Suspending agent containing cyflumetofen and spirodiclofen and application thereof

Abstract

The invention provides a suspending agent containing cyflumetofen and spirodiclofen and application of the suspending agent. The suspending agent is prepared from the following components in percentage by weight: 10 to 30 percent of cyflumetofen, 10 to 30 percent of spirodiclofen, 1 to 10 percent of wetting dispersant, 0.05 to 0.2 percent of pH regulator, 1 to 7 percent of antifreezing agent, 0.05 to 0.2 percent of xanthan gum, 0.2 to 0.8 percent of magnesium aluminum silicate, 0.05 to 0.2 percent of mildew preventive, 0.05 to 0.2 percent of defoaming agent and the balance of deionized water, wherein the total weight percent of the components is 100 percent. The wetting dispersant is prepared from TERSPERSE 2700 and Atlox4913, and the mass ratio of the TERSPERSE 2700 to the Atlox4913 is (1 to 5) to (1 to 5). According to the suspending agent formula disclosed by the embodiment of the invention, the storage results at different temperatures are relatively good, the particle size increase is relatively small, and the suspension rate is 90% or above. And after heat storage and freeze thawing tests at different temperatures, solidification does not occur after normal-temperature storage, and the storage stability is obviously improved. Field test results show that the 38% cyflumetofen-spirodiclofen SC provided by the invention has a good effect on prevention and treatment of citrus tree red mites, and the stable lasting period is 20-30 days.

Description

Technical Field

[0001] The invention belongs to the field of pesticide preparations, and particularly relates to a suspension containing cyfluthrin and spiroclofonate and an application thereof. Background Art

[0002] Cyflumetofen is a new type of acyl acetonitrile acaricide. It is a non-systemic acaricide with the main mode of action being contact killing. Its mechanism of action is to inhibit mitochondrial protein complex II, hinder electron (hydrogen) transfer, and destroy phosphorylation reactions.

[0003] Spirodiclofen is a tetronic acid acaricide with contact killing effect and no systemic properties. It mainly inhibits fat synthesis and blocks the energy metabolism of mites. It has excellent egg-killing effect and also has a good contact killing effect on young mites.

[0004] Cyflumetofen and spirodiclofen are representative pesticides for the prevention and control of citrus red spiders in production. The two have different mechanisms of action. Mixing can improve the prevention effect and effectively control pest resistance. Shanghai Shengnong, our company, conducted a test on the combined toxicity of cyflumetofen and spirodiclofen on citrus red spiders. Among them, the co-toxicity coefficient of cyflumetofen and spirodiclofen mixed in a ratio of 1:1 was the highest, and the synergistic effect was the most obvious. Among the existing pesticide registrations, Shaanxi Yitianfeng Crop Science and Technology Co., Ltd. registered 400 g / L cyflumetofen·spirodiclofen suspension (mass fraction 37% (cyflumetofen 18.5%, spirodiclofen 18.5%)) for the prevention and control of citrus red spiders; Shanghai Shengnong Biochemical Products Co., Ltd. registered 400 g / L cyflumetofen·spirodiclofen (mass fraction 38% (cyflumetofen 19%, spirodiclofen 19%)) suspension for the prevention and control of citrus red spiders. The existing products have insufficient formulation stability during use, which affects the prevention and control effect of the formulation to a certain extent. Summary of the invention

[0005] The present invention provides a suspension containing cyflumetofen and spiroclofonate and application thereof, and the specific technical scheme is as follows:

[0006] A suspension containing cyflumetofen and spirodiclofen, comprising the following ingredients in percentage by weight: 10-30% of cyflumetofen, 10-30% of spirodiclofen, 1-10% of a wetting and dispersing agent, 0.05-0.2% of a pH regulator, 1-7% of an antifreeze agent, 0.05-0.2% of xanthan gum, 0.2-0.8% of magnesium aluminum silicate, 0.05-0.2% of a mildew preventer, 0.05-0.2% of a defoamer, and up to 100% of deionized water;

[0007] The wetting and dispersing agent consists 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 suspending agent comprises the following ingredients in percentage by weight: 15-25% of cyfluthrin, 15-25% of spirodiclofen, 1-10% of wetting and dispersing agent, 0.05-0.2% of pH regulator, 1-7% of antifreeze agent, 0.05-0.2% of xanthan gum, 0.2-0.8% of magnesium aluminum silicate, 0.05-0.2% of mildew inhibitor, 0.05-0.2% of defoamer, and deionized water to 100%.

[0009] Preferably, the suspending agent comprises the following ingredients in percentage by weight: 19% of cyfluthrin, 19% of spirodiclofen, 1-10% of wetting and dispersing agent, 0.05-0.2% of pH regulator, 1-7% of antifreeze agent, 0.05-0.2% of xanthan gum, 0.2-0.8% of magnesium aluminum silicate, 0.05-0.2% of mildew inhibitor, 0.05-0.2% of defoamer, and deionized water to 100%.

[0010] Preferably, the suspension contains the following ingredients in percentage by weight: 19% of cyfluthrin, 19% of spirocyclofen, 6% of wetting and dispersing agent, 0.1% of pH regulator, 5% of antifreeze agent, 0.16% of xanthan gum, 0.5% of magnesium aluminum silicate, 0.1% of mildew inhibitor, 0.1% of defoamer, and deionized water to 100%; the mass ratio of TERSPERSE 2700 to At l ox 4913 is 1:2.

[0011] In the present invention, the pH regulator is citric acid, the mildew inhibitor is sodium benzoate, the defoaming agent is SAG1572, and the antifreeze agent is propylene glycol.

[0012] The suspending agent provided by the invention is used for preventing and controlling red spider mites on citrus trees.

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

[0014] The storage results of the suspension concentrate formula of the embodiment of the present invention at different temperatures are all good, the particle size growth is small, and the suspension rate is all above 90%. After hot storage and freeze-thaw tests at different temperatures, no solidification occurs when it is transferred to room temperature storage, and the storage stability is significantly improved. The field test results show that the 38% cyfluthrin and spirocyclofen SC provided by the present invention has a good effect on the prevention and control of citrus red spider mites, with a stable lasting period of 20-30 days, and is safe for citrus trees. The drug can be promoted and used as a drug for the prevention and control of citrus red spider mites, and a recommended concentration of 5000-4000 times is used. Use the spray method to apply the drug once at the initial peak period of red spider mites. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 : DSC curves of cyfluthrin (left) and cyfluthrin·spiroclofonate (right, mass ratio 1:1). DETAILED DESCRIPTION

[0016] The present invention can be better understood according to the following examples. However, it is easy for those skilled in the art to understand that the contents described in the examples are only used to illustrate the present invention, and should not and will not limit the present invention described in detail in the claims.

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

[0018] Depend on Figure 1 The DSC test results show that after the mixture of cyflumetofen and spirodiclofen, the initial melting point is 69.75℃, which is 10℃ lower than the melting point of cyflumetofen original drug. The melting point of cyflumetofen is not very high. After compounding with spirodiclofen, the melting point of the mixture is significantly reduced, which is manifested as the processing difficulty of the low melting point suspension: it may melt and paste during sand grinding, making it difficult to sand grind; during hot storage, the original drug may melt, crystallize, and increase in particle size, and may crystallize and precipitate after thermal conversion, and the stability will deteriorate.

[0019] Example 2: Preparation of 38% cyfluthrin and spiroclofonate suspension

[0020] Preparation method: According to the formula, first add part of water, antifreeze, wetting dispersant and part of defoamer, use laboratory dispersing sand mill to shear for 3-5 minutes, then add part of thickener, mildew inhibitor and technical, continue to shear for 5-10 minutes, transfer to laboratory dispersing sand mill for sand milling (material amount: zirconium bead amount = 1:1.2), sand milling time 1.0-1.5h, particle size control D90≤5μm, filter zirconium beads after sand milling, then add remaining thickener, remaining defoamer and remaining water, shear and mix evenly, and perform detection and analysis of various technical indicators.

[0021] Detection method: The mass fraction of active ingredients was determined by HPLC; pH value, suspension rate, pourability, persistent foaming, wet sieving test, low temperature stability and heat storage stability test were all determined according to national standards.

[0022] Suspension Concentrate Formulation Example 1

[0023] Table 1 Suspension agent formulation

[0024] Material Name Example 1 Comparative Example 1 Comparative Example 2 Cyflumetofen / % 19 19 19 Spirodiclofen / % 19 19 19 TERSPERSE 2700 2 6 - Atlox 4913 4 - 6 pH adjuster / % 0.1 0.1 0.1 antifreeze / % 5 5 5 Xanthan gum / % 0.16 0.16 0.16 Magnesium aluminum silicate / % 0.5 0.5 0.5 Antifungal agent / % 0.1 0.1 0.1 Defoaming agent / % 0.1 0.1 0.1 Deionized water / % Up to 100 Up to 100 Up to 100

[0025] Note: pH regulator citric acid, mildew inhibitor sodium benzoate, defoamer SAG1572, antifreeze agent propylene glycol suspension formula index test 1

[0026] Table 2 Suspension Concentrate Formula Index Results

[0027] Indicator testing Example 1 Comparative Example 1 Comparative Example 2 Cyflumetofen content at room temperature / % 19.07 18.97 19.04 Spirodiclofen content at room temperature / % 18.98 18.95 18.90 Suspension rate of cyfluthrin at room temperature / % 98.43 91.38 90.25 Suspension rate of spirodiclofen at room temperature / % 99.64 92.87 91.02 54℃ hot storage cyfluthrin content / % 18.88 18.74 18.83 Spirodiclofen content at 54℃ heat storage / % 18.86 18.71 18.65 54℃ heat storage cyflumetofen suspension rate / % 95.50 88.48 87.91 54℃ hot storage spirodiclofen suspension rate / % 96.79 90.85 90.01 60℃ hot storage cyfluthrin content / % 18.85 18.70 18.81 Spirodiclofen content at 60℃ hot storage / % 18.73 18.60 18.52 60℃ hot storage cyflumetofen suspension rate / % 91.49 82.05 80.16 60℃ hot storage spiroclofen suspension rate / % 93.31 85.91 84.28 Cold storage cyfluthrin content / % 18.89 18.79 18.87 Spirodiclofen content in cold storage / % 18.80 18.75 18.72 Suspension rate of cyfluthrin in cold storage / % 97.69 90.32 89.24 Cold storage spirodiclofen suspension rate / % 99.09 90.97 90.03 Freeze-thaw cyfluthrin content / % 18.90 18.73 18.86 Freeze-thaw spirodiclofen content / % 18.83 18.68 18.70 Freeze-thaw cyfluthrin suspension rate / % 94.99 85.86 86.17 Freeze-thaw spirodiclofen suspension rate / % 96.99 88.25 87.15 Particle size D90 / μm when stored at room temperature 2.982 3.002 2.995 Freeze-thaw storage particle size / μm 8.009 15.40 14.78 Low temperature storage particle size / μm 3.027 4.950 6.601 54℃ thermal storage particle size / μm 4.717 13.982 16.705 60℃ thermal storage particle size / μm 5.411 15.072 18.035 pH 6.37 6.52 6.06 Foaming property(mL) 30 40 45

[0028] Suspension Concentrate Formulation Example 2

[0029] Table 3 Suspension additive formula

[0030]

[0031]

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

[0033] Suspension Concentrate Formula Index Test 1

[0034] Table 4 Suspension Concentrate Formula Index Results

[0035] Indicator testing Comparative Example 3 Comparative Example 4 Content of Cyflumetofen at room temperature % 18.94 19.05 Suspension rate of cyfluthrin at room temperature % 93.48 90.35 Spirodiclofen content at room temperature / % 19.02 18.97 Suspension rate of spirodiclofen at room temperature / % 91.27 90.42 Hot storage cyfluthrin content % 18.86 18.93 Suspension rate of cyfluthrin in hot storage % 90.54 85.54 Spirodiclofen content in hot storage / % 18.89 18.83 Suspension rate of spirodiclofen in hot storage / % 90.52 82.97 Cold storage cyflumetofen content % 18.79 18.99 Suspension rate of cyfluthrin in cold storage % 91.16 87.48 Spirodiclofen content in cold storage / % 18.95 18.87 Cold storage spirodiclofen suspension rate / % 89.53 86.08 pH 6.41 6.35 Persistent foaming mL 45 53 D90 particle size at room temperature / μm 3.038 3.125 Hot storage D90 particle size / μm 9.720 13.144 Cold storage D90 particle size / μm 5.884 8.053

[0036] The storage results of the suspension concentrate of the embodiment of the present invention at different temperatures are good, the particle size growth is small, and the suspension rate is >90%. After hot storage and freeze-thaw tests at different temperatures, no solidification occurs when it is transferred to room temperature storage, and the storage stability is significantly improved.

[0037] Example 3: Field efficacy test of 38% cyfluthrin and spiroclofonate suspension in controlling citrus red spider mites

[0038] Experimental unit: Institute of Plant Protection, Guangxi Academy of Agricultural Sciences

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

[0040] Tested crops: citrus trees

[0041] Target of control: Red spider

[0042] Experimental Design:

[0043] Table 5 Experimental design of test drugs

[0044]

[0045] Application method: Apply the pesticide when the red spider mites are at their peak on citrus trees. First spray a blank control, until the front and back of the leaves are evenly wet and about to drip. Then prepare the pesticide according to the control water volume, and spray the diluted pesticide in a small area.

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

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

[0048] Survey method, time and frequency: before medication and on the 1st, 3rd, 10th, 15th, 20th and 30th days after medication (i.e. September 1st, September 2nd, September 4th, September 11th, September 16th, September 21st and September 30th), for a total of 7 surveys.

[0049] Survey method: In each plot, two trees were surveyed. One tender shoot was marked in each of the five directions of east, west, south, north and center for each tree. The number of active mites on five leaves (50 in total) were surveyed in each direction. The leaf surface was directly observed with a handheld magnifying glass, the number of mites was counted, and the insect population reduction rate and control effect were calculated.

[0050]

[0051] The experimental data were analyzed for significance of differences using Duncan's new multiple range method in DPS (7.05) statistical analysis software.

[0052] Results and analysis:

[0053] The results of the test of 38% cyfluthrin and spiroclofen SC against red spider mites in citrus trees are shown in Table 2. The results of the DMRT test and analysis showed that:

[0054] One day after the application, the protective efficacy of the treatment with 38% cyfluthrin·spirocyclofen SC at 5000 times was significantly lower than that of the control 20% cyfluthrin SC, and had no significant difference from the control 24% spirocyclofen SC; the protective efficacy of the treatments with 38% cyfluthrin·spirocyclofen SC at 4500 times and 4000 times had no significant difference from that of the control 20% cyfluthrin SC, but was significantly higher than that of the control 24% spirocyclofen SC.

[0055] Three days after application, the control efficacy of the two treatments with 38% cyfluthrin·spirodiclofen SC 5000 times and 4500 times was not significantly different from that of the two controls; the control efficacy of the treatment with 38% cyfluthrin·spirodiclofen SC 4000 times was extremely significantly higher than that of the control 20% cyfluthrin SC, and was not significantly different from the control 24% spirodiclofen SC.

[0056] Ten days after the application, the control effect of the treatment with 38% cyfluthrin·spirodiclofen SC 5000 times was not significantly different from that of the two controls; the control effect of the treatment with 38% cyfluthrin·spirodiclofen SC 4500 times was significantly higher than that of the control 20% cyfluthrin SC, and was not significantly different from the control 24% spirodiclofen SC; the control effect of the treatment with 38% cyfluthrin·spirodiclofen SC 4500 times was extremely significantly higher than that of the control 20% cyfluthrin SC, and was not significantly different from the control 24% spirodiclofen SC.

[0057] 15 days after application, the protective effects of the three treatments of 38% cyfluthrin·spiroclofonate SC at 5000 times, 4500 times and 4000 times were significantly higher than that of the control 20% cyfluthrin SC, but there was no significant difference with the control 24% spiroclofonate SC.

[0058] 20 days after application, the efficacy of the two treatments of 38% butyrocyprofen·spirocyclofen SC 5000 times and 4500 times was not significantly different from that of the two controls; the efficacy of 38% butyrocyprofen·spirocyclofen SC 4000 times was extremely significantly higher than that of the two controls.

[0059] 30 days after application, the control effect of the treatment with 38% butyrate·spirodiclofen SC 5000 times was not significantly different from that of the two controls; the control effect of the treatment with 38% butyrate·spirodiclofen SC 4500 times was significantly higher than that of the control 20% butyrate SC, and was not significantly different from the control 24% spirodiclofen SC; the control effect of the treatment with 38% butyrate·spirodiclofen SC 4500 times was extremely significantly higher than that of the two controls.

[0060] Effect on Crops During the entire test period, the 38% cyfluthrin·spirocyclofen SC treatments had no phytotoxic effects on the citrus trees, and the citrus trees grew normally.

[0061] Impact on other organisms

[0062] The survey results show that other pests and non-target organisms occur less frequently, and no obvious effects of the agent on other non-target organisms or concurrent control of other pests were observed.

[0063] Table 6 Test results of 38% cyfluthrin and spiroclofonate SC against red spider mites in citrus trees

[0064]

[0065]

[0066] The above description is only a preferred embodiment of the present invention. For those skilled in the art, appropriate improvements can be made without departing from the raw materials of the present invention, and these improvements are also within the scope of protection of the present invention.

Claims

1. A suspension concentrate comprising cyfluthrin and spiroclofonate, characterized in that: The invention comprises the following ingredients in percentage by weight: 10-30% of cyfluthrin, 10-30% of spirodiclofen, 1-10% of wetting and dispersing agent, 0.05-0.2% of pH adjusting agent, 1-7% of antifreeze agent, 0.05-0.2% of xanthan gum, 0.2-0.8% of magnesium aluminum silicate, 0.05-0.2% of mildew inhibitor, 0.05-0.2% of defoaming agent, and deionized water to 100%; The wetting and dispersing agent consists of TERSPERSE 2700 and Atlox 4913, and the mass ratio of TERSPERSE 2700 to Atlox 4913 is 1-5:1-5.

2. The suspending agent according to claim 1, characterized in that The invention comprises the following ingredients in percentage by weight: 15-25% of cyfluthrin, 15-25% of spirocyclofen, 1-10% of wetting and dispersing agent, 0.05-0.2% of pH adjusting agent, 1-7% of antifreeze agent, 0.05-0.2% of xanthan gum, 0.2-0.8% of magnesium aluminum silicate, 0.05-0.2% of mildewproof agent, 0.05-0.2% of defoaming agent and deionized water up to 100%.

3. The suspending agent according to claim 2, characterized in that The invention comprises the following ingredients in percentage by weight: 19% of cyfluthrin, 19% of spirocyclofen, 1-10% of wetting and dispersing agent, 0.05-0.2% of pH adjusting agent, 1-7% of antifreeze agent, 0.05-0.2% of xanthan gum, 0.2-0.8% of magnesium aluminum silicate, 0.05-0.2% of mildewproof agent, 0.05-0.2% of defoaming agent and 100% of deionized water.

4. The suspension according to claim 3, characterized in that The composition comprises the following ingredients in percentage by weight: 19% of cyfluthrin, 19% of spirodiclofen, 6% of wetting and dispersing agent, 0.1% of pH regulator, 5% of antifreeze agent, 0.16% of xanthan gum, 0.5% of magnesium aluminum silicate, 0.1% of mildew inhibitor, 0.1% of defoamer, and deionized water to 100%; The mass ratio of TERSPERSE 2700 to Atlox 4913 is 1:

2.

5. The suspending agent according to any one of claims 1 to 4, characterized in that The pH adjuster is citric acid, the mildew inhibitor is sodium benzoate, the defoaming agent is SAG1572, and the antifreeze agent is propylene glycol.

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

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