An insecticidal microemulsion composition

Abstract

This invention provides an insecticidal microemulsion composition of flonicamid and spinosad, which can be used to control various pests such as aphids, leafhoppers, planthoppers, and thrips, and is particularly effective against eggplant thrips. The addition of polyether-modified organosilicon as a synergist significantly enhances the efficacy of the flonicamid and spinosad microemulsion. The polyether-modified organosilicon also reduces the persistent foaming of the pesticide, preventing foaming and thus reducing its effectiveness.

Description

Technical Field

[0001] This invention relates to the field of pesticide formulations, and in particular to an insecticidal microemulsion composition of flupyradifurone and spinosad. Background Technology

[0002] Currently, pests and diseases are one of the main factors affecting crop yields. In agricultural production practices, the application of chemical agents remains the most effective means of controlling crop pests and diseases. However, the use of chemical agents to control crop pests and diseases can have serious impacts on the ecological environment: on the one hand, the large-scale application of chemical agents can easily lead to pesticide residues, causing serious pollution to the air, water, and soil; on the other hand, long-term, high-dose application of single chemical agents can easily lead to pesticide resistance in plant pathogens and pests, and also affect the survival of natural enemies. Several technical means can be used to mitigate or overcome these problems, such as using green and environmentally friendly pesticide formulations, reducing the use of toxic volatile organic solvents, and extending the effective period; conducting rational pesticide compounding to broaden the control spectrum and improve control efficacy, thereby reducing the amount of pesticide used, lowering pesticide residues, and delaying the occurrence and development of pesticide resistance in target organisms.

[0003] Therefore, developing pesticide compound formulations with excellent pest and disease control effects and green environmental protection characteristics remains a major task for pesticide technicians in the field.

[0004] Flupyradifurone, also known as flonicamid, is a nicotinamide insecticide developed by Ishihara Sangyo Co., Ltd. of Japan. Its structural formula is as follows:

[0005]

[0006] Flupyradifurone has the molecular formula C9H6F3N3O and a relative molecular weight of 229.2. Its chemical name is N-cyanomethyl-4-(trifluoromethyl)nicotinamide. It is soluble in water and readily soluble in organic solvents such as methanol and acetone. Flupyradifurone works by inhibiting the sucking action of pests; after ingesting the pesticide, pests quickly stop sucking and eventually starve to death. It is effective against various piercing-sucking pests and has good penetrating properties. Flupyradifurone can be formulated into water-dispersible granules, suspensions, and other formulations.

[0007] Ethyl spinosad, also known as spinosad, is a macrocyclic lactone compound developed by Dow AgroSciences (now Corteva). Its structural formula is as follows:

[0008]

[0009] Ethyl spinosad is mainly composed of ethyl spinosad-J (sp i netoram-J, 75.5%), with the molecular formula C. 42 H69 NO 10 ) and ethyl spinosad-L (sp i netoram-L, 20.7%, molecular formula C 43 H 69 NO 10 This mixture consists of two substances with similar physicochemical properties; both are sparingly soluble in water but readily soluble in organic solvents such as methanol, ethyl acetate, and xylene. Ethyl spinosad stimulates the central nervous system of pests, causing non-functional muscle contractions, tremors, and exhaustion. Prolonged over-excitation leads to neuromuscular fatigue and ultimately death. It has both stomach poison and contact action and can be used to control lepidopteran pests such as the diamondback moth, beet armyworm, and rice leaf roller, as well as thrips and other tsioptera. Ethyl spinosad can be formulated into water-dispersible granules and suspensions.

[0010] Microemulsions are environmentally friendly formulations developed by replacing some or all of the organic solvents in emulsifiable concentrates with water. They utilize emulsifiers to uniformly disperse liquid pesticides in water, forming a transparent or semi-transparent O / W state. Microemulsions use a higher amount of surfactant, which can lead to poor low-temperature stability. Furthermore, improper formulation composition can cause emulsion instability, resulting in suspended solids or crystallization in the diluted solution during field application. This can affect pesticide deposition and adhesion on the target, or clog spray nozzles.

[0011] Eggplant thrips are small, reproduce rapidly, and can occur in multiple generations per year with overlapping generations. They lay eggs in stems, leaves, and flowers. Adults and nymphs feed on the sap of the heart leaves, tender stems, and young fruits, and also damage flowers, causing the heart leaves to fail to unfold, young buds to curl, flowers to pollinate poorly, and many deformed fruits. Thrips often hide on the undersides of leaves and in flowers, making them well-concealed. Conventional chemical control methods are generally ineffective.

[0012] Chinese patent application CN201310524629.1 discloses an insecticidal composition of ethyl spinosad and flonicamid, and also discloses various formulations, including microemulsions, and their preparation methods. However, this application only lists the types and content ranges of adjuvants used in various formulations, without specifically disclosing the formulation of any formulation. The examples do not provide specific formulations or related quality indicators for any formulation, and there is no field efficacy data for the ethyl spinosad and flonicamid microemulsion.

[0013] Therefore, it is still necessary to develop pesticide formulations that combine flonicamid and spinosad to meet the needs of thrips control in eggplant. Summary of the Invention

[0014] This invention provides a microemulsion composition of flupyradifurone and spinosad, comprising the following components by weight percentage:

[0015] Flupyradifurone 3-30%, Ethyl spinosad 2-6%, Emulsifier 13-18%, Synergist 2-6%, Organic solvent 43-47%, Water to make up to 100%.

[0016] Preferably, the ratio of flonicamid to spinosad is 5:1 to 1:2.

[0017] Preferably, the emulsifier is one or more of the following: agricultural emulsion series, calcium dodecylbenzenesulfonate, tristyrylphenol polyoxyethylene ether ammonium sulfate, castor oil polyoxyethylene ether phosphate, isotridecyl alcohol polyoxyethylene ether, and nonylphenol polyoxyethylene ether.

[0018] Preferably, the synergist is a polyether-modified organosilicon.

[0019] Preferably, the organic solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate, N-formylmorpholine, N,N-dimethyldecylamide, and N-methylpyrrolidone.

[0020] The insecticidal microemulsion composition of the present invention is prepared by the following method:

[0021] First, dissolve flonicamid and spinosad in an organic solvent and stir until homogeneous; then add emulsifiers and synergists to form an emulsion; finally, add water to make the finished product and test it.

[0022] By adopting the above technical solution, the present invention has the following beneficial effects:

[0023] (1) The insecticidal microemulsion composition of the present invention can be used to control a variety of pests such as aphids, leafhoppers, planthoppers, and thrips, among which it is particularly effective against eggplant thrips. Eggplant thrips have overlapping generations and are good at hiding. Both flonicamid and spinosad have stomach poison and contact action, as well as systemic action, and have diverse modes of action, which can effectively solve the problem of eggplant thrips' good concealment and difficulty in pesticide penetration, thus achieving efficient control.

[0024] (2) The addition of polyether-modified organosilicon as a synergist in this invention significantly improves the efficacy of the combined microemulsion of flonicamid and spinosad. In the prior art, numerous pesticide synergists exist, but not all pesticide active ingredients or formulations are suitable. This invention specifically selects polyether-modified organosilicon, which can significantly improve the insecticidal effects of flonicamid and spinosad. Surprisingly, polyether-modified organosilicon also reduces persistent foaming of the pesticide. Excessive foaming increases the difficulty of pesticide spraying, affects the normal operation of spraying equipment (e.g., clogging nozzles), and also affects the pesticide's coverage and adhesion, resulting in uneven adhesion of the pesticide to crops or pests, thus reducing the pesticide's effectiveness. Attached Figure Description

[0025] Figure 1 This is a flowchart illustrating the preparation process of the insecticidal microemulsion composition of the present invention. Detailed Implementation

[0026] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0027] Example 1: 20% Flupyradifurone·Ethyl Spondioxin Microemulsion

[0028] The present invention will be further explained below with reference to specific embodiments.

[0029]

[0030]

[0031] The preparation method is as follows:

[0032] Flupyradifurone, spinosad, butyl acetate, N-formylmorpholine, and N,N-dimethyldecylamide were mixed and stirred until homogeneous.

[0033] Calcium dodecylbenzenesulfonate, tristyrylphenol polyoxyethylene ether ammonium sulfate, isotridecyl alcohol polyoxyethylene ether, and polyether-modified organosilicon are added to form an emulsion.

[0034] Add water to make the finished product.

[0035] Comparative Example 1:

[0036] Comparative Example 1 product was prepared according to the formulation and preparation method of Example 1, except that modified soybean oil (Fengbei) was added as a synergist.

[0037] Comparative Example 2:

[0038] Comparative Example 2 was prepared according to the formulation and preparation method of Example 1, except that polyether-modified organosilicon was not added.

[0039] Multiple batches of the example and comparative products were prepared and their quality indicators were tested. The relevant data are shown in the table below:

[0040]

[0041]

[0042] In Comparative Examples 1 and 2, polyether-modified silicone was not added, which had an impact on the persistent foaming property and did not meet the requirement of ≤50 mL. There were no significant differences in other quality indicators. Without being bound by any theory, the inventors believe that polyether-modified silicone may play a certain defoaming role.

[0043] Example 2: Bioassay Experiment

[0044] Referring to the bioassay standard method NY / T1154.1 - 2006, the drop method was used: Thrips on eggplant leaves were collected and placed in a glass tube for standby. After anesthetizing the eggplant thrips with ether, thrips with the same instar were selected and placed in a petri dish. The thrips in the dish were dropped with 0.1 μL each using a micro-drop pipette. After the treatment, they were put into fresh eggplant leaves for feeding. 20 thrips were dropped for each treatment, with 4 replicates set, and a treatment with the corresponding organic solvent without the药剂 was set as a control.

[0045] One day later, the experimental data were statistically analyzed, and the mortality rate (%) and corrected mortality rate (%) were calculated. If the control mortality rate < 5%, no correction was needed; if the control mortality rate was between 5% - 20%, correction was needed; if the control mortality rate > 20%, the experiment needed to be redone. Taking the logarithm of the药剂 concentration (mg / L) as the independent variable x and the probit value of the corrected mortality rate as the dependent variable y, the toxicity regression equations were established respectively, and the EC50 of the single agent and each formulated mixture and the co-toxicity coefficient of the formulated mixture were calculated using DPS software. The co-toxicity coefficient method (CTC) was used to evaluate the interaction of the药剂 mixtures, that is, CTC ≤ 80 was antagonistic effect, 80 < CTC < 120 was additive effect, and CTC ≥ 120 was synergistic effect.

[0046] The experimental data are shown in the following table

[0047] EC50 ATI TTI CTC Ethyl spinosad 0.248 100 Flupyradifurone 1.758 14.11 2:1 0.259 95.75 71.37 134.17 1:1 0.284 87.32 57.05 153.06 1:2 0.397 62.47 42.74 146.17 1:3 0.506 49.01 35.58 137.75 1:4 0.532 46.62 31.29 149.00 1:5 0.620 40.00 28.42 140.73

[0048] Thus, it can be seen that when the ratio of flonicamid to spinetoram is within the range of 5:1 - 1:2, the co-toxicity coefficient is greater than 120, and a synergistic effect can be produced.

[0049] Example 3: Field Experiment

[0050] Experiment time and location: In the middle of March, it was carried out in a vegetable base greenhouse in Shouguang City, Shandong Province.

[0051] Test药剂: The 20% flonicamid·spinetoram microemulsion prepared in Example 1 of this application, the control药剂 of Comparative Examples 1 and 2, and a water control.

[0052] Experiment method: A total of 12 plots were set, arranged in a randomized block design, and the plot area was 20m 2Example 1, Comparative Examples 1 and 2, and the water control were each repeated three times. The pesticide was applied by spraying, with 30 ml of the microemulsion diluted in 50 kg of water per acre, sprayed onto the eggplant plants. The initial population of eggplant thrips was counted before application, and 1 day and 3 days after application to calculate the control efficacy. The calculation formula is as follows:

[0053]

[0054] Experimental results:

[0055]

[0056] The experimental data above show that the sample in Example 1 of this application has good control efficacy against eggplant thrips, reaching over 75% after one day and nearly 90% after three days. Comparative Examples 1 and 2 showed no significant difference in control efficacy, both around 65%. Although Comparative Example 1 added modified soybean oil as a synergist, it had no effect on the microemulsion of this application. It is worth noting that the pesticides in Comparative Examples 1 and 2 produced a lot of foam when diluted with water, which did not dissipate for a long time. This led to nozzle clogging in the later stages of spraying and caused uneven spraying of the pesticide solution.

[0057] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An insecticidal microemulsion composition, characterized in that, By weight percentage, it contains the following components: flonicamid 3-30%, ethyl spinosad 2-6%, emulsifier 13-18%, synergist 2-6%, organic solvent 43-47%, and water to make up 100%; The ratio of flonicamid to spinosad is 5:1-1:2; The emulsifier is one or more of the following: calcium dodecylbenzenesulfonate, tristyrylphenol polyoxyethylene ether ammonium sulfate, castor oil polyoxyethylene ether phosphate, isotridecyl alcohol polyoxyethylene ether, and nonylphenol polyoxyethylene ether. The synergist is a polyether-modified organosilicon; The organic solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate, N-formylmorpholine, N,N-dimethyldecylamide, and N-methylpyrrolidone.

2. The method for preparing the insecticidal microemulsion composition according to claim 1, characterized in that, Includes the following steps: First, dissolve flonicamid and spinosad in an organic solvent and stir until homogeneous; then add emulsifiers and synergists to form an emulsion; finally, add water to make the finished product and test it.

3. The application of the insecticidal microemulsion composition according to claim 1 or the insecticidal microemulsion composition prepared by the preparation method of claim 2 in the control of crop pests.

4. The application of the insecticidal microemulsion according to claim 3, characterized in that, The crop pests mentioned include aphids, leafhoppers, planthoppers, and thrips.

5. The application of the insecticidal microemulsion according to claim 4, characterized in that, The crop pest in question is the eggplant thrips.

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