Preparation containing spinetoram and tolfenpyrad and application thereof

Abstract

The invention belongs to the technical field of insecticides, and particularly relates to a preparation containing spinetoram and tolfenpyrad, and the preparation is a microcapsule suspension-suspending agent, a suspending agent, a microemulsion, an emulsion in water, water dispersible granules and wettable powder. The preparation comprises the following components in percentage by weight: 2-6% of spinetoram, 18-26% of tolfenpyrad and 1-5% of a synergist. And the synergist is prepared from dodecyl dimethyl benzyl ammonium chloride, GY-Spry and Silwet L-77. The invention further discloses a preparation method of the synergist. The 26% spinetoram-tolfenpyrad suspending agent prepared by the invention has excellent suspension rate performance, the prepared suspending agent is qualified, and the synergistic agent is added into the microcapsule-suspending agent and the suspending agent, so that the pest control effect of the agent can be remarkably improved, the pesticide dosage is further reduced, and the environmental pollution is alleviated.

Description

Technical Field

[0001] The invention belongs to the technical field of insecticides, and specifically relates to a preparation containing spinetoram and tolfenpyrad and an application thereof. Background Art

[0002] Spinetoram is a new spinosyn insecticide produced by Dow Agrochemicals. Among the spinosyn insecticides, spinetoram is a new and unique active ingredient and a highly effective, broad-spectrum insecticide. It is mainly used to control lepidoptera and thysanoptera larvae, and has a good control effect on vegetable pests such as diamondback moth, beet armyworm, leaf miner, thrips, armyworm, and bean pod borer. It is widely used in the rotation of drug varieties for resistance management of vegetable pests.

[0003] Tolfenpyrad is a new type of pyrazole heterocyclic insecticide and acaricide that can inhibit the oxidative phosphorylation of insects. Its mechanism of action is to affect the mitochondrial electron transport system complex I, thereby hindering the transfer of electrons in the mitochondrial metabolic system, making it impossible for insects to provide and store energy. It is called a mitochondrial electron transport complex inhibitor (MET I) and also has egg-killing, feeding inhibition, and egg-laying inhibition effects.

[0004] Patent document CN104663669A discloses a composite insecticidal composition containing tolfenpyrad and spinetoram and its use, wherein the weight ratio of tolfenpyrad and spinetoram is 0.1-80:0.5-80. The insecticidal composition can produce a high synergistic effect, overcome and delay pest resistance, has a fast insecticidal speed, a long lasting effect, reduces the cost of medication, and has a significantly higher control effect than a single dose. The composite insecticidal composition can control lepidopteran pests occurring on crops, and can be particularly used to control cotton bollworms and stem borers, and its effect is significantly higher than a single dose. The dosage form is an emulsifiable concentrate, a suspension concentrate, an aqueous emulsion, a wettable powder, a microemulsion or a water-dispersible granule.

[0005] The prior art discloses that the combination of spinetoram and tolfenpyrad has a significant synergistic effect, and also discloses a suspension preparation containing spinetoram and tolfenpyrad; however, there is no related research on the synergist of the combination of spinetoram and tolfenpyrad in the prior art, and in actual use, the field control effect of the agent on crop pests still has room for improvement. In recent years, due to the excessive use of pesticides, environmental and ecological problems have become increasingly prominent, so the development and evaluation of new synergistic adjuvants is particularly important. Summary of the invention

[0006] The present invention provides a preparation containing spinetoram and tolfenpyrad and its application. The technical solution of the present invention is:

[0007] A preparation comprising spinetoram and tolfenpyrad, wherein the preparation is a microcapsule suspension-suspension agent, suspension agent, microemulsion, water emulsion, water dispersible granule, or wettable powder; the preparation contains the following components in weight percentages: spinetoram 2-6%, tolfenpyrad 18-26%, and synergist 1-5%;

[0008] The synergist consists of dodecyl dimethyl benzyl ammonium chloride, GY-Spry, and Silwet L-77. Preferably, the mass ratio of dodecyl dimethyl benzyl ammonium chloride, GY-Spry, and Silwet L-77 in the synergist is 1-3:1-3:1-3.

[0009] Preferably, the preparation is a suspension agent or a microcapsule suspension-suspension agent.

[0010] The present invention provides a suspension agent comprising spinetoram and tolfenpyrad, containing the following components in weight percentages: spinetoram 2-6%, tolfenpyrad 18-26%, synergist 1-5%, wetting and dispersing agent 4-12%, thickening agent 0.1-1.5%, suspending agent 0.1-1%, defoaming agent 0.1-1%, antifreeze agent 3-8%, preservative 0.05-0.5%, and deionized water to make up 100%.

[0011] The present invention provides a suspension agent comprising spinetoram and tolfenpyrad, containing the following components in weight percentages: spinetoram 4%, tolfenpyrad 22%, synergist 2-4%, wetting and dispersing agent 4-12%, thickening agent 0.1-1.5%, suspending agent 0.1-1%, defoaming agent 0.1-1%, antifreeze agent 3-8%, preservative 0.05-0.5%, and deionized water to make up 100%.

[0012] The present invention provides a suspension agent comprising spinetoram and tolfenpyrad, containing the following components in weight percentages: spinetoram 4%, tolfenpyrad 22%, synergist 3%, calcium lignosulfonate 2%, sodium dodecyl sulfate 4%, Morwet-D450 2%, xanthan gum 0.2%, magnesium aluminum silicate 0.8%, organic bentonite 0.5%, glycerol 5%, sodium benzoate 0.2%, SAG1572 0.2%, and deionized water to make up 100%; the mass ratio of dodecyl dimethyl benzyl ammonium chloride, GY-Spry, and Silwet L-77 in the synergist is 1:1:1.

[0013] The present invention provides a microcapsule suspension-suspension agent comprising spinetoram and tolfenpyrad, which is prepared by mixing 8% spinetoram microcapsules and 44% tolfenpyrad suspension agent in a mass ratio of 1:1;

[0014] The 8% spinetoram microcapsules contain the following components in weight percentage: spinetoram 8%, solvent oil 200# 12%, calcium lignosulfonate 3%, Tween 80 4%, ethylenediamine 1%, and deionized water to make up 100%;

[0015] The 44% tolfenpyrad suspension contains the following components in weight percentage: tolfenpyrad 44%, synergist 6%, calcium lignosulfonate 4%, sodium dodecyl sulfate 4%, Morwet-D450 3%, xanthan gum 0.4%, magnesium aluminum silicate 0.9%, organic bentonite 0.5%, glycerol 5%, sodium benzoate 0.2%, SAG1572 0.2%, and deionized water to make up 100%; The mass ratio of the synergists dodecyldimethylbenzylammonium chloride, GY-Spry and Silwet L-77 is 1:1:1.

[0016] The use of the suspension agent described in the present invention for controlling diamondback moth, thrips, flea beetle, rust mite, psyllid, tea geometrid, tea green leafhopper, rust mite, psyllid, leaf miner, leaf roller of crops.

[0017] Adopting the above technical solution, the present invention has the following beneficial effects:

[0018] The 26% spinetoram·tolfenpyrad suspension prepared by the present invention has excellent suspension rate performance, and the prepared suspension is qualified; the microcapsule suspension-suspension agent performance of the 26% spinetoram·tolfenpyrad prepared by the present invention is excellent.

[0019] Adding dodecyldimethylbenzylammonium chloride, GY-Spry, and Silwet L-77 alone to the 26% spinetoram·tolfenpyrad suspension can improve the control effect of the medicament on diamondback moth of cabbage, and there are significant differences compared with the formulation without adding synergist, which can significantly improve the control effect of the medicament; After selecting the synergists dodecyldimethylbenzylammonium chloride, GY-Spry and Silwet L-77 with obvious synergistic effects and combining them, the synergistic effect is further improved. When the dosage of the 26% spinetoram·tolfenpyrad suspension is 20 mL / mu, the control effect on diamondback moth of cabbage is 100% 7 days after application. Similarly, the microcapsule suspension-suspension of 26% spinetoram·tolfenpyrad also has excellent control effect on diamondback moth. Specific Embodiments

[0020] The following further explains the specific embodiments of the present invention in conjunction with specific examples.

[0021] Example 1: Preparation of 26% spinetoram·tolfenpyrad suspension

[0022] Test materials:

[0023] Technical ingredients: spinetoram, tolfenpyrad; Wetting and dispersing agents: calcium lignosulfonate, sodium dodecyl sulfate, Morwet-D450; Synergists: octadecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, GY-Spry, Sil wet L-77; Thickeners: magnesium aluminum silicate, xanthan gum; Suspending agents: organic bentonite; Antifreezing agents: glycerol; Preservatives: sodium benzoate; Defoaming agents: SAG1572; Solvents: deionized water;

[0024] Instruments: electronic balance, dispersion sand mill, pH meter, high performance liquid chromatography, laser particle size distribution analyzer, water bath, etc.;

[0025] Preparation method: According to the formula composition, first add part of deionized water, antifreezing agent, preservative, wetting and dispersing agent and part of defoaming agent, shear with a laboratory dispersion sand mill for 5 - 10 min, then add thickener, spinetoram, tolfenpyrad, continue to shear for 10 - 15 min, transfer to a dispersion sand mill for sanding, the sanding time is 1.0 - 1.5 h, the particle size is controlled so that D90 ≤ 5 μm, filter the zirconium beads after sanding, then add the remaining defoaming agent and the remaining deionized water, shear and mix evenly, and conduct detection and analysis of various technical indicators;

[0026] Detection method: The mass fraction of active ingredients is determined by HPLC method; The pH value, suspension rate, pourability, persistent foaming property, wet screening test, low temperature stability and heat storage stability test are all determined according to national standards.

[0027] Screening of suspending agent formula:

[0028] Table 1: Suspending agent formula

[0029]

[0030]

[0031] Results and analysis:

[0032] The 26% spinetoram·tolfenpyrad suspending agent prepared by the present invention has excellent suspension rate performance, and the prepared suspending agent is qualified.

[0033] Table 2: 26% spinetoram·tolfenpyrad suspending agent

[0034]

[0035] Example 2: Preparation of 26% spinetoram·tolfenpyrad microcapsule suspension-suspending agent Preparation of spinetoram microcapsules:

[0036] Formula: 8% spinetoram, 12% solvent oil 200#, 3% calcium lignin sulfonate, 4% Tween 80, 1% ethylenediamine, and deionized water to make up to 100%.

[0037] Preparation of aqueous phase: dissolve calcium lignin sulfonate in deionized water and prepare it as aqueous phase.

[0038] Preparation of oil phase: dissolve spinetoram, Tween 80 and capsule skin material MDI200 in solvent oil 200# to form an oil phase for use. Pour the oil phase into the water phase at a uniform speed under high shear conditions of 8000rpm and shear for 5 minutes to form a stable water-in-oil emulsion at room temperature. Transfer the stable emulsion to a three-necked flask, dissolve the initiator ethylenediamine in deionized water, and drop it into the emulsion at a uniform speed under mechanical stirring at a certain speed. The interfacial polymerization reaction is reacted at a certain temperature for a certain time. After the reaction is completed, spinetoram microcapsules are obtained.

[0039] Tolfenpyrad suspension preparation: Reference Example 1

[0040] Tolfenpyrad 44%, synergist 6%, calcium lignin sulfonate 4%, sodium lauryl sulfate 4%, Morwet-D4503%, xanthan gum 0.4%, magnesium aluminum silicate 0.9%, organic bentonite 0.5%, glycerol 5%, sodium benzoate 0.2%, SAG1572 0.2%, and deionized water to make up 100%; the mass ratio of the synergist dodecyl dimethyl benzyl ammonium chloride, GY-Spry and Sil wet L-77 is 1:1:1.

[0041] Preparation of 26% Spinetoram·Tolfenpyrad Microcapsule Suspension-Suspension Concentrate:

[0042] 8% spinetoram microcapsules: 44% tolfenpyrad suspension = 1:1 (mass ratio). Accurately weigh 8% spinetoram microcapsules: 44% tolfenpyrad suspension and other materials in a beaker, and stir them with a magnetic stirrer to obtain.

[0043] Example 3: Field control effect of 26% spinetoram-toluamide preparation on Plutella xylostella

[0044] Test crops: Cabbage, which grew basically the same and well in the test area;

[0045] Test pest: Diamondback moth

[0046] Test agent: Example 1 formulations 1-9, microcapsule suspension-suspension concentrate in Example 2

[0047] Experimental design: Set up treatment groups and blank control groups, with 4 replicates for each treatment, arranged in random blocks, and set up protection rows around each plot.

[0048] Test method: When applying the pesticide, the diamondback moth in the field is in the peak egg hatching stage to the third instar larvae stage. Use a backpack sprayer to spray evenly according to the designed dosage, with a spray volume of 35L / 667m2.

[0049] Survey method: According to the relevant content of "GB / T17980.13-2000 Pesticide Field Efficacy Test Guidelines (I) Insecticide Control of Lepidoptera Larvae on Cruciferous Vegetables", the number of live larvae on 10 cabbages in each plot was investigated. During the trial period, the survey was conducted twice: the base number of insects was investigated before the application of pesticides, and the number of residual live insects was investigated 7 days after the application of pesticides, and the control effect was calculated.

[0050] Control effect (%) = [1-(number of live insects in the control area before drug administration × number of live insects in the treatment area after drug administration) / (number of live insects in the control area after drug administration × number of live insects in the treatment area before drug administration)] × 100.

[0051] Test results

[0052] As shown in Table 3, compared with the blank control, the addition of octadecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, GY-Spry, and S il wet L-77 to the 26% spinetoram·tofenamide suspension concentrate can improve the control effect of the agent on cabbage diamondback moth, among which formulas 3-5 showed significant differences from formula 1, which can significantly improve the control effect of the agent; formula 2 did not show significant differences from formula 1. After selecting the combination of dodecyl dimethyl benzyl ammonium chloride, GY-Spry and S il wet L-77, which have obvious synergistic effects, the synergistic effect was further improved. When the dosage of 26% spinetoram·tofenamide suspension concentrate was 20 mL / mu, the control effect on cabbage diamondback moth was 100% 7 days after the application.

[0053] Table 3: Field control effect of 26% ethyl spinetoram·tofenamide suspension on cabbage diamondback moth

[0054]

[0055] Finally, it should be noted that the above examples are only some specific embodiments of the present invention. Obviously, the present invention is not limited to the above examples, and there are many variations. All variations that can be directly derived or associated with the content disclosed by a person skilled in the art are considered to be within the scope of protection of the present invention.

Claims

1. A preparation comprising spinetoram and tolfenpyrad, characterized in that: The preparation is a microcapsule suspension-suspension concentrate, a suspension concentrate, a microemulsion, an aqueous emulsion, a water-dispersible granule, and a wettable powder; the preparation contains the following ingredients in percentage by weight: 2-6% spinetoram, 18-26% tolfenpyrad, and 1-5% of a synergist; The synergist consists of dodecyl dimethyl benzyl ammonium chloride, GY-Spry and Silwet L-77.

2. The preparation according to claim 1, characterized in that The mass ratio of the synergist dodecyl dimethyl benzyl ammonium chloride, GY-Spry and Silwet L-77 is 1-3:1-3:1-3.

3. The preparation according to claim 2, characterized in that The preparation is a suspension.

4. The preparation according to claim 2, characterized in that The preparation is a microcapsule suspension-suspension concentrate.

5. The preparation according to claim 3, characterized in that The invention comprises the following ingredients in percentage by weight: 2-6% of spinetoram, 18-26% of tolfenpyrad, 1-5% of synergist, 4-12% of wetting and dispersing agent, 0.1-1.5% of thickener, 0.1-1% of suspending agent, 0.1-1% of defoamer, 3-8% of antifreeze agent, 0.05-0.5% of preservative, and 100% of deionized water; the synergist is composed of dodecyl dimethyl benzyl ammonium chloride, GY-Spry and Silwet L-77.

6. The preparation according to claim 4, characterized in that The method is prepared by mixing 8% spinetoram microcapsules and 44% tolfenpyrad suspension in a mass ratio of 1:1; The 8% spinetoram microcapsules contain the following weight percentage ingredients: spinetoram 8%, solvent oil 200# 12%, calcium lignin sulfonate 3%, Tween 80 4%, ethylenediamine 1%, and deionized water to make up 100%; The tolfenpyrad suspension contains the following ingredients in percentage by weight: 44% tolfenpyrad, 6% synergist, 4% calcium lignin sulfonate, 4% sodium lauryl sulfate, 3% Morwet-D450, 0.4% xanthan gum, 0.9% magnesium aluminum silicate, 0.5% organic bentonite, 5% glycerol, 0.2% sodium benzoate, 0.2% SAG1572, and deionized water to make up 100%; the mass ratio of the synergist dodecyl dimethyl benzyl ammonium chloride, GY-Spry and Silwet L-77 is 1:1:

1.

7. Use of the suspension concentrate according to any one of claims 1 to 6 for preventing and controlling Plutella xylostella, thrips, yellow-striped flea beetle, rust louse, psyllid, tea geometrid, tea green leafhopper, rust louse, psyllid, leaf miner and leaf roller.

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