A flupyradifurone-spirotetramat insecticidal composition and its application

Abstract

This invention discloses an insecticidal composition of flonicamid and spirotetramat, the raw materials of which include at least flonicamid and spirotetramat, wherein the weight ratio of flonicamid to spirotetramat is 2:(1-5). This invention utilizes the synergistic effect of octadecanol polyoxyethylene ether and secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer, which can increase the compatibility of the active ingredients during use and exhibit excellent penetration after application to the surface of plant leaves, resulting in better efficacy against eggplant thrips. Furthermore, the use of polycarboxylate as a dispersant and magnesium aluminum silicate and xanthan gum as thickeners can increase the suspension rate of the flonicamid·spirotetramat suspension and improve the storage stability of the pesticide.

Description

Technical Field

[0001] This invention relates to an insecticidal composition of flonicamid and spirotetramat, specifically to the field of biocides. Background Technology

[0002] Eggplant thrips are a common pest during eggplant growth, feeding on the sap of leaves and young fruits, causing leaf curling, deformed fruits, fruit drop, and fruit blemishes. They also transmit various plant viruses, seriously harming crop production. Flupyradifurone is an insect growth regulator that inhibits feeding; it is systemic and has strong penetration within the plant. Spirotetramat interferes with the synthesis of lipids in pests, leading to larval death and reducing adult reproductive capacity. Flupyradifurone and spirotetramat have different mechanisms of action, exhibiting excellent synergistic effects. Furthermore, their different mechanisms of action effectively delay the development of pesticide resistance and extend the lifespan of the pesticides.

[0003] Chinese invention patent CN201110269576.4 discloses an ultra-low volume liquid containing flonicamid, using low-volatile oil as a solvent. The active ingredient penetrates deep into the leaves, is resistant to rain washout, and has a prolonged residual effect. However, pesticides using oil as a solvent are prone to causing poisoning to workers during application, posing a safety risk. Furthermore, oily solvents are not easily degraded, leading to significant environmental pressure after use. Chinese invention patent CN202111087508.6 discloses a pesticide composition containing spirotetramat and flonicamid. The resulting suspension or water-dispersible granules have significant efficacy against hemiptera or lepidopteran pests. However, it is ineffective against small, well-hidden pests like eggplant thrips, easily leading to high pesticide residues in vegetable plants. Summary of the Invention

[0004] To improve the efficacy of pesticides against eggplant thrips, reduce pesticide dosage, and improve pesticide stability, the first aspect of the present invention provides an insecticidal composition of flonicamid and spirotetramat, wherein the raw materials for preparation include at least flonicamid and spirotetramat, and the weight ratio of flonicamid to spirotetramat is 2:(1-5).

[0005] In a preferred embodiment, the weight ratio of flupyradifurone to spirotetramat is 2:(1-4).

[0006] In a preferred embodiment, the weight ratio of flupyradifurone to spirotetramat is 2:3.

[0007] In a preferred embodiment, the pesticide composition is selected from one of the following formulations: aqueous suspension, emulsion, wettable powder, and water-dispersible granules.

[0008] In a preferred embodiment, the raw materials for preparing the aqueous suspension include, by weight: 1-10 parts of dispersant, 1-5 parts of thickener, 1-3 parts of wetting agent, 1-3 parts of antifreeze agent, 1-2 parts of defoamer, 0.1-0.3 parts of preservative, and water to make up to 100 parts.

[0009] In a preferred embodiment, the mass ratio of flupyradifurone and spirotetramat in the aqueous suspension is 30-50%.

[0010] In a preferred embodiment, the mass ratio of flupyradifurone and spirotetramat in the aqueous suspension is 40%.

[0011] In a preferred embodiment, the wetting agent is selected from one or a combination of several of fatty alcohol polyoxyethylene ether, EO / PO block copolymer, fatty alcohol polyoxyethylene ether sulfate, and fatty alcohol polyoxyethylene ether phosphate.

[0012] In a preferred embodiment, the fatty alcohol polyoxyethylene ether is a long-chain fatty alcohol polyoxyethylene ether with 8-16 carbon atoms.

[0013] In a preferred embodiment, the fatty alcohol polyoxyethylene ether is octadecanol polyoxyethylene ether with a hydroxyl value of 220-260 mg KOH / g.

[0014] In a preferred embodiment, the EO / PO block copolymer is a secondary alcohol fatty alcohol polyoxyethylene ether EO / PO block copolymer. The secondary alcohol fatty alcohol polyoxyethylene ether EO / PO block copolymer is prepared by reacting fatty alcohol with EO ethylene oxide (C2H4O) and PO propylene oxide (C3H6O) in a specific molar ratio.

[0015] In a preferred embodiment, the wetting agent is a combination of octadecanol polyoxyethylene ether and secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer.

[0016] In a preferred embodiment, the weight ratio of the octadecanol polyoxyethylene ether and the secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer is 1:(1-3); more preferably, the weight ratio of the octadecanol polyoxyethylene ether and the secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer is 1:1.

[0017] During the experiment, the applicant discovered that spirotetramat and flonicamid exhibit poor dispersibility in aqueous solutions but are readily soluble in oily solvents. However, using oil as a solvent can easily cause poisoning to workers applying the pesticides, posing a certain health hazard. Therefore, using water as a solvent can significantly reduce the danger of the pesticides. The applicant utilizes the synergistic effect of octadecanol polyoxyethylene ether and secondary fatty alcohol polyoxyethylene ether EO / PO block copolymers, which can increase the compatibility of the active ingredients in aqueous solutions and exhibit excellent penetration after application to plant leaf surfaces, resulting in better efficacy against eggplant thrips. The reason may be that octadecanol polyoxyethylene ether has a longer molecular chain segment, and the weaker polarity of the alkyl chain leads to better compatibility with spirotetramat and flonicamid, thus increasing the dispersion of spirotetramat and flonicamid in liquid formulations. The applicant further discovered that the synergistic effect of octadecanol polyoxyethylene ether and secondary alcohol fatty alcohol polyoxyethylene ether EO / PO block copolymer can extend the efficacy time of the pesticide. This may be because the synergistic effect improves the pesticide's permeability on the plant surface, increasing the amount absorbed and thus resulting in superior application efficacy. Furthermore, the introduction of the secondary alcohol fatty alcohol polyoxyethylene ether EO / PO block copolymer increases the steric hindrance of the group arrangement, forming larger voids between the liquid films and creating smaller dispersed particles, further enhancing the dispersion effect of the suspension. Simultaneously, the weaker liquid film strength between particles reduces foaming and lowers the risk during application.

[0018] In a preferred embodiment, the defoamer is selected from one or a combination of several of polyether defoamers, silicone defoamers, and mineral oil defoamers.

[0019] In a preferred embodiment, the defoamer is an organosilicone defoamer.

[0020] In a preferred embodiment, the dispersant is selected from one or a combination of several of alkyl naphthalene sulfonates, lignin sulfonates, polycarboxylate salts, and phosphate esters.

[0021] In a preferred embodiment, the dispersant is a polycarboxylate.

[0022] In a preferred embodiment, the thickener is selected from one or a combination of several of magnesium aluminum silicate, carboxymethyl cellulose, xanthan gum, bentonite, attapulgite, and talc.

[0023] In a preferred embodiment, the thickener is a combination of magnesium aluminum silicate and xanthan gum. The magnesium aluminum silicate has a particle size of 2000 mesh.

[0024] In a preferred embodiment, the weight ratio of magnesium aluminum silicate to xanthan gum is 1:(0.2-0.8).

[0025] In a preferred embodiment, the weight ratio of magnesium aluminum silicate to xanthan gum is 1:0.5.

[0026] In a preferred embodiment, the antifreeze is an alcohol-based antifreeze, and more preferably, the antifreeze is propylene glycol.

[0027] In a preferred embodiment, the preservative is Kathon.

[0028] A second aspect of the present invention provides a method for preparing an insecticidal composition of flonicamid·spirotetramat, comprising the following steps:

[0029] Flupyradifurone, spirotetramat, dispersant, wetting agent, antifreeze, thickener, defoamer, preservative, and water are added to a shearing reactor. After shearing for 20-40 minutes, the mixture is fed into a sand mill. After sand milling, a suspension containing flupyradifurone and spirotetramat is obtained.

[0030] A third aspect of the present invention provides an application of a flupyradifurone-spirotetramat insecticidal composition, characterized in that it is used to control eggplant thrips and in the control of Solanaceae and Leguminosae vegetables.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] (1) The flupyradifurone-spirotetramat insecticidal composition of the present invention utilizes the synergistic effect of octadecanol polyoxyethylene ether and secondary alcohol fatty alcohol polyoxyethylene ether EO / PO block copolymer, which can increase the compatibility of the active ingredient in the aqueous solution and has excellent permeability after being applied to the surface of plant leaves, and has better efficacy against eggplant thrips.

[0033] (2) The flupyradifurone-spirotetramat insecticidal composition of the present invention uses polycarboxylate as a dispersant and magnesium aluminum silicate and flavonoid gum as thickeners, which can increase the suspension rate of flupyradifurone-spirotetramat suspension and improve the storage stability of the agent.

[0034] (3) The flupyradifurone-spirotetramat insecticidal composition of the present invention can reduce the foaming rate of the suspension during use and improve the safety of use by introducing secondary alcohol fatty alcohol polyoxyethylene ether EO / PO block copolymer and organosilicon defoamer. Detailed Implementation

[0035] Example 1

[0036] A flupyradifurone-spirotetramat insecticidal composition, the raw materials for preparation include, by weight, 16 parts flupyradifurone, 24 parts spirotetramat, 5 parts dispersant, 4 parts thickener, 2 parts wetting agent, 2 parts antifreeze agent, 1 part defoamer, 0.2 parts preservative, and water to make up to 100 parts.

[0037] The dispersant is a polycarboxylate, purchased from BASF, model Sokalan HP.

[0038] The wetting agent is a combination of octadecanol polyoxyethylene ether and secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer in a weight ratio of 1:1. The octadecanol polyoxyethylene ether has a hydroxyl value of 220-260 mgKOH / g and was purchased from Jinan Yongchen Chemical Co., Ltd. The secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer was purchased from Jinen (Guangzhou) New Materials Co., Ltd., model EP5035.

[0039] The defoamer is an organosilicon defoamer, purchased from Daejeon Chemical, model AT-930.

[0040] The thickener is a combination of magnesium aluminum silicate and xanthan gum, wherein the magnesium aluminum silicate has a particle size of 2000 mesh and is purchased from Maclean, and the weight ratio of magnesium aluminum silicate to xanthan gum is 1:0.5.

[0041] The antifreeze is propylene glycol, and the preservative is Kathon.

[0042] A method for preparing an insecticidal composition of flonicamid·spirotetramat includes the following steps:

[0043] Flupyradifurone, spirotetramat, dispersant, wetting agent, antifreeze, thickener, defoamer, preservative, and water are added to a shearing reactor. After shearing for 30 minutes, the mixture is fed into a sand mill. After sand milling, a suspension containing flupyradifurone and spirotetramat is obtained.

[0044] Example 2

[0045] A flupyradifurone-spirotetramat insecticidal composition, with the same steps as in Example 1, except that the wetting agent is a combination of lauryl alcohol polyoxyethylene ether and secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer in a weight ratio of 1:1. The lauryl alcohol polyoxyethylene ether was purchased from Jinan Yongchen Chemical Co., Ltd.

[0046] Example 3

[0047] A flupyradifurone-spirotetramat insecticidal composition, with the same steps as in Example 1, except that the weight ratio of the octadecanol polyoxyethylene ether and the secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer is 3:1.

[0048] Example 4

[0049] A flupyradifurone-spirotetramat insecticidal composition, with the same steps as in Example 1, except that the thickener is a combination of bentonite and xanthan gum.

[0050] Performance testing

[0051] 1. Toxicity Testing: The western flower thrips (Frankliniella occidentalis) was used as the test target. Field-collected nymphs were reared indoors until they reached the second instar. Flupyradifurone technical grade was produced by Jiangxi Huihe Chemical Co., Ltd. (PD20171710); spirotetramat technical grade was produced by Jiangxi Huihe Chemical Co., Ltd. (PD20171529). Flupyradifurone and spirotetramat technical grades were weighed using an electronic balance and dissolved in acetone to prepare single-agent stock solutions. The flupyradifurone and spirotetramat stock solutions were further mixed at ratios of 16:8, 16:16, 16:24, 16:32, and 16:40 to prepare various mixed formulation stock solutions. Based on the preliminary experiment, each stock solution was diluted with 0.1% Tween-80 aqueous solution to prepare five series of drug solutions with mass concentration gradients of 0.5 mg / L, 1 mg / L, 2 mg / L, 4 mg / L, and 8 mg / L, with a blank control included. Fresh eggplant tender leaves were immersed in the test drug solution for 10 seconds, then removed, dried, and placed in a petri dish containing 1% moisturizing filter paper. Test insects were inoculated, with 30 insects per replicate and 4 replicates per treatment. A treatment without the drug was included as a blank control. The test insects were kept and observed under conditions of 25℃, 70% humidity, and a photoperiod of L:D = (16:8) h. The results were investigated 48 hours after treatment (mortality criterion: the insect body could not move when lightly touched with a brush), and the total number of insects and the number of deaths were recorded. The mortality rate was calculated as follows: The calculation is performed as a percentage (%), and the result is rounded to two decimal places: Where: P1—mortality rate, in percentage (%); K—number of dead insects, in heads; N—total number of insects treated, in heads. The test results are shown in Table 1.

[0052] DPS data processing software was used to perform regression analysis on the logarithmic concentrations of each single agent and different ratios of mixtures, as well as the corresponding probability values ​​of mortality, to calculate the LC50 of each agent. 50 The 95% confidence limit and co-toxicity coefficient of the mixture were determined to compare synergistic effects. The test results are shown in Table 2.

[0053] The synergistic effect of the mixture was calculated according to Sun Yunpei's method. That is, the co-toxicity coefficient CTC≤80 showed an antagonistic effect, 80<CTC<120 showed an additive effect, and CTC≥120 showed a synergistic effect.

[0054] Table 1

[0055]

[0056] Table 2

[0057]

[0058] 2. Suspension rate test: The suspension rate of the compositions in Examples 1-4 was tested according to Method 2 of GB / T 14825-2006. The test results are shown in Table 3.

[0059] 3. Appearance test of heat-stored formulations: The appearance of the samples of the compositions in Examples 1-4 after heat storage was tested. The test results are shown in Table 3.

[0060] Table 3

[0061]

[0062]

Claims

1. A flupyradifurone-spirotetramat insecticidal composition, characterized in that, The raw materials for preparation include at least flonicamid and spirotetramat, wherein the weight ratio of flonicamid to spirotetramat is 2:3; The pesticide composition is in the form of an aqueous suspension. The raw materials for preparing the aqueous suspension, by weight, include: 1-10 parts of dispersant, 1-5 parts of thickener, 1-3 parts of wetting agent, 1-3 parts of antifreeze agent, 1-2 parts of defoamer, 0.1-0.3 parts of preservative, and water to make up to 100 parts. The dispersant is a polycarboxylate; the wetting agent is a combination of octadecanol polyoxyethylene ether and secondary fatty alcohol polyoxyethylene ether EO / PO block copolymer, with a weight ratio of 1:1; the hydroxyl value of the octadecanol polyoxyethylene ether is 220-260 mgKOH / g; The defoamer is an organosilicon defoamer; the thickener is a combination of magnesium aluminum silicate and xanthan gum, wherein the particle size of the magnesium aluminum silicate is 2000 mesh, and the weight ratio of magnesium aluminum silicate to xanthan gum is 1:0.5; the antifreeze agent is propylene glycol, and the preservative is Kathon; The aforementioned flupyradifurone·spirotetramat insecticidal composition is used to control eggplant thrips and is also applied to the control of thrips in Solanaceae and Leguminosae vegetables.

2. A method for preparing the insecticidal composition of flonicamid·spirotetramat according to claim 1, characterized in that, Includes the following steps: Flupyradifurone, spirotetramat, dispersant, wetting agent, antifreeze, thickener, defoamer, preservative, and water are added to a shearing reactor. After shearing for 20-40 minutes, the mixture is fed into a sand mill. After sand milling, a suspension containing flupyradifurone and spirotetramat is obtained.

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