High-systemic pyriproxyfen composition as well as preparation method and application thereof

Abstract

The invention provides a high systemic pyriproxyfen composition and a preparation method and application thereof.The composition is prepared from, by weight, 1-20% of pyriproxyfen serving as an active ingredient, 10-50% of rosin-based vegetable oil serving as a synergistic additive and 0-20% of sophorolipid. The permeability of the pyriproxyfen on leaf surfaces and the conductivity of the pyriproxyfen in plants are changed, the conduction of the pyriproxyfen from a pesticide application part to a newborn tissue and a target pest feeding part is promoted, and the quick-acting property, the persistence and the pesticide effect of the preparation are improved.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of pesticide formulations, and particularly relates to a high systemic pyriproxyfen composition and a preparation method and application thereof. BACKGROUND

[0002] Pyriproxyfen is a benzene ether insect growth regulator, a new type of insecticide belonging to juvenile hormone analogues, which has the characteristics of low toxicity, long persistence, safety to crops, low toxicity to fish, and small impact on the ecological environment. It has good control effect on whiteflies, scales, diamondback moth, beet armyworm, corn earworm, pear woodlouse, and thrips, etc. At the same time, it has very good control effect on sanitary pests such as flies and mosquitoes. It can be used to control pests of Homoptera, Thysanoptera, Diptera, and Lepidoptera. Its inhibitory effect on insects is manifested in affecting the molting and reproduction of insects.

[0003] Turpentine oil (pine oil) is a volatile mixture extracted from pine resin, the core component of which is monoterpenes, accounting for about 60-90%. The bicyclic structure and methyl branch chain make it difficult to dissolve in water, but easy to dissolve in lipid substances (such as insect wax layer), and the bicyclic structure can enhance the penetration ability to resin and rubber. Low molecular weight and high vapor pressure support rapid diffusion. The raw material of pine-based vegetable oil solvent is mainly pine resin or pine resin refined pine oil, by-product after pine rosin, and vegetable oil monoalkyl ester, which can be used for the preparation of emulsifiable concentrate, microemulsion, dispersible oil suspension concentrate, and microcapsule suspension concentrate.

[0004] In the prior art, pine-based vegetable oil is mainly used for simple replacement of traditional solvents in emulsifiable concentrate formulations to achieve the purpose of reducing volatility, improving solubility, and improving environmental friendliness. CN119302303A discloses an emulsion in water containing pyriproxyfen, wherein it is mentioned that pine-based vegetable oil can be used as an organic solvent, but there is no related example, and no other properties of pine-based vegetable oil are mentioned. CN103271035A and the like disclose active ingredient compositions containing pyriproxyfen, which focus on the synergistic effect of active ingredient compounding, and although pine-based vegetable oil is mentioned as an organic solvent, there is no related example, and no other properties of pine-based vegetable oil are mentioned. SUMMARY

[0005] The present application aims to provide a high systemic pyriproxyfen composition and a preparation method and application thereof, and based on this, the present application is completed.

[0006] The technical solution of the present application is as follows:

[0007] A high systemic pyriproxyfen composition, according to weight percentage, the composition comprises effective ingredient pyriproxyfen 1-20%, synergistic adjuvant pine-based vegetable oil 10-50%, and sophorolipid 0-20%.

[0008] Preferably, the turpentine-based plant oil is selected from one of ND-35, ND-45, ND-60, ND-100.

[0009] Preferably, the turpentine-based plant oil is ND-60.

[0010] Preferably, the mass ratio of the turpentine-based plant oil and sophorolipid is 2-5:1.

[0011] Further preferably, the mass ratio of the turpentine-based plant oil and sophorolipid is 4:1.

[0012] Preferably, the composition further comprises an adjuvant selected from one or more of emulsifiers, thickeners, preservatives, antifreezing agents, antifoaming agents, dispersants, capsule wall materials, solvents.

[0013] Preferably, the composition can be prepared into emulsifiable concentrate, microcapsule suspension.

[0014] Further preferably, the emulsifiable concentrate comprises the following ingredients: pyrimithrin 1-20%, turpentine-based plant oil 10-50%, sophorolipid 0-20%, emulsifier 5-20%, solvent balance.

[0015] Further preferably, the microcapsule suspension comprises the following ingredients: pyrimithrin 1-20%, solvent oil 15-25%, decanamide 1-10%, turpentine-based plant oil 10-50%, sophorolipid 0-20%, emulsifier 0.1-10%, dispersant 0%-5%, capsule wall material 1%-5%, solidifying agent 0-2%, preservative 0.1-0.5%, thickener 0%-3%, antifoaming agent 0.1%-0.5%, antifreezing agent 0%-10%, water balance.

[0016] Further preferably, the emulsifiable concentrate is prepared according to the following steps:

[0017] S1: pyrimithrin, turpentine-based plant oil, sophorolipid, solvent, emulsifier are added into a reaction kettle;

[0018] S2: heated to 40℃;

[0019] S3: stirred uniformly at 200-500 rpm / min;

[0020] S4: obtained systemic formulation.

[0021] Further preferably, the microcapsule suspension is prepared according to the following steps:

[0022] S1: pyrimithrin, decanamide, solvent oil are stirred and dissolved, then capsule wall material is added and stirred to form oil phase;

[0023] S2: deionized water, dispersant, emulsifier, a small amount of antifoaming agent are stirred and mixed uniformly to form water phase;

[0024] S3: The oil phase is added dropwise into the water phase, and a mixed emulsion is formed after shearing for 20 min;

[0025] S4: The curing agent is added dropwise into the mixed emulsion, and after stirring for 10 min, the temperature is raised to 60℃, and the temperature is kept for 3 hours, and then the temperature is reduced to below 40℃ by stirring, to form the piperophos microcapsule;

[0026] S5: The dispersant, thickening agent, antifreezing agent, preservative, and the remaining defoaming agent are mixed uniformly with the piperophos microcapsule to form the piperophos microcapsule suspension.

[0027] The high-uptake piperophos composition described in the application is used for controlling agricultural pests.

[0028] Preferably, the agricultural pests include hemipteran pests and lepidopteran pests.

[0029] Further preferably, the hemipteran pests are whiteflies.

[0030] The beneficial effects of the application are:

[0031] 1. The application uses the combination of turpentine-based vegetable oil ND-60 and sophorolipid as a synergistic adjuvant, changes the permeability of piperophos on the leaf surface and the conductivity in the plant body, promotes the conduction of piperophos from the application site to the newly formed tissue (such as the top leaves) and the feeding site of the target pests, and improves the quick-acting property, the persistence, and the efficacy of the preparation.

[0032] 2. The piperophos emulsion provided by the application has good quick-acting property and long persistence.

[0033] 3. The microcapsule suspension provided by the application has high safety and is friendly to the environment. DETAILED DESCRIPTION

[0034] In order for those skilled in the art to better understand the technical solutions of the present application, the present application will be further described in detail below in combination with specific examples. Obviously, the described examples are only some of the embodiments of the present application, but not all the embodiments. Based on the examples in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0035] In the following examples, the test methods used are conventional methods unless otherwise specified.

[0036] In the following examples, the raw materials, reagents, etc. used are commercially available unless otherwise specified.

[0037] I. Preparation Examples

[0038] Example 1

[0039] Pyrithrin 10% active;

[0040] Rosin-based vegetable oil ND-60, 20%;

[0041] Sophorolipid 10%;

[0042] Emulsifier 507, 8%;

[0043] Emulsifier 601, 7%;

[0044] Solvent oil 150#, q.s. to 100%.

[0045] Example 2

[0046] Pyrithrin 10% active;

[0047] Rosin-based vegetable oil ND-60, 22.5%;

[0048] Sophorolipid 7.5%;

[0049] Emulsifier 507, 8%;

[0050] Emulsifier 601, 7%;

[0051] Solvent oil 150#, q.s. to 100%.

[0052] Example 3

[0053] Pyrithrin 10% active;

[0054] Rosin-based vegetable oil ND-60, 24%;

[0055] Sophorolipid 6%;

[0056] Emulsifier 507, 8%;

[0057] Emulsifier 601, 7%;

[0058] Solvent oil 150#, q.s. to 100%.

[0059] Example 4

[0060] Pyrithrin 10% active;

[0061] Rosin-based vegetable oil ND-60, 25%;

[0062] Sophorolipid 5%;

[0063] Emulsifier 507, 8%;

[0064] Emulsifier 601, 7%;

[0065] Solvent oil 150#, q.s. to 100%.

[0066] Examples 1-4 are prepared into pyriproxy butyl emulsifiable concentrate according to the preparation method of the present application.

[0067] Example 5

[0068] Pyriproxy butyl technical material, 15%;

[0069] Solvent oil 150#, 20%;

[0070] Decanamide, 5%;

[0071] Rosin based plant oil ND-60, 24%;

[0072] Sophorolipid 6%;

[0073] Diphenyl methane diisocyanate, 2%;

[0074] Triethylenetetramine, 0.6%;

[0075] Polycarboxylate dispersant, 2.1%;

[0076] Fatty alcohol polyoxyethylene ether, 0.2%;

[0077] Phosphate ester dispersant, 1.5%;

[0078] Silicone antifoaming agent, 0.1%;

[0079] BIT preservative, 0.1%;

[0080] Xanthan gum, 0.2%;

[0081] Ethylene glycol, 4%;

[0082] Deionized water, to 100%.

[0083] Example 5 is prepared into pyriproxy butyl microcapsule suspension according to the preparation method of the present application.

[0084] Comparative Example 1

[0085] Pyriproxy butyl technical material, 10%;

[0086] Emulsifier 507, 8%;

[0087] Emulsifier 601, 7%;

[0088] Solvent oil 150#, to 100%.

[0089] Comparative Example 2

[0090] Pyriproxy butyl technical material, 10%;

[0091] Rosin based plant oil ND-60, 30%;

[0092] Emulsifier 507, 8%;

[0093] Emulsifier 601, 7%;

[0094] Add solvent oil 150# to bring the total to 100%.

[0095] Comparative Example 3

[0096] pyriproxyfen technical grade, 10%;

[0097] Pine resin-based vegetable oil ND-60, 15%;

[0098] Sophorolipid 15%;

[0099] Emulsifier 507, 8%;

[0100] Emulsifier 601, 7%;

[0101] Add solvent oil 150# to bring the total to 100%.

[0102] Comparative Examples 1 to 3 were prepared into pyriproxyfen emulsifiable concentrates according to the preparation method of the present invention.

[0103] Comparative Example 4

[0104] pyriproxyfen technical grade, 15%;

[0105] Solvent oil 150#, 20%;

[0106] Decylamide, 5%;

[0107] Diphenylmethane diisocyanate, 2%;

[0108] Triethylenetetramine, 0.6%;

[0109] Polycarboxylate dispersant, 2.1%;

[0110] Fatty alcohol polyoxyethylene ether, 0.2%;

[0111] Phosphate ester dispersant, 1.5%;

[0112] Organosilicon defoamer, 0.1%;

[0113] BIT preservative, 0.1%;

[0114] Xanthan gum, 0.2%;

[0115] Ethylene glycol, 4%;

[0116] Add deionized water to bring the solution to 100%.

[0117] Comparative Example 4 was prepared into a pyriproxyfen microcapsule suspension according to the preparation method of the present invention.

[0118] II. Systemic Absorption Test

[0119] Tested crop: Cucumber.

[0120] Tested agents: Example 1, Example 2, Example 3, Example 4, Comparative Example 1, Comparative Example 2, Comparative Example 3.

[0121] The test was set up with 8 groups of treatments, namely T1: blank control; T2: spraying Comparative Example 1; T3: spraying Comparative Example 2; T4: spraying Comparative Example 3; T5: spraying Example 1; T6: spraying Example 2; T7: spraying Example 3; T8: spraying Example 4.

[0122] The method of application was to prepare 1000 times dilution of the agent, and to spray the fully expanded true leaves at the lowermost part of the plant using a handheld micro-sprayer, with the spraying amount controlled at 1-2 μL / cm 2 The leaf area was placed in an artificial climate incubator after application, and the environmental conditions were controlled at a temperature of 25±2℃, a relative humidity of 70±5%, and a light cycle of 14h light / 10h dark.

[0123] The investigation method was to sample the growing point of the top leaf without application, the stem segments at the upper and lower parts of the treated leaf, and the whole plant roots at different time points (0h, 6h, 24h, 48h, 72h) after application, with 3 plants (with consistent growth) for each treatment and each time point independently repeated, to detect the residue amount of pyriproxyfen in each part of the plant. Among them, the initial deposition amount of pyriproxyfen was observed at 0h after application; the initial absorption and short-distance conduction of pyriproxyfen were observed at 6h and 24h after application; and the conduction peak of pyriproxyfen to the top leaf was observed at 48h and 72h after application.

[0124] The detection method of pyriproxyfen residue was to add fresh samples into extraction solvent acetonitrile, to uniformly homogenize the extraction after grinding with a tissue grinder, to perform salting-out stratification, solid-phase extraction, nitrogen blowing concentration, to re-dissolve with mobile phase, to pass through a 0.22 μm filter membrane, and to detect and analyze using a high-performance liquid chromatograph, to calculate the content of pyriproxyfen in each sample.

[0125] Through detection, the test results are shown in the following table, compared with T1 and T2, T3-T8 all have synergistic effect, among them, at the same sampling time point (especially 24h, 48h, 72h), the residue amount of pyriproxyfen in the top leaf of T7 is the highest, which is significantly higher than that of other treatment groups; the conduction efficiency (top leaf content / initial deposition amount) of T7 is significantly higher than that of other treatment groups; pyriproxyfen cannot be detected in all parts of the control group.

[0126] The above test results show that the combination of pine resin-based plant oil and sophorolipid can significantly improve the systemic conduction of pyriproxyfen in cucumber, and when the mass ratio of pine resin-based plant oil and sophorolipid is 4:1, the effect is the best.

[0127] Table 1 Pyriproxyfen residue determination results

[0128]

[0129]

[0130]

[0131]

[0132]

[0133] III. Field efficacy test

[0134] Test agent: Example 3, Example 5, Comparative Example 1, Comparative Example 4.

[0135] Test crop: Cucumber.

[0136] Test target: Whitefly (Trialeurodes vaporariorum).

[0137] Test site: Songfeng Vegetable Professional Cooperative in Songjiang District, Shanghai.

[0138] Test design: A total of 5 treatments were set, which were blank control, Example 3, Example 5, Comparative Example 1, Comparative Example 4, each treatment was repeated 3 times, and the area of each treatment plot was 20 m 2 . The plots were randomly arranged, and the amount of each treatment was 90 g.a.i. / hm 2 . The amount of water was 60 kg / acre. At the peak of whitefly occurrence, uniform spraying treatment was carried out by using Gongnong-16 type knapsack manual sprayer.

[0139] Efficacy investigation method: The base number of active larvae was investigated before drug, and the number of active larvae was investigated 1 day, 3 days, 5 days, 7 days and 14 days after drug. When investigating, 3 plants were investigated in each plot, and 10 leaves were fixedly investigated in each plant. The mite population reduction rate of each plot was calculated according to the base number before drug

[0140] The test results are shown in the following table. Compared with Comparative Example 1, the control effect of Example 3 is obviously improved, the quick-acting property is good, and the effective period is long, and the control effect is maintained at more than 90% 14 days after drug; compared with Comparative Example 4, the control effect of Example 5 is also obviously improved; compared with Example 3, the quick-acting property of Example 5 is poor, but the effective period is long, and the control effect of Example 5 is better than that of Example 3 14 days after drug.

[0141] Table 2 Field efficacy test of whitefly

[0142]

[0143] The test results show that the combination of ND-60 and sophorolipid can effectively improve the systemic translocation of pyriproxyfen in crops, thereby improving the quick-acting property of the preparation and increasing the persistence period of the preparation. The emulsifiable concentrate has good quick-acting property, and the microcapsule suspension can further prolong the persistence period, and the selection can be made according to the actual situation during the prevention and control process.

[0144] Although the embodiments of the present application are disclosed for illustrative purposes, those skilled in the art can understand that various substitutions, changes and modifications are possible without departing from the spirit and scope of the present application and the appended claims, and therefore the scope of the present application is not limited to the disclosed content of the embodiments.

Claims

1. A high systemic pypriofen composition, characterized by, The composition comprises 1-20% of active ingredient pyriproxyfen, 10-50% of synergistic adjuvant rosin-based plant oil, and 0-20% of sophorolipid, by weight percentage.

2. The high systemic pypriophos composition according to claim 1, wherein The rosin-based plant oil is selected from one of ND-35, ND-45, ND-60, and ND-100.

3. The high systemic pypriophos composition according to claim 2, wherein The rosin-based plant oil is ND-60.

4. The high systemic pypriophos composition according to claim 1, wherein The mass ratio of the rosin-based plant oil and the sophorolipid is 2-5:

1.

5. The high systemic pypriophos composition according to claim 4, wherein The mass ratio of the rosin-based plant oil and the sophorolipid is 4:

1.

6. The high systemic pypriophos composition according to claim 1, wherein The composition further comprises auxiliary materials selected from one or more of emulsifiers, dispersants, thickening agents, preservatives, antifreezing agents, antifoaming agents, capsule wall materials, solidifying agents, and solvents.

7. The high systemic pypriophos composition according to claim 6, wherein The composition can be prepared into emulsifiable concentrate or microcapsule suspension.

8. The high systemic pypriophos composition according to claim 7, wherein The emulsifiable concentrate comprises the following ingredients: 1-20% of pyriproxyfen, 10-50% of rosin-based plant oil, 0-20% of sophorolipid, 5-20% of emulsifiers, and the rest of solvent.

9. The high systemic pypriophos composition according to claim 7, wherein The microcapsule suspension comprises the following ingredients: 1-20% of pyriproxyfen, 15-25% of solvent oil, 1-10% of decanamide, 10-50% of rosin-based plant oil, 0-20% of sophorolipid, 0.1-10% of emulsifiers, 0-5% of dispersants, 1-5% of capsule wall materials, 0-2% of solidifying agents, 0.1-0.5% of preservatives, 0-3% of thickening agents, 0.1-0.5% of antifoaming agents, 0-10% of antifreezing agents, and the rest of water.

10. The flowable composition according to claim 8, wherein The specific preparation steps are as follows: S1: pyriproxyfen, rosin-based plant oil, sophorolipid, solvent, and emulsifiers are added into a reaction kettle; S2: heated to 40℃; S3: stirred at 200-500 rpm / min to uniform; S4: obtained systemic formulation.

11. The suspension of microcapsules according to claim 9, characterized in that The specific preparation steps are as follows: S1: pyriproxyfen, decanamide, and solvent oil are stirred and dissolved, then the capsule wall materials are added and stirred to form an oil phase; S2: deionized water, dispersants, emulsifiers, and a small amount of antifoaming agents are stirred and mixed to form an aqueous phase; S3: the oil phase is added dropwise into the aqueous phase, and a mixed emulsion is formed after shearing for 20 min; S4: the solidifying agent is added dropwise into the mixed emulsion, stirred for 10 min, heated to 60℃, and kept for 3 hours, then stirred to cool down to below 40℃, to form pyriproxyfen microcapsules; S5: dispersants, thickening agents, antifreezing agents, preservatives, and the rest of antifoaming agents are stirred and mixed with the pyriproxyfen microcapsules to form pyriproxyfen microcapsule suspension.

12. Use of the high systemic pyriproxyfen composition according to any one of claims 1-9 for controlling agricultural pests.

13. The use according to claim 12, characterized in that, The agricultural pests are whitefly.

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