10 percent of additive, 0.1 to 2 percent of stabilizer and the balance of adsorption carrier. The metalaxyl-M and fluazinam compounded granule disclosed by the invention is simple in preparation method, has the characteristics of full water solubility, good stability, safety and convenience in use and the like, can meet various pesticide application modes such as spraying, drip irrigation, broadcast application, flying prevention and the like at the same time, and has a relatively excellent prevention and treatment effect on diseases such as potato late blight, pepper phytophthora blight and Chinese cabbage clubroot.

Description

Technical Field

[0001] The present invention relates to an agricultural fungicide, in particular to a granule formula containing metalaxyl-M and fluazinam compound and a preparation method thereof. Technical Background

[0002] Metalaxyl-M is an amide fungicide with protective and curative properties. It is absorbed by plant roots, stems, and leaves and, along with water transported through the body, is transferred to various plant organs. It is highly effective against diseases of vegetables, fruit trees, tobacco, oilseed crops, cotton, and grains caused by downy mildew, phytophthora, and pythium.

[0003] Fluazinam is a pyridinamine derivative and a dinitroaniline fungicide with no systemic activity. It is a broad-spectrum, highly effective, and protective fungicide. It has good activity against Alternaria, Phytophthora, Plasmopara, Sclerotinia, and Venturia. It also has good control effects against Botrytis cinerea, which is resistant to benzimidazole and dicarboximide fungicides, and is effective against rice damping-off disease caused by Rhizopus. It also has the ability to control phytophagous mites.

[0004] Thymol is a botanical active ingredient isolated and extracted from the Chinese herb thyme. It is easily degraded in the natural environment, safe for humans and animals, and environmentally friendly. It has a distinct fragrance and possesses insecticidal, bactericidal, and antiseptic properties. As a synergist, thymol exhibits significant synergistic effects when combined with metalaxyl-M and fluazinam, significantly enhancing its bactericidal efficacy.

[0005] Domestic invention patent 201610290212.7 discloses a "fungicide composition containing fluazinam and metalaxyl-M." This formulation also uses granules. According to the patent specification, the process uses brick slag as an adsorption carrier, making the resulting product non-water-soluble and dispersible, limiting it to broadcast application only. Furthermore, the preparation process requires airflow pulverization, followed by granulation and drying, making it complex.

[0006] The present invention overcomes the above shortcomings by compounding metalaxyl-M and fluazinam to prepare granules. A water-soluble filler is used as an adsorption carrier, resulting in good water solubility, dispersion in water without residue precipitation, good efficacy, and a simple production process. The granules can be used for various application methods, including spraying, drip irrigation, broadcasting, and aerial spraying. Compounding metalaxyl-M and fluazinam achieves synergistic effects with different bactericidal mechanisms, expanding the control spectrum. Furthermore, the use of the plant-derived ingredient thymol as a synergist can significantly enhance the bactericidal efficacy of the formulation, effectively delay the development of drug resistance in pathogens, and protect the healthy growth of crops. Summary of the Invention

[0007] The specific technical solutions of the present invention are as follows:

[0008] A granule of metalaxyl-M and fluazinam compound and a preparation method thereof, characterized in that: the granule of metalaxyl-M and fluazinam is prepared by using metalaxyl-M and fluazinam as bactericidal active ingredients, using thymol as a synergist, adding a solvent, an auxiliary agent, a stabilizer and an adsorption carrier

[0009] The weight percentages of the above components are:

[0010] Metalaxyl 0.1-10%;

[0011] Fluazinam 0.1-10%;

[0012] Thymol 1-5%;

[0013] Solvent 4-10%

[0014] Additives 1-10%;

[0015] Stabilizer 0.1-2%;

[0016] The adsorption carrier is replenished to 100%.

[0017] Preferably, the weight percentages of the above components are:

[0018] Metalaxyl 1-5%;

[0019] Fluazinam 1-5%;

[0020] Thymol 2-3%;

[0021] Solvent 4-8%

[0022] Additives 4-8%;

[0023] Stabilizer 0.1-0.5%;

[0024] The adsorption carrier is replenished to 100%.

[0025] The thymol described above is a synergist.

[0026] The solvent mentioned above is one or a combination of more than one of cyclohexanone, ethanol, methanol and sec-butyl acetate.

[0027] The auxiliary agent mentioned above is one or a combination of more than one of alkylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, calcium dodecylbenzenesulfonate, phenylethylphenol polyoxyethylene ether, calcium lignin sulfonate, white carbon black, and alkylphenol formaldehyde resin polyoxyethylene ether.

[0028] The stabilizer mentioned above is one or a combination of more than one of citric acid, triphenylphosphite, butylated hydroxyanisole, butylated hydroxytoluene and tert-butylhydroquinone.

[0029] The above-mentioned adsorption carrier is one or a combination of more than one of amylase polymer, attapulgite, diatomaceous earth and brick slag.

[0030] The preparation method of the present invention comprises the following steps:

[0031] Step (1): Add fluazinam technical and thymol technical to a solvent preheated to 40 degrees Celsius, stir and dissolve at a speed of 200-300 rpm until fluazinam technical and thymol technical are completely dissolved, then add metalaxyl technical and adjuvant and stir and dissolve at a speed of 100-200 rpm until the solution becomes clear and transparent.

[0032] Step (2): Add the adsorption carrier to the mixing agitator, add the liquid medicine to the spraying device, turn on the mixing agitator, and stir at a speed of 100-200 rpm. While the mixing agitator is rotating at a constant speed, turn on the spraying device and aim the nozzle at the adsorption carrier to spray evenly. After the liquid medicine is sprayed, turn off the spraying device and continue to rotate and stir the mixing agitator at a speed of 100-200 rpm for 30 minutes.

[0033] Step (3): Place the carrier that has absorbed the drug solution in step (2) in a 40-50° C. forced air dryer and dry for 30 minutes.

[0034] The invention is used for preventing and treating crop diseases such as potato late blight, pepper blight and cabbage clubroot.

[0035] Advantages of the present invention:

[0036] 1. The control spectrum of metalaxyl-M and fluazinam has been expanded. They are highly active against various diseases caused by downy mildew, phytophthora, pythium, and Plasmopara, and are particularly effective against potato late blight, pepper blight, and cabbage clubroot.

[0037] 2. The formula uses thymol, a botanical ingredient, as a synergist, significantly enhancing the efficacy of the drug. Thymol, a botanical active ingredient isolated and extracted from the Chinese herb thyme, is easily degraded in the natural environment, making it safe for humans and animals and environmentally friendly. It exhibits significant synergistic effects when combined with metalaxyl-M and fluazinam.

[0038] 3. The formula uses water-soluble fillers as adsorption carriers, which have good water solubility, disperse in water without residue precipitation, have good efficacy, do not require air flow crushing and granulation process, and have a simple production process. It can meet the needs of multiple application methods such as spraying, drip irrigation, broadcasting, and aerial spraying, thus saving costs. DETAILED DESCRIPTION

[0039] In order to better understand the essence of the present invention, the technical content of the invention is described in detail with reference to embodiments below, but the present invention is not limited thereto.

[0040] In the present invention, all raw materials involved are commercially available products or obtained by conventional methods in the art. Among them, the auxiliary agents phenylethylphenol polyoxyethylene ether and calcium dodecylbenzenesulfonate were purchased from Jiangsu Kaiyuan Technology Co., Ltd., diatomaceous earth and amylase polymer were purchased from Hebei Jiashili Chemical Co., Ltd., and the synergist thymol was purchased from Shenzhen Guoxin Flavors and Fragrances Co., Ltd.

[0041] Example 1 Indoor toxicity determination of different ratios of metalaxyl-M and fluazinam against potato late blight

[0042] Test Methods: Using the growth rate method, five treatments were prepared. Each treatment contained a 1000 mg / L concentration of the virus-infected culture medium. Each treatment was plated (9 cm diameter) with 20 ml of the virus-infected culture medium. Four replicates were performed, with a control plate containing no inoculation. The prepared potato late blight pathogen was punched into a cake using a 4 mm inner diameter punch. A cake was inoculated in the center of each plate, and the plates were then incubated in a constant temperature incubator at 20-23°C for 10-15 days. The diameter of the colony growth in each treatment was measured using the cross-hatch method, and the relative inhibition rate was calculated to compare the antibacterial efficacy.

[0043] Calculation formula:

[0044] Colony growth diameter (mm) = average colony diameter - 4

[0045] Inhibition growth rate = (control colony growth diameter - treated colony growth diameter) / control colony growth diameter × 100%

[0046] The results are shown in Table 1

[0047] Table 1 Results of indoor toxicity test of different ratios of metalaxyl-M and fluazinam against potato late blight

[0048]

[0049] As can be seen from Table 1, when the ratio of metalaxyl-M to fluazinam is 1:1, the antibacterial effect on potato late blight is the best, with an inhibition rate of 87.97%, which is significantly better than other ratios.

[0050] Example 22% Metalaxyl-Fluazinam Granules

[0051] According to the following weight ratio:

[0052] Metalaxyl 1%;

[0053] Fluazinam 1%;

[0054] Thymol 2%;

[0055] Cyclohexanone: 2%;

[0056] Ethanol: 2%

[0057] Phenethylphenol polyoxyethylene ether 3%;

[0058] Calcium dodecylbenzenesulfonate 1%

[0059] Citric acid 0.1%;

[0060] The amylase polymer was made up to 100%.

[0061] The preparation method of the granules in Example 2 comprises the following steps:

[0062] Step (1): Add fluazinam technical and thymol technical to a solvent preheated to 40 degrees Celsius, stir and dissolve at a speed of 200-300 rpm until fluazinam technical and thymol technical are completely dissolved, then add metalaxyl technical and adjuvant and stir and dissolve at a speed of 100-200 rpm until the solution becomes clear and transparent.

[0063] Step (2): Add the adsorption carrier to the mixing agitator, add the liquid medicine to the spraying device, turn on the mixing agitator, and stir at a speed of 100-200 rpm. While the mixing agitator is rotating at a constant speed, turn on the spraying device and aim the nozzle at the adsorption carrier to spray evenly. After the liquid medicine is sprayed, turn off the spraying device and continue to rotate and stir the mixing agitator at a speed of 100-200 rpm for 30 minutes.

[0064] Step (3): Place the carrier that has absorbed the drug solution in step (2) in a 40-50° C. forced air dryer and dry for 30 minutes.

[0065] Example 34% Metalaxyl-Fluazinam Granules

[0066] According to the following weight ratio:

[0067] Metalaxyl 2%;

[0068] Fluazinam 2%;

[0069] Thymol 2%;

[0070] Cyclohexanone: 3%;

[0071] Ethanol: 2%

[0072] Phenethylphenol polyoxyethylene ether 4.5%;

[0073] Calcium dodecylbenzenesulfonate 1%;

[0074] Citric acid 0.1%;

[0075] The amylase polymer was made up to 100%.

[0076] The preparation method of the granules in Example 3 is the same as that in Example 2.

[0077] Example 46% Metalaxyl-Fluazinam Granules

[0078] According to the following weight ratio:

[0079] Metalaxyl 3%;

[0080] Fluazinam 3%;

[0081] Thymol 2%;

[0082] Cyclohexanone: 4%;

[0083] Ethanol: 2.5%

[0084] Phenethylphenol polyoxyethylene ether 4.5%;

[0085] Calcium dodecylbenzenesulfonate 1.5%

[0086] Citric acid 0.1%;

[0087] The amylase polymer was made up to 100%.

[0088] The preparation method of the granules in Example 4 is the same as that in Example 2.

[0089] Example 58% Metalaxyl-Fluazinam Granules

[0090] According to the following weight ratio:

[0091] Metalaxyl 4%;

[0092] Fluazinam 4%;

[0093] Thymol 2%;

[0094] Cyclohexanone: 4.5%;

[0095] Ethanol: 2.5%

[0096] Phenethylphenol polyoxyethylene ether 5.5%;

[0097] Calcium dodecylbenzenesulfonate 1%;

[0098] Citric acid 0.1%;

[0099] The amylase polymer was made up to 100%.

[0100] The preparation method of the granules in Example 5 is the same as that in Example 2.

[0101] Example 6 10% Metalaxyl-Fluazinam Granules

[0102] According to the following weight ratio:

[0103] Metalaxyl 5%;

[0104] Fluazinam 5%;

[0105] Thymol 2%;

[0106] Cyclohexanone: 5%;

[0107] Ethanol: 3%

[0108] Phenethylphenol polyoxyethylene ether 6%;

[0109] Calcium dodecylbenzenesulfonate 2%;

[0110] Citric acid 0.1%;

[0111] The amylase polymer was made up to 100%.

[0112] The preparation method of the granules in Example 6 is the same as that in Example 2.

[0113] Comparative Example 110% Metalaxyl-Fluazinam Granules

[0114] According to the following weight ratio:

[0115] Metalaxyl 5%;

[0116] Fluazinam 5%;

[0117] Cyclohexanone: 5%;

[0118] Ethanol: 3%

[0119] Phenethylphenol polyoxyethylene ether 6%;

[0120] Calcium dodecylbenzenesulfonate 2%;

[0121] Citric acid 0.1%;

[0122] The amylase polymer was made up to 100%.

[0123] The difference between Comparative Example 1 and Example 6 is that no synergist thymol is added. The preparation method of the granules in Comparative Example 1 is the same as that in Example 2.

[0124] Comparative Example 2: 10% Metalaxyl-Fluazinam Granules

[0125] According to the following weight ratio:

[0126] Metalaxyl 5%;

[0127] Fluazinam 5%;

[0128] Thymol 2%;

[0129] Cyclohexanone: 5%;

[0130] Ethanol: 3%

[0131] Phenethylphenol polyoxyethylene ether 6%;

[0132] Calcium dodecylbenzenesulfonate 2%;

[0133] Citric acid 0.1%;

[0134] Brick slag is added to 100%.

[0135] The difference between Comparative Example 2 and Example 6 is that the amylase polymer is replaced by brick slag.

[0136] The preparation method of the granules in Comparative Example 2 is the same as that in Example 2.

[0137] Comparative Example 3: 10% Metalaxyl-Fluazinam Granules

[0138] According to the following weight ratio:

[0139] Metalaxyl 5%;

[0140] Fluazinam 5%;

[0141] Thymol 2%;

[0142] Ethanol: 4%;

[0143] Calcium lignin sulfonate 6%;

[0144] Silica 2%;

[0145] Citric acid 0.1%;

[0146] Diatomaceous earth to 100%.

[0147] The preparation method of the granules in Comparative Example 3 is as follows: first, the metalaxyl-M solvent is removed by ethanol, then adsorbed by white carbon black, and then the remaining materials are mixed together, pulverized by air flow, granulated, and finally dried to obtain the granules.

[0148] Example 7 Performance Determination of Metalaxyl-Fluazinam Granules

[0149] The performance of the 10% metalaxyl-fluazinam granules of Example 6, Comparative Example 2, and Comparative Example 3 was tested. The results are shown in Table 2.

[0150] Table 2 Performance index test results of 10% metalaxyl-fluazinam granules

[0151]

[0152]

[0153] From the results in Table 2, it can be seen that the water-soluble dispersibility and heat storage stability of Example 6 are better than those of Comparative Examples 2 and 3, and Example 6 can be applied to various application methods such as spraying, drip irrigation, broadcasting, and aerial spraying, while Comparative Example 2 can only be applied to broadcasting, and Comparative Example 3 can only be applied to spraying and broadcasting.

[0154] Example 8 Field efficacy test for preventing and controlling pepper blight

[0155] Experimental location: Chengmai, Hainan

[0156] Test agents: Example 6, Comparative Example 1, 10% metalaxyl-M granules, 10% fluazinam granules, diluted with water to 30 L for conventional spraying. The results are shown in Table 3.

[0157] Table 3: Field efficacy test results for controlling pepper blight

[0158]

[0159] As can be seen from Table 3, the average control effect of Example 6 of the present invention on pepper blight 7 days and 14 days after application is significantly higher than that of other control agents, and has excellent control effect.

[0160] Example 9 Field efficacy test for preventing and treating cabbage clubroot

[0161] Experimental location: Lingshui, Hainan

[0162] Test agents: Example 6, Comparative Example 1, 10% metalaxyl-M granules, 10% fluazinam granules, mixed with soil and spread. The results are shown in Table 4.

[0163] Table 4: Field efficacy test results for controlling cabbage clubroot

[0164]

[0165] As can be seen from Table 4, the average control effect of Example 6 of the present invention on cabbage clubroot 15 days and 30 days after application was significantly higher than that of other control agents, showing excellent control effect.

[0166] The above is a detailed introduction to the metalaxyl-fluazinam granules and the preparation method thereof provided by the present invention. Specific examples are used herein to illustrate the principles and implementation methods of the present invention in detail. The description of the above examples is only intended to help understand the present invention and its core concept, but is not limited thereto.

Claims

1. A granule prepared by compounding metalaxyl-M and fluazinam, characterized in that: The weight percentages of the components are: 0.1-10% of metalaxyl-M, 0.1-10% of fluazinam, 1-5% of synergist, 4-10% of solvent, 1-10% of auxiliary agent, 0.1-2% of stabilizer, and the balance is adsorption carrier.

2. The granules of metalaxyl-M and fluazinam compounded according to claim 1, characterized in that: The weight percentages of the components are preferably: 1-5% of metalaxyl-M, 1-5% of fluazinam, 2-3% of synergist, 4-8% of solvent, 4-8% of auxiliary agent, 0.1-0.5% of stabilizer, and the balance is adsorption carrier.

3. The granules prepared by mixing metalaxyl-M and fluazinam according to claim 1 or 2, characterized in that: Among the weight percentages of the components, the optimal ratio of metalaxyl-M to fluazinam is 1:

1.

4. The granules prepared by compounding metalaxyl-M and fluazinam according to claim 1 or 2, characterized in that: The synergist is thymol.

5. The granules prepared by mixing metalaxyl-M and fluazinam according to claim 1 or 2, characterized in that: The adsorption carrier is an amylase polymer.

6. The granules prepared by mixing metalaxyl-M and fluazinam according to claim 1 or 2, characterized in that: The preparation method of the granules comprises the following steps: Step (1): Add fluazinam technical and thymol technical to a solvent preheated to 40 degrees Celsius, stir and dissolve at a speed of 200-300 rpm until fluazinam technical and thymol technical are completely dissolved, then add metalaxyl technical and adjuvant and stir and dissolve at a speed of 100-200 rpm until the solution becomes clear and transparent. Step (2): Add the adsorption carrier to the mixing agitator, add the liquid medicine to the spraying device, turn on the mixing agitator, and stir at a speed of 100-200 rpm. While the mixing agitator is rotating at a constant speed, turn on the spraying device and aim the nozzle at the adsorption carrier to spray evenly. After the liquid medicine is sprayed, turn off the spraying device and continue to rotate and stir the mixing agitator at a speed of 100-200 rpm for 30 minutes. Step (3): Place the carrier that has absorbed the drug solution in step (2) in a 40-50° C. forced air dryer and dry for 30 minutes.

7. The granules prepared from metalaxyl-M and fluazinam according to claim 1, characterized in that: It can be used to prevent and control crop diseases such as potato late blight, pepper blight and cabbage clubroot.

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