Suspending agent containing fluopyram and difenoconazole

Abstract

The invention provides a suspending agent containing fluopyram and difenoconazole. The suspending agent comprises the following components in percentage by weight: 15% of fluopyram, 15% of difenoconazole, 1-3% of a wetting agent, 3.5-5.5% of a dispersing agent, 0.5-2% of a thickening agent, 0.1-1% of a preservative, 2-6% of an anti-freezing agent, 0.1-1% of a defoaming agent and the balance of deionized water. The preparation method comprises the following steps: mixing the polycarboxylate dispersing agent, the EO-PO block copolymer wetting dispersing agent, the macromolecular comb copolymer dispersing agent and the defoaming agent according to the formula, adding deionized water, mixing, dispersing and shearing for 5 minutes, then adding fluopyram and difenoconazole active compounds, continuously shearing for 5 minutes, adding the preservative, the magnesium aluminum silicate and the xanthan gum ethylene glycol dispersion liquid, uniformly stirring, and finally adding the defoaming agent. And shearing for 15 minutes to prepare suspension slurry. And transferring the suspension slurry to a sand mill for cooling and sanding, with the first-stage sanding temperature not exceeding 30 DEG C and the second-stage and third-stage sanding temperatures not exceeding 35 DEG C, thereby preparing the qualified suspension.

Description

Technical Field

[0001] The invention relates to the technical field of pesticides, in particular to a suspension of fluopyram and difenoconazole. Background Art

[0002] At present, suspension concentrates are gradually playing an important role in agricultural pest control. Agricultural suspension concentrates are made by mixing pesticide technical, pesticide adjuvant ingredients and water. Pesticide adjuvants generally include dispersants, wetting agents, thickeners, stabilizers, antifreeze agents and other ingredients.

[0003] When pesticide products are sprayed, wetting agents can reduce the surface tension of pesticide droplets, making it easier for the active ingredients of pesticides to adhere to the target, thereby improving the utilization rate of pesticides. Dispersants play an important role in suspending agents, providing stable electrostatic and steric effects for the suspension system, thereby maintaining the long-term storage stability of the pesticide suspension system. In addition, the adsorption of dispersants on the surface of pesticide particles is a prerequisite for achieving the stability of the suspension system. Selecting the appropriate dispersant combination and ratio is an important step in achieving the stability of the suspension system.

[0004] Luo Qiang (Preparation and Physical and Chemical Stability Study of 20% Fluopyram Suspension Concentrate, 2020) conducted a detailed study on the application of polycarboxylate dispersants and methyl acrylate dispersants in 20% fluopyram suspension concentrate. On this basis, this application optimizes the formulation according to the characteristics and needs of citrus gum disease prevention and control, so that 30% fluopyram·fenpropimorph suspension concentrate has stable physical properties and excellent prevention and control effects. Summary of the invention

[0005] The object of the present invention is to provide a fluopyram and difenoconazole suspension concentrate and a preparation method thereof. The specific technical scheme is as follows:

[0006] A suspension containing fluopyram and difenoconazole, comprising the following ingredients (by weight percentage): 15% fluopyram, 15% difenoconazole, 1-3% wetting agent, 3.5-5.5% dispersant, 0.5-2% thickener, 0.1-1% preservative, 2-6% antifreeze agent, 0.1-1% defoamer, and deionized water is added to 100%. The wetting agent is an EO-PO block copolymer; the dispersant is composed of one or two of polycarboxylate or high molecular comb copolymer; the thickener is magnesium aluminum silicate and xanthan gum; the preservative is 1,2-phenylisothiazoline-3-one; the antifreeze agent is ethylene glycol; and the defoamer is silicone.

[0007] Preferably, the suspension of fluopyram and difenoconazole comprises the following ingredients (by weight percentage): fluopyram 15%, difenoconazole 15%, wetting agent 2%, dispersant 4.5%, thickener 0.65%, preservative 0.1%, antifreeze agent 4.0%, defoamer 0.2%, and deionized water is supplemented to 100%.

[0008] Preferably, the wetting agent EO-PO block copolymer is Ethylan NS 500LQ; the dispersant polycarboxylate is Agrilan 789D; and the polymer comb-like copolymer is Agrilan 855, wherein the ratio of the polycarboxylate dispersant to the polymer comb-like copolymer dispersant is 1.25:1.

[0009] The suspension agent of the present invention is prepared by the following method: dispersant, wetting agent and defoamer are prepared according to the formula, deionized water is added and mixed, dispersed and sheared for 5 minutes, fluopyram and difenoconazole original drugs are added, shearing is continued for 5 minutes, preservative, magnesium aluminum silicate and xanthan gum ethylene glycol dispersion are added, and shearing is continued for 15 minutes to prepare a suspension slurry. The suspension slurry is transferred to a sand mill for cooling and sand milling, the first-stage sand milling temperature does not exceed 30° C., and the second and third-stage sand milling temperatures do not exceed 35° C. to prepare a qualified suspension.

[0010] The suspending agent of the invention is used for preventing and treating citrus resinosis.

[0011] Beneficial technical effects of the present invention:

[0012] The suspension prepared by the invention has excellent physical properties and high stability; the suspension prepared by the invention has excellent prevention and treatment effects. DETAILED DESCRIPTION

[0013] The present invention is further explained below in conjunction with specific implementation methods. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present invention.

[0014] Formulation Examples

[0015] Dispersant polycarboxylate Agrilan 789D, produced by Nouryon Chemicals Ltd.;

[0016] Wetting agent EO-PO block copolymer Ethylan NS 500LQ, produced by Nouryon Chemicals Co., Ltd.

[0017] The dispersant polymer comb copolymer Agrilan 855 was produced by Nouryon Chemicals Ltd.;

[0018] Thickener magnesium aluminum silicate SF-04, produced by Suzhou Guojian Huitou Mineral New Materials;

[0019] Thickener xanthan gum, produced by Zhongxuan Biochemical Co., Ltd.;

[0020] Preservative 1,2-phenylisothiazoline-3-one G20S, produced by Shanghai Bit Biotechnology Co., Ltd.;

[0021] Antifreeze ethylene glycol, produced by Shell;

[0022] Defoaming agent silicone SAG1572, produced by Momentive Silicone Materials Co., Ltd.

[0023] Example 1 Preparation of 30% Fluopyram Difenoconazole Suspension Concentrate

[0024] Prepare according to the proportion (by weight percentage) of the formula in Table 1. Preparation method: Add deionized water to the dispersant, wetting agent and defoamer according to the formula, disperse and shear for 5 minutes, then add fluopyram and difenoconazole technical, continue shearing for 5 minutes, add preservatives, magnesium aluminum silicate and xanthan gum ethylene glycol dispersion, shear for 15 minutes, and prepare a suspension slurry. Transfer the above suspension slurry to a sand mill for cooling and sand milling, control the first-level sand milling temperature not to exceed 30°C, and the second and third-level sand milling temperatures not to exceed 35°C, to prepare a qualified suspension.

[0025] Example 2-9 Preparation of 30% Fluopyram Difenoconazole Suspension Concentrate

[0026] Same as Example 1, the proportions (by weight percentage) of the formula are prepared according to Table 1.

[0027] Table 1 Example formulation

[0028]

[0029] Quality index test method:

[0030] The content of active ingredients is determined according to HPLC; the pH value is determined according to GB / T1601-1993; the suspension rate is carried out according to GB / T14825-2006; the pourability test is carried out according to GB / T31737-2015; the wet sieving test is carried out according to GB / T16150-1995; the persistent foaming test is carried out according to GB / T28137-2011; the low temperature stability test is carried out according to GB / T19137-2003; and the hot storage stability test is carried out according to GB / T19136-2003.

[0031] Table 2 Quality index test results of Examples 1-9

[0032]

[0033] The quality test results in Table 2 show that Examples 1-9 have reached the corresponding quality standards in terms of pH value, suspension rate, pourability, persistent foaming, low temperature stability, and heat storage stability. The suspension rates of fluopyram and difenoconazole in Example 2 are significantly higher than those in other examples. When the dispersant Agrilan 789D of Example 2 is 2.5% by weight and Agrilan 855 is 2% by weight, it is better than the formula of a single dispersant and can significantly improve the suspension rate of the preparation. The comparison of Examples 2, 6, and 7 shows that when the weight percentage of the wetting agent Ethylan NS 500LQ is 2%-3%, the product quality is qualified. Taking all factors into consideration, when the weight percentage of the composite dispersant Agrilan 789D is 2.5%, the weight percentage of Agrilan 855 is 2%, and the weight percentage of the wetting agent Ethylan NS 500LQ is 2%, the performance of the preparation is significantly better than that of other example formulas.

[0034] Biological Examples

[0035] Test name: Field efficacy test of 30% fluopyram·difenoconazole suspension for the control of citrus gum disease

[0036] Test period: May 26, 2022 - June 25, 2022

[0037] Test crops: citrus trees

[0038] Target: Citrus resin fungus (Phomopsis cytosporella)

[0039] Test reagents:

[0040] 30% Fluopyram·Difenoconazole SC prepared in Examples 1, 2, 5, 7, 8, 9

[0041] Test site and cultivation: Grape Town, Yangshuo County, Guilin City, Guangxi, the orchard has good drainage and irrigation conditions and a high level of management. The planted citrus trees have citrus resin disease all year round. The test fruit trees are growing well, and the planting specifications are 3.0 meters × 4.0 meters. The cultivation conditions (soil type, water and fertilizer management, transplanting period, planting density, growth period, water layer management) of all test plots in the test orchard are uniform.

[0042] Application method: Use spraying method to evenly apply the pesticide to the citrus trees, and fully wet the 30% fluopyram·difenoconazole suspension water. The appropriate application period is before the onset of citrus gum disease or in the early stage; the dosage is 75 mg / kg of active ingredient (i.e. 4000 times diluted liquid), and the water consumption is 1500L / hm 2 .

[0043] Survey time and frequency: This experiment conducted 3 surveys. The first survey was the base number survey before the application of pesticides. The second survey was conducted on June 10, 15 days after the first application of pesticides, to investigate the control effect. The third survey was conducted on June 25, 15 days after the second application of pesticides, to investigate the control effect.

[0044] Methodology:

[0045] Since the fruit was not diseased during the experiment, only the disease condition of the leaves was investigated. Two plants were investigated in each plot, and samples were taken from five points in the east, west, south, north and center of each plant. Two branches were investigated at each point, and four leaves under the top leaf of each branch were investigated. Leaf grading standard:

[0046] Level 0: no disease;

[0047] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0048] Level 3: The lesion area accounts for 6% to 10% of the entire leaf area;

[0049] Level 5: The lesion area accounts for 11% to 25% of the entire leaf area;

[0050] Level 7: The lesion area accounts for 26% to 50% of the entire leaf area;

[0051] Level 9: The lesion area accounts for more than 51% of the entire leaf area.

[0052] Calculation method of drug efficacy:

[0053]

[0054]

[0055] CK0 and Pt0 are the diseased indices of the blank control area and the drug-treated area before medication, respectively; CK1 and Pt1 are the diseased indices of the blank control area and the drug-treated area after medication, respectively.

[0056] Table 3 The efficacy of each agent in preventing citrus gum disease

[0057]

[0058] Note: The efficacy in the table was analyzed by variance analysis using Duncan's new multiple range method in DPS7.05 software. Different uppercase and lowercase letters indicate significant differences at the 1% and 5% levels, respectively.

[0059] Conclusion: All formulations of 30% fluopyram·difenoconazole suspension concentrate have good control effects on citrus gum disease, among which Example 2 (Agrilan 789D (weight percentage 2.5%), Agrilan 855 (weight percentage 2%), and wetting agent Ethylan NS 500LQ (weight percentage 2%)) have the highest control effect on citrus gum disease. Moreover, this formulation is safe for citrus at the dosage provided, and has no obvious adverse effects on other organisms, and can be used to control citrus gum disease.

[0060] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the technical solutions of the embodiments of the present invention.

Claims

1. A suspension containing fluopyram and difenoconazole, comprising the following ingredients (by weight percentage): fluopyram 15%, difenoconazole 15%, wetting agent 1-3%, dispersant 3.5-5.5%, thickener 0.5-2%, preservative 0.1-1%, antifreeze 2-6%, defoamer 0.1-1%, and deionized water is added to 100%. The wetting agent is EO-PO block copolymer; the dispersant is composed of one or two of polycarboxylate or high molecular comb copolymer; the thickener is magnesium aluminum silicate and xanthan gum; the preservative is 1,2-phenylisothiazoline-3-one; the antifreeze is ethylene glycol; the defoamer is silicone.

2. The suspending agent according to claim 1, characterized in that The wetting agent EO-PO block copolymer is EthylanNS 500LQ; the dispersant polycarboxylate is Agrilan 789D; the polymer comb-like copolymer is Agrilan 855, wherein the ratio of the polycarboxylate dispersant to the polymer comb-like copolymer dispersant is 1.25:

1.

3. The suspending agent according to any one of claims 1 to 2, characterized in that The wetting agent EO-PO block copolymer is Ethylan NS 500LQ; the dispersant polycarboxylate is Agrilan 789D; the polymer comb-like copolymer is Agrilan 855, wherein the ratio of the polycarboxylate dispersant to the polymer comb-like copolymer dispersant is 1.25:

1.

4. The suspending agent according to any one of claims 1 to 3, characterized in that Dispersant, wetting agent and defoamer are prepared according to the formula, added to deionized water and mixed, dispersed and sheared for 5 minutes, then fluopyram and difenoconazole technical are added, and shearing is continued for 5 minutes, and preservatives, magnesium aluminum silicate and xanthan gum ethylene glycol dispersion are added, and shearing is carried out for 15 minutes to prepare a suspension slurry. The above suspension slurry is transferred to a sand mill for cooling and sand milling, and the first-level sand milling temperature does not exceed 30°C, and the second and third-level sand milling temperatures do not exceed 35°C to prepare a qualified suspension.

5. Use of the suspension concentrate according to any one of claims 1 to 3 for preventing and treating citrus gum disease.

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