A suspension containing cyflumetofen and spirodiclofen and its use

Abstract

The application provides a suspension agent containing butylfluorfon and spirodiclofen and application thereof, the suspension agent contains the following weight percentage ingredients: butylfluorfon 10-30%, spirodiclofen 10-30%, wet dispersant 1-10%, pH regulator 0.05-0.2%, antifreezing agent 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, antifungal agent 0.05-0.2%, defoaming agent 0.05-0.2%, deionized water to 100%; the wet dispersant is composed of TERSPERSE 2700 and Atlox 4913, and the mass ratio of TERSPERSE 2700 and Atlox 4913 is 1-5:1-5. The storage results of the suspension agent formula of the embodiment of the application at different temperatures are all good, the particle size growth is small, and the suspension rate is all above 90%. After the heat storage and freeze-thaw test at different temperatures, no solidification occurs when being transferred to normal temperature storage, and the storage stability is obviously improved. The field test results show that the 38% butylfluorfon and spirodiclofen SC provided by the application has good effect on preventing and treating citrus red mite, and the stable effective period is 20-30 days.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of pesticide preparation, and particularly relates to a suspension concentrate containing cyflumetofen and spirodiclofen and application thereof. BACKGROUND

[0002] Cyflumetofen belongs to a novel acylacetonitrile acaricide, and is a non-systemic acaricide, and the main action mode is contact killing, and the action mechanism is to inhibit mitochondrial protein complex II, hinder electron (hydrogen) transmission, and destroy phosphorylation reaction.

[0003] Spirodiclofen is a quinone acid acaricide, has contact killing action, is non-systemic, mainly inhibits fat synthesis, blocks energy metabolism of mites, has excellent ovicidal effect, and also has good contact killing action on juvenile mites.

[0004] Cyflumetofen and spirodiclofen are representative agents for preventing and treating citrus red mites in production, have different action mechanisms, can improve the prevention effect by mixing, and effectively control pest resistance. Through the joint toxicity determination test of cyflumetofen and spirodiclofen on citrus red mites by Shanghai Shengnong Biochemical Products Co., Ltd., the synergistic effect is the most obvious when cyflumetofen and spirodiclofen are mixed at a ratio of 1:1. The existing pesticide registration of 400 g / L cyflumetofen·spirodiclofen suspension concentrate (mass fraction 37% (cyflumetofen 18.5%, spirodiclofen 18.5%)) for citrus red mite prevention and control is registered by Shanxi Yitian Fengzuo Crop Technology Co., Ltd.; and the existing pesticide registration of 400 g / L cyflumetofen·spirodiclofen (mass fraction 38% (cyflumetofen 19%, spirodiclofen 19%)) suspension concentrate for citrus red mite prevention and control is registered by Shanghai Shengnong Biochemical Products Co., Ltd. The existing product has insufficient preparation stability when in use, thereby affecting the preparation prevention and control effect to a certain extent. SUMMARY

[0005] The present application provides a suspension concentrate containing cyflumetofen and spirodiclofen and application thereof, and the specific technical solutions are as follows:

[0006] A suspension concentrate containing cyflumetofen and spirodiclofen comprises the following components in weight percentage: cyflumetofen 10-30%, spirodiclofen 10-30%, wetting dispersant 1-10%, pH regulator 0.05-0.2%, antifreezing agent 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, antifungal agent 0.05-0.2%, defoaming agent 0.05-0.2%, and deionized water to 100%.

[0007] The wetting dispersant is composed of TERSPERSE 2700 and Atl ox 4913, and the mass ratio of TERSPERSE 2700 to Atl ox 4913 is 1-5:1-5.

[0008] Preferably, the suspension agent comprises the following ingredients by weight percentage: butiflucymate 15-25%, spirodiclofen 15-25%, wetting dispersant 1-10%, pH regulator 0.05-0.2%, anti-freezing agent 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, anti-mildew agent 0.05-0.2%, defoaming agent 0.05-0.2%, and deionized water to 100%.

[0009] Preferably, the suspension agent comprises the following ingredients by weight percentage: butiflucymate 15-25%, spirodiclofen 15-25%, wetting dispersant 1-10%, pH regulator 0.05-0.2%, anti-freezing agent 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, anti-mildew agent 0.05-0.2%, defoaming agent 0.05-0.2%, and deionized water to 100%.

[0010] Preferably, the suspension agent comprises the following ingredients by weight percentage: butiflucymate 15-25%, spirodiclofen 15-25%, wetting dispersant 1-10%, pH regulator 0.05-0.2%, anti-freezing agent 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, anti-mildew agent 0.05-0.2%, defoaming agent 0.05-0.2%, and deionized water to 100%.

[0011] In the present application, the pH regulator is citric acid, the anti-mildew agent is sodium benzoate, the defoaming agent is SAG1572, and the anti-freezing agent is propylene glycol.

[0012] The suspension agent provided by the present application is used for preventing and treating red spider mites of citrus trees.

[0013] Compared with the prior art, the present application has the following beneficial effects:

[0014] The storage results of the suspension agent formula of the present application at different temperatures are good, the particle size growth is small, and the suspension rate is more than 90%. After the hot storage and freeze-thaw test at different temperatures, no solidification occurs when stored at room temperature, and the storage stability is obviously improved. The field test results show that the 38% butiflucymate·spirodiclofen SC provided by the present application has good effect on preventing and treating red spider mites of citrus trees, the stable effective period is 20-30 days, and it is safe to citrus trees. The drug can be used as a pesticide for preventing and treating red spider mites of citrus trees, and the recommended use concentration is 5000-4000 times. The spraying method is used for spraying once at the initial peak period of red spider mites. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 DSC curve of butiflucymate (left) and butiflucymate·spirodiclofen (right, mass ratio 1:1). DETAILED DESCRIPTION

[0016] The application can be better understood from the following examples. However, it will be readily apparent to those skilled in the art that the examples described are for illustrative purposes only and should not be used to limit the present application as described in the claims.

[0017] Example 1: DSC test of the original drug melting point

[0018] From Figure 1 The DSC test results show that the initial melting point of the mixture of butylfluorfon and spirodiclofen is 69.75°C, which is 10°C lower than the melting point of butylfluorfon. The melting point of butylfluorfon is not very high, and after compounding with spirodiclofen, the melting point of the mixture is significantly reduced, which shows the processing difficulty of low melting point suspension concentrate: it may melt and paste during sanding, and it is difficult to sand; the original drug may melt, crystallize and increase in particle size during hot storage, and after heat transfer, it may crystallize, precipitate and have poor stability.

[0019] Example 2: Preparation of 38% butylfluorfon and spirodiclofen suspension concentrate

[0020] Preparation method: according to the formula composition, first add part of water, antifreeze, wetting dispersant and part of defoamer, use laboratory dispersion sand mill to shear for 3-5 min, then add part of thickening agent, antifungal agent and original drug, continue to shear for 5-10 min, then transfer to laboratory dispersion sand mill for sanding (material amount: zirconium bead amount = 1:1.2), sanding time 1.0-1.5 h, particle size control D90≤5 μm, filter zirconium beads after sanding, then add the rest of the thickening agent, the rest of the defoamer and the rest of the water, shear and mix uniformly, and detect and analyze various technical indexes.

[0021] Detection method: the mass fraction of active ingredient is determined by HPLC method; pH value, suspension rate, pouring property, persistent foaming property, wet sieve test, low temperature stability and hot storage stability test are determined according to national standard.

[0022] Suspension concentrate formula example 1

[0023] Table 1 Suspension concentrate additive formula

[0024] Material name Example 1 Comparative Example 1 Comparative Example 2 Bifenoxate / % 19 19 19 Spirodiclofen / % 19 19 19 TERSPERSE 2700 2 6 - Atlox 4913 4 - 6 pH adjuster / % 0.1 0.1 0.1 Anti-freeze / % 5 5 5 Xanthan gum / % 0.16 0.16 0.16 Veegum / % 0.5 0.5 0.5 Mold inhibitor / % 0.1 0.1 0.1 Defoamer / % 0.1 0.1 0.1 Deionized water / % To 100 To 100 To 100

[0025] Note: pH regulator citric acid, antifungal agent sodium benzoate, defoamer SAG1572, antifreeze propylene glycol Suspension concentrate formula index test 1

[0026] Table 2 Suspension concentrate formula index results

[0027] Indicator test Example 1 Comparative Example 1 Comparative Example 2 Bifenoxate content at room temperature / % 19.07 18.97 19.04 Spirodiclofen content at room temperature / % 18.98 18.95 18.90 Bifenoxate suspension rate at room temperature / % 98.43 91.38 90.25 Spirodiclofen suspension rate at room temperature / % 99.64 92.87 91.02 Bifenoxate content at 54°C heat storage / % 18.88 18.74 18.83 Spirodiclofen content at 54°C heat storage / % 18.86 18.71 18.65 Bifenoxate suspension rate at 54°C heat storage / % 95.50 88.48 87.91 Spirodiclofen suspension rate at 54°C heat storage / % 96.79 90.85 90.01 Bifenoxate content at 60°C heat storage / % 18.85 18.70 18.81 Spirodiclofen content at 60°C heat storage / % 18.73 18.60 18.52 Bifenoxate suspension rate at 60°C heat storage / % 91.49 82.05 80.16 Spirodiclofen suspension rate at 60°C heat storage / % 93.31 85.91 84.28 Bifenoxate content at cold storage / % 18.89 18.79 18.87 Spirodiclofen content at cold storage / % 18.80 18.75 18.72 Bifenoxate suspension rate at cold storage / % 97.69 90.32 89.24 Spirodiclofen suspension rate at cold storage / % 99.09 90.97 90.03 Bifenoxate content at freeze-thaw / % 18.90 18.73 18.86 Spirodiclofen content at freeze-thaw / % 18.83 18.68 18.70 Bifenoxate suspension rate at freeze-thaw / % 94.99 85.86 86.17 Spirodiclofen suspension rate at freeze-thaw / % 96.99 88.25 87.15 D90 particle size at room temperature / pm 2.982 3.002 2.995 D90 particle size at freeze-thaw / pm 8.009 15.40 14.78 D90 particle size at low temperature / pm 3.027 4.950 6.601 D90 particle size at 54°C heat storage / pm 4.717 13.982 16.705 D90 particle size at 60°C heat storage / pm 5.411 15.072 18.035 PH 6.37 6.52 6.06 Foaming (mL) 30 40 45

[0028] Suspension concentrate formula example 2

[0029] Table 3 Suspension concentrate additive formula

[0030]

[0031]

[0032] Note: Comparative Example 3 is a registered product of our company (Diflovidazin 200 g / L, Spirodiclofen 200 g / L, corresponding mass fractions are 19% and 19% respectively)

[0033] Test 1 of the formulation index of the suspension concentrate

[0034] Table 4 Results of the formulation index of the suspension concentrate

[0035] Indicator test Comparative Example 3 Comparative Example 4 Bifenoxate content at room temperature / % 18.94 19.05 Bifenoxate suspension rate at room temperature / % 93.48 90.35 Spirodiclofen content at room temperature / % 19.02 18.97 Spirodiclofen suspension rate at room temperature / % 91.27 90.42 Bifenoxate content at heat storage / % 18.86 18.93 Bifenoxate suspension rate at heat storage / % 90.54 85.54 Spirodiclofen content at heat storage / % 18.89 18.83 Spirodiclofen suspension rate at heat storage / % 90.52 82.97 Bifenoxate content at cold storage / % 18.79 18.99 Bifenoxate suspension rate at cold storage / % 91.16 87.48 Spirodiclofen content at cold storage / % 18.95 18.87 Spirodiclofen suspension rate at cold storage / % 89.53 86.08 PH 6.41 6.35 Persistent foaming (mL) 45 53 D90 particle size at room temperature / pm 3.038 3.125 D90 particle size at heat storage / pm 9.720 13.144 D90 particle size at cold storage / pm 5.884 8.053

[0036] The storage results of the suspension concentrate formulation of the embodiments of the present application are all good at different temperatures, the particle size growth is small, and the suspension rate is > 90%. After the heat storage and freeze-thaw test at different temperatures, no solidification occurs when transferred to normal temperature storage, and the storage stability is obviously improved.

[0037] Example 3: Field efficacy test of 38% diflovidazin and spirodiclofen suspension concentrate for controlling citrus red mite

[0038] Test undertaking unit: Guangxi Zhuang Autonomous Region Academy of Agricultural Sciences, Institute of Plant Protection

[0039] Test pesticide: 38% suspension concentrate (Example 1)

[0040] Test crop: citrus trees

[0041] Control object: red mite

[0042] Test design:

[0043] Table 5 Test design of the test pesticide

[0044]

[0045] Method of application: The pesticide was applied at the initial peak of citrus red mite, the blank control was sprayed first, and the leaves were evenly wetted on both sides until dripping, then the pesticide was diluted according to the amount of water used in the control, and the diluted pesticide was sprayed in the plot.

[0046] Application equipment: Toyota FT-18 type backpack electric sprayer, conical nozzle, nozzle aperture 1.3 mm, average spraying speed 1.1 L / min.

[0047] Application time and frequency: The test was applied once, and the application time was September 1, 2021.

[0048] Investigation method, time and frequency: before and after drug 1, 3, 10, 15, 20, 30 days (i.e. September 1, September 2, September 4, September 11, September 16, September 21, September 30), a total of 7 investigations.

[0049] Investigation method: 2 trees were investigated in each plot, and 1 tender shoot was marked in each of the five directions of east, west, south and north of each tree, the number of active mites on 5 leaves (a total of 50 leaves) in each direction was investigated, the leaves were directly observed with a hand magnifying glass, the number of mites was counted, and the mite population reduction rate and control effect were calculated.

[0050]

[0051] The test data was analyzed for significant difference by Duncan's new multiple range method in DPS (7.05) statistical analysis software.

[0052] Results and analysis:

[0053] The test results of 38% flufoxafofen ester · spirodiclofen SC in preventing and treating citrus red spider mites are shown in Table 2, and the results show that:

[0054] One day after drug, the control effect of 38% flufoxafofen ester · spirodiclofen SC 5000 times treatment was significantly lower than that of the control 20% flufoxafofen ester SC, and there was no significant difference with the control 24% spirodiclofen SC; the control effects of 38% flufoxafofen ester · spirodiclofen SC 4500 times and 4000 times treatments had no significant difference with the control 20% flufoxafofen ester SC, and were significantly higher than the control 24% spirodiclofen SC.

[0055] Three days after drug, the control effects of 38% flufoxafofen ester · spirodiclofen SC 5000 times and 4500 times treatments had no significant difference with the control effects of the two controls; the control effect of 38% flufoxafofen ester · spirodiclofen SC 4000 times treatment was extremely significantly higher than that of the control 20% flufoxafofen ester SC, and had no significant difference with the control 24% spirodiclofen SC.

[0056] Ten days after drug, the control effect of 38% flufoxafofen ester · spirodiclofen SC 5000 times treatment had no significant difference with the control effects of the two controls; the control effect of 38% flufoxafofen ester · spirodiclofen SC 4500 times treatment was significantly higher than that of the control 20% flufoxafofen ester SC, and had no significant difference with the control 24% spirodiclofen SC; the control effect of 38% flufoxafofen ester · spirodiclofen SC 4500 times treatment was extremely significantly higher than that of the control 20% flufoxafofen ester SC, and had no significant difference with the control 24% spirodiclofen SC.

[0057] After 15 days, the control effects of 38% flufoxafoir·spirodiclofen SC 5000 times, 4500 times and 4000 times were significantly higher than that of the control 20% flufoxafoir SC, and had no significant difference with the control 24% spirodiclofen SC.

[0058] After 20 days, the control effects of 38% flufoxafoir·spirodiclofen SC 5000 times and 4500 times had no significant difference with those of the two controls; the control effect of 38% flufoxafoir·spirodiclofen SC 4000 times was significantly higher than those of the two controls.

[0059] After 30 days, the control effect of 38% flufoxafoir·spirodiclofen SC 5000 times had no significant difference with those of the two controls; the control effect of 38% flufoxafoir·spirodiclofen SC 4500 times was significantly higher than that of the control 20% flufoxafoir SC, and had no significant difference with the control 24% spirodiclofen SC; the control effect of 38% flufoxafoir·spirodiclofen SC 4500 times was significantly higher than those of the two controls.

[0060] Effects on crops During the whole test, the 38% flufoxafoir·spirodiclofen SC at various doses had no phytotoxicity to citrus trees, and the citrus trees grew normally.

[0061] Effects on other organisms

[0062] The investigation results showed that other pests and non-target organisms occurred less, and no obvious effects of the pesticide on other non-target organisms or the synergistic effects on other pests were observed.

[0063] Table 6 Test results of 38% flufoxafoir·spirodiclofen SC for controlling red spider mites on citrus trees

[0064]

[0065]

[0066] 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 suspension comprising cyflumetofen and spirodiclofen, characterized in that, The suspension agent comprises the following ingredients by weight percentage: butylfluoride 10-30%, spirodiclofen 10-30%, TERSPERSE 2700 1-10%, Atlox 4913 1-10%, pH regulator 0.05-0.2%, propylene glycol 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, mildewcide 0.05-0.2%, antifoaming agent 0.05-0.2%, deionized water to 100%. The mass ratio of the TERSPERSE 2700 and Atlox 4913 is 1:

2.

2. The suspension concentrate according to claim 1, characterized in that, The suspension agent comprises the following ingredients by weight percentage: butylfluoride 15-25%, spirodiclofen 15-25%, TERSPERSE 2700 1-10%, Atlox 4913 1-10%, pH regulator 0.05-0.2%, propylene glycol 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, mildewcide 0.05-0.2%, antifoaming agent 0.05-0.2%, deionized water to 100%.

3. The suspension concentrate according to claim 2, characterized in that, The suspension agent comprises the following ingredients by weight percentage: butylfluoride 19%, spirodiclofen 19%, TERSPERSE 2700 1-10%, Atlox 4913 1-10%, pH regulator 0.05-0.2%, propylene glycol 1-7%, xanthan gum 0.05-0.2%, magnesium aluminum silicate 0.2-0.8%, mildewcide 0.05-0.2%, antifoaming agent 0.05-0.2%, deionized water to 100%.

4. The suspension concentrate according to claim 3, characterized in that, The suspension agent comprises the following ingredients by weight percentage: butylfluoride 19%, spirodiclofen 19%, TERSPERSE 2700 2%, Atlox 4913 4%, pH regulator 0.1%, propylene glycol 5%, xanthan gum 0.16%, magnesium aluminum silicate 0.5%, mildewcide 0.1%, antifoaming agent 0.1%, deionized water to 100%.

5. The suspension concentrate according to any one of claims 1 to 4, characterized in that, The pH regulator is citric acid, the mildewcide is sodium benzoate, and the antifoaming agent is SAG1572.

6. Use of the suspension agent according to any one of claims 1-4 for controlling red spider mites on citrus trees.

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