Spinosad suspending agent and preparation method thereof

Abstract

The invention relates to the technical field of pesticide suspending agents, in particular to a spinosad suspending agent and a preparation method thereof. The spinosad suspending agent is prepared from the following raw materials in parts by mass: 2 to 15 parts of spinosad, 5 to 15 parts of an emulsifying agent, 1 to 3 parts of a dispersing agent, 1 to 3 parts of a wetting agent, 0.1 to 0.5 part of a thickening agent, 0.1 to 0.5 part of a defoaming agent, 2 to 6 parts of an anti-freezing agent and 6 to 10 parts of a film coating agent, according to the spinosad suspending agent and the preparation method thereof, the film coating agent is added to coat spinosad and a preparation thereof, the photolysis resisting effect can be achieved, and the stability of the agent is improved; the prepared spinosad suspending agent has good stability and temperature resistance and is convenient to store; the spinosad suspending agent prepared by the invention has a good control effect on psylla chinensis, the lasting period is prolonged, the utilization rate of effective components is improved, the dosage can be reduced, and the cost is saved.

Description

Technical Field

[0001] The present application relates to the technical field of pesticide suspension concentrates, and in particular to a spinosad suspension concentrate and a preparation method thereof. Background Art

[0002] Spinosad is a macrolide insecticide produced by fermentation of soil actinomycetes (Saccharopolyspora spinosa). Its mechanism of action is to activate the nicotinic acetylcholine receptors and gamma-aminobutyric acid receptors in the insect nervous system, leading to sustained nerve excitation and ultimately death. Spinosad is widely used as an insecticide due to its high efficacy, low toxicity, and high safety against non-target organisms.

[0003] Spinosad molecules contain multiple conjugated double bonds and macrolide structures, which easily absorb ultraviolet (UV) light, triggering photolysis reactions and leading to the degradation of the active ingredients. Studies have shown that under natural light (especially the UV band), the half-life of spinosad can be shortened to several hours. Therefore, spinosad is extremely susceptible to light factors and degradation during storage, transportation and use.

[0004] When pesticide suspension concentrates with spinosad as the active ingredient are exported to other countries, due to the long transportation time, the pesticide suspension concentrates are prone to particle aggregation, sedimentation or crystal growth during storage, which leads to the destruction of the suspension system. In addition, the spinosad suspension concentrates will accelerate the Brownian motion of particles at high temperatures (>40°C), intensifying stratification and agglomeration, affecting the redispersibility before use. This poses a serious test to the product quality of the spinosad suspension concentrates.

[0005] Therefore, how to effectively solve the problems of spinosad's easy photolysis and poor high temperature resistance has become an urgent problem to be solved. Summary of the Invention

[0006] In view of the deficiencies in the prior art, the present application provides a spinosad suspension concentrate and a preparation method thereof.

[0007] In the first aspect, the present application provides a spinosad suspension concentrate, which adopts the following technical solution: A spinosad suspension comprises the following raw materials in parts by mass: 2-15 parts of spinosad, 5-15 parts of emulsifier, 1-3 parts of dispersant, 1-3 parts of wetting agent, 0.1-0.5 parts of thickener, 0.1-0.5 parts of defoamer, 2-6 parts of antifreeze and 6-10 parts of coating agent.

[0008] By adopting the above technical solution, since spinosad and its preparations are easily decomposed under light conditions, the raw materials are improved in this application, and the added coating agent can adsorb spinosad and form a film layer on the surface of spinosad and its preparations, which can play a role in resisting photolysis, improve the stability of the agent, and extend the duration of the agent; secondly, the added coating agent is a degradable coating agent, and the added coating agent serves as a carrier of spinosad, which can adsorb spinosad and its preparations, thereby preparing a degradable slow-release film-coated insecticide, effectively controlling the release rate of the active ingredient, and extending the duration of the agent.

[0009] Preferably, the coating agent comprises the following raw materials in parts by mass: 10-15 parts of lignin nanoparticle / surfactant composite material, 5-10 parts of zein, 5-10 parts of gelatin, 1-3 parts of glycerol, 1-2 parts of glucose and 0.5-2 parts of acetic acid.

[0010] By adopting the above-mentioned technical scheme, the present application uses zein and gelatin as base materials and glycerol and glucose as modifiers to prepare a degradable zein / gelatin composite solution, and the prepared composite solution is blended with a lignin nanoparticle / surfactant composite material to obtain a coating agent containing the lignin nanoparticle / surfactant composite material. The prepared coating agent can adsorb and load spinosad and its preparations to obtain a slow-release film-coated insecticide, which can control the release rate of the active ingredients and extend the duration of the agent's use. In addition, the prepared coating agent forms a film layer on the surface of spinosad and its preparations, thereby playing an anti-photolysis role, improving the stability of the agent and extending the duration of the agent's use.

[0011] The prepared film-forming agent is a degradable film-forming agent. After the spinosad suspension is applied, the film-forming agent remaining in the soil can be self-degraded, effectively reducing the pollution of pesticide residues to the environment.

[0012] Preferably, the lignin nanoparticle / surfactant composite material comprises the following raw materials in parts by weight: 1-3 parts of alkali lignin, 4-8 parts of anionic surfactant, 2-5 parts of sodium chloride and 6-18 parts of nonionic surfactant.

[0013] Preferably, the anionic surfactant is a mixture of a first anionic surfactant and a second anionic surfactant; the mass ratio of the first anionic surfactant to the second anionic surfactant is (1-3):1.

[0014] Preferably, the anionic surfactant is sodium α-olefin sulfonate.

[0015] Preferably, the nonionic surfactant is coconut oil fatty acid diethanolamide.

[0016] Preferably, the preparation method of the lignin nanoparticle / surfactant composite material comprises the following steps: Alkali lignin is dissolved in a solvent, and a first portion of anionic surfactant is added and mixed to obtain a lignin concentrate; the prepared lignin concentrate is mixed with a second portion of anionic surfactant, a nonionic surfactant, and sodium chloride to obtain a lignin nanoparticle / surfactant composite material.

[0017] By adopting the above technical solution, in this application, a lignin concentrate is prepared using an anionic surfactant sodium α-olefin sulfonate as an antisolvent. The prepared lignin concentrate is then mixed with an anionic surfactant sodium α-olefin sulfonate, and then mixed with a non-ionic surfactant coconut oil fatty acid diethanolamide and sodium chloride to obtain a lignin nanoparticle / surfactant composite material with stability and temperature resistance.

[0018] After the coating agent containing the lignin nanoparticle / surfactant composite material is mixed with other raw materials, the lignin nanoparticle / surfactant composite material forms a protective layer with stability and temperature resistance on the surface of spinosad and its preparation, thereby effectively improving the stability and temperature resistance of spinosad and its preparation.

[0019] Preferably, the preparation method of the coating agent comprises the following steps: dissolving zein in a solvent, adding gelatin and mixing to obtain a composite solution; adding glycerol and glucose to the composite solution and mixing them to obtain a modified composite solution; The lignin nanoparticle / surfactant composite material is added to the modified composite solution and mixed to obtain a coating agent.

[0020] Preferably, the emulsifier is at least one of calcium dodecylbenzenesulfonate, phenylphenol polyoxyethylene ether phosphate, styrene polyoxyethylene ether ammonium sulfate, sorbitan trioleate, isomeric decanol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether and castor oil polyoxyethylene ether.

[0021] Further preferably, the emulsifier is calcium dodecylbenzenesulfonate and castor oil polyoxyethylene ether; the mass ratio of calcium dodecylbenzenesulfonate and castor oil polyoxyethylene ether is (1-3):1.

[0022] Preferably, the dispersant is at least one of polyethylene glycol, polyvinyl alcohol, polyvinyl pyrrolidone and Tersperse 2500.

[0023] Preferably, the wetting agent is at least one of fatty alcohol polyoxyethylene ether, Morwet EFW, isopropyl naphthalene sulfonate and polystyrene polyoxyethylene ether.

[0024] Preferably, the thickener is at least one of xanthan gum, carboxymethyl cellulose and magnesium aluminum silicate.

[0025] Preferably, the defoaming agent is at least one of an organosilicon defoaming agent, polyalkylsiloxane, mineral oil, fatty alcohol and tributyl phosphate.

[0026] Preferably, the antifreeze agent is at least one of ethylene glycol, propylene glycol, glycerol, polyethylene glycol and urea.

[0027] In a second aspect, the present application provides a method for preparing a spinosad suspension concentrate, using the following technical solution: A method for preparing a spinosad suspension concentrate, comprising the following steps: (1) Weigh each raw material according to the formula; (2) Using water as a medium, spinosad, an emulsifier, a dispersant, a wetting agent, a thickener, a defoaming agent, an antifreeze agent, and a coating agent are uniformly mixed to obtain an aqueous suspension, and the obtained aqueous suspension is ground and sheared to prepare a spinosad suspension concentrate.

[0028] In summary, this application includes at least one of the following beneficial technical effects: 1. The present application discloses a spinosad suspension concentrate and a preparation method thereof. The addition of a coating agent to coat the spinosad and its preparation can play a role in resisting photolysis, thereby improving the stability of the agent and extending the duration of the agent's use. 2. The present application discloses a spinosad suspension concentrate and a preparation method thereof. The prepared spinosad suspension concentrate has good stability and temperature resistance and is easy to store; 3. The spinosad suspension prepared in the present application has a good control effect on pear psyllids, and has a prolonged effective period, improved utilization of active ingredients, can reduce the dosage of the drug, and save costs. DETAILED DESCRIPTION

[0029] The technical solution of the present application is further illustrated below through specific embodiments. The specific embodiments do not limit the scope of protection of the present application; some non-essential modifications and adjustments made by others based on the concept of the present application still fall within the scope of protection of the present application.

[0030] The raw materials involved in this application are all commercially available products, among which: Zein, gelatin, glycerol, glucose, and acetic acid were purchased from Shanghai Aladdin Reagent Co., Ltd.

[0031] Alkali lignin, purchased from Merck, CAS number: 8068-05-1; Sodium α-olefin sulfonate, 35% aqueous solution, was purchased from Shanghai MacLean Reagent Co., Ltd.; Coconut oil fatty acid diethanolamide, 1:1.5 type, was purchased from Shanghai MacLean Reagent Co., Ltd.; Spinosad was purchased from Hebei Mojin Biotechnology Co., Ltd., CAS number: 131929-60-7.

[0032] The present application is further described in detail below with reference to the following examples and comparative examples.

[0033] Preparation Example 1: A method for preparing a lignin nanoparticle / surfactant composite material comprises the following steps: (1) Dissolve 2 g of alkali lignin in tetrahydrofuran solution and mix for 12 hours to obtain an alkali lignin solution with a mass fraction of 2 wt%; (2) adding 3 g of sodium α-olefin sulfonate to the solution and performing ultrasonic mixing for 20 minutes, and evaporating tetrahydrofuran from the prepared dispersion using a rotary evaporator to obtain a lignin concentrate; (3) The prepared lignin concentrate was mixed with 3 g of sodium α-olefin sulfonate, 12 g of coconut oil fatty acid diethanolamide, 4 g of sodium chloride, and 200 ml of water to obtain a lignin nanoparticle / surfactant composite material.

[0034] Preparation Example 2: A method for preparing a lignin nanoparticle / surfactant composite material comprises the following steps: (1) Dissolve 1 g of alkali lignin in tetrahydrofuran solution and mix for 12 hours to obtain an alkali lignin solution with a mass fraction of 2 wt%; (2) adding 2 g of sodium α-olefin sulfonate to the solution and performing ultrasonic mixing for 20 minutes, and evaporating tetrahydrofuran from the prepared dispersion using a rotary evaporator to obtain a lignin concentrate; (3) The prepared lignin concentrate was mixed with 2 g of sodium α-olefin sulfonate, 6 g of coconut oil fatty acid diethanolamide, 2 g of sodium chloride, and 200 ml of water to obtain a lignin nanoparticle / surfactant composite material.

[0035] Preparation Example 3: A method for preparing a lignin nanoparticle / surfactant composite material comprises the following steps: (1) Dissolve 3 g of alkali lignin in tetrahydrofuran solution and mix for 12 hours to obtain an alkali lignin solution with a mass fraction of 2 wt%; (2) adding 4 g of sodium α-olefin sulfonate to the solution and performing ultrasonic mixing for 20 minutes, and evaporating tetrahydrofuran from the prepared dispersion using a rotary evaporator to obtain a lignin concentrate; (3) The prepared lignin concentrate was mixed with 4 g of sodium α-olefin sulfonate, 18 g of coconut oil fatty acid diethanolamide, 5 g of sodium chloride, and 200 ml of water to obtain a lignin nanoparticle / surfactant composite material.

[0036] Preparation Example 4: Preparation of coating agent: The coating agent includes the following raw materials: 13 g of lignin nanoparticle / surfactant composite material, 7 g of zein, 7 g of gelatin, 2 g of glycerol, 1.5 g of glucose and 1 g of acetic acid.

[0037] The lignin nanoparticle / surfactant composite material was prepared according to Preparation Example 1.

[0038] The preparation method of the coating agent comprises the following steps: Add water to acetic acid to prepare an acetic acid solution with a mass concentration of 80%; Add gelatin to 10 times its mass of water, let it stand for 10 minutes, heat it in a water bath to 50°C, and stir until it is completely dissolved to obtain a gelatin solution; Dissolve zein in 80% acetic acid solution and mix well; slowly pour the warm gelatin solution into the zein ethanol solution and stir at 50°C to obtain a composite solution; Add 30 g of glycerol, glucose, and water to the composite solution and mix to obtain a modified composite solution; The lignin nanoparticle / surfactant composite material and 100 g of water were added to the modified composite solution and mixed to obtain a coating agent.

[0039] Preparation Example 5: Preparation of coating agent: The coating agent includes the following raw materials: 13 g of lignin nanoparticle / surfactant composite material, 7 g of zein, 7 g of gelatin, 2 g of glycerol, 1.5 g of glucose and 1 g of acetic acid.

[0040] The lignin nanoparticle / surfactant composite material was prepared according to Preparation Example 2.

[0041] The preparation method of the coating agent comprises the following steps: Add water to acetic acid to prepare an acetic acid solution with a mass concentration of 80%; Add gelatin to 10 times its mass of water, let it stand for 10 minutes, heat it in a water bath to 50°C, and stir until it is completely dissolved to obtain a gelatin solution; Dissolve zein in 80% acetic acid solution and mix well; slowly pour the warm gelatin solution into the zein ethanol solution and stir at 50°C to obtain a composite solution; Add 30 g of glycerol, glucose, and water to the composite solution and mix to obtain a modified composite solution; The lignin nanoparticle / surfactant composite material and 100 g of water were added to the modified composite solution and mixed to obtain a coating agent.

[0042] Preparation Example 6: Preparation of coating agent: The coating agent includes the following raw materials: 13 g of lignin nanoparticle / surfactant composite material, 7 g of zein, 7 g of gelatin, 2 g of glycerol, 1.5 g of glucose and 1 g of acetic acid.

[0043] The lignin nanoparticle / surfactant composite material was prepared according to Preparation Example 3.

[0044] The preparation method of the coating agent comprises the following steps: Add water to acetic acid to prepare an acetic acid solution with a mass concentration of 80%; Add gelatin to 10 times its mass of water, let it stand for 10 minutes, heat it in a water bath to 50°C, and stir until it is completely dissolved to obtain a gelatin solution; Dissolve zein in 80% acetic acid solution and mix well; slowly pour the warm gelatin solution into the zein ethanol solution and stir at 50°C to obtain a composite solution; Add 30 g of glycerol, glucose, and water to the composite solution and mix to obtain a modified composite solution; The lignin nanoparticle / surfactant composite material and 100 g of water were added to the modified composite solution and mixed to obtain a coating agent.

[0045] Preparation Example 7: Preparation of coating agent: The coating agent includes the following raw materials: 10 g of lignin nanoparticle / surfactant composite material, 5 g of zein, 5 g of gelatin, 1 g of glycerol, 1 g of glucose and 0.5 g of acetic acid.

[0046] The lignin nanoparticle / surfactant composite material was prepared according to Preparation Example 2.

[0047] The preparation method of the coating agent comprises the following steps: Add water to acetic acid to prepare an acetic acid solution with a mass concentration of 80%; Add gelatin to 10 times its mass of water, let it stand for 10 minutes, heat it in a water bath to 50°C, and stir until it is completely dissolved to obtain a gelatin solution; Dissolve zein in 80% acetic acid solution and mix well; slowly pour the warm gelatin solution into the zein ethanol solution and stir at 50°C to obtain a composite solution; Add 30 g of glycerol, glucose, and water to the composite solution and mix to obtain a modified composite solution; The lignin nanoparticle / surfactant composite material and 100 g of water were added to the modified composite solution and mixed to obtain a coating agent.

[0048] Preparation Example 8: Preparation of coating agent: The coating agent includes the following raw materials: 15 g of lignin nanoparticle / surfactant composite material, 10 g of zein, 10 g of gelatin, 3 g of glycerol, 2 g of glucose and 2 g of acetic acid.

[0049] The lignin nanoparticle / surfactant composite material was prepared according to Preparation Example 3.

[0050] The preparation method of the coating agent comprises the following steps: Add water to acetic acid to prepare an acetic acid solution with a mass concentration of 80%; Add gelatin to 10 times its mass of water, let it stand for 10 minutes, heat it in a water bath to 50°C, and stir until it is completely dissolved to obtain a gelatin solution; Dissolve zein in 80% acetic acid solution and mix well; slowly pour the warm gelatin solution into the zein ethanol solution and stir at 50°C to obtain a composite solution; Add 30 g of glycerol, glucose, and water to the composite solution and mix to obtain a modified composite solution; The lignin nanoparticle / surfactant composite material and 100 g of water were added to the modified composite solution and mixed to obtain a coating agent.

[0051] Example 1: A spinosad suspension concentrate comprises the following raw materials: 8g of spinosad, 8g of an emulsifier, 2g of a dispersant, 2g of a wetting agent, 0.3g of a thickener, 0.3g of a defoaming agent, 4g of an antifreeze agent, and 8g of a coating agent.

[0052] The emulsifiers are calcium dodecylbenzenesulfonate and castor oil polyoxyethylene ether; the mass ratio of calcium dodecylbenzenesulfonate to castor oil polyoxyethylene ether is 2:1.

[0053] The dispersant is polyethylene glycol 200.

[0054] The wetting agent is Morwet EFW.

[0055] The thickener is magnesium aluminum silicate.

[0056] The defoaming agent is tributyl phosphate.

[0057] The antifreeze agent is ethylene glycol.

[0058] The coating agent is prepared according to Preparation Example 4.

[0059] A method for preparing a spinosad suspension concentrate, comprising the following steps: (1) Weigh each raw material according to the formula; (2) Spinosad, an emulsifier, a dispersant, a wetting agent, a thickener, a defoaming agent, an antifreeze agent, a coating agent, and 100 g of water were uniformly mixed to obtain an aqueous suspension. The aqueous suspension was ground in a sand mill at 25°C ± 5°C for 60 minutes, and then sheared in a shearing machine for 10 minutes to prepare a spinosad suspension concentrate.

[0060] Example 2: A spinosad suspension concentrate comprises the following raw materials: 8g of spinosad, 8g of an emulsifier, 2g of a dispersant, 2g of a wetting agent, 0.3g of a thickener, 0.3g of a defoaming agent, 4g of an antifreeze agent, and 8g of a coating agent.

[0061] The emulsifiers are calcium dodecylbenzenesulfonate and castor oil polyoxyethylene ether; the mass ratio of calcium dodecylbenzenesulfonate to castor oil polyoxyethylene ether is 2:1.

[0062] The dispersant is polyethylene glycol 200.

[0063] The wetting agent is Morwet EFW.

[0064] The thickener is magnesium aluminum silicate.

[0065] The defoaming agent is tributyl phosphate.

[0066] The antifreeze agent is ethylene glycol.

[0067] The coating agent is prepared according to Preparation Example 5.

[0068] A method for preparing a spinosad suspension concentrate, comprising the following steps: (1) Weigh each raw material according to the formula; (2) Spinosad, an emulsifier, a dispersant, a wetting agent, a thickener, a defoaming agent, an antifreeze agent, a coating agent, and 100 g of water were uniformly mixed to obtain an aqueous suspension. The aqueous suspension was ground in a sand mill at 25°C ± 5°C for 60 minutes, and then sheared in a shearing machine for 10 minutes to prepare a spinosad suspension concentrate.

[0069] Example 3: A spinosad suspension concentrate comprises the following raw materials: 8g of spinosad, 8g of an emulsifier, 2g of a dispersant, 2g of a wetting agent, 0.3g of a thickener, 0.3g of a defoaming agent, 4g of an antifreeze agent, and 8g of a coating agent.

[0070] The emulsifiers are calcium dodecylbenzenesulfonate and castor oil polyoxyethylene ether; the mass ratio of calcium dodecylbenzenesulfonate to castor oil polyoxyethylene ether is 2:1.

[0071] The dispersant is polyethylene glycol 200.

[0072] The wetting agent is Morwet EFW.

[0073] The thickener is magnesium aluminum silicate.

[0074] The defoaming agent is tributyl phosphate.

[0075] The antifreeze agent is ethylene glycol.

[0076] The coating agent is prepared according to Preparation Example 6.

[0077] A method for preparing a spinosad suspension concentrate, comprising the following steps: (1) Weigh each raw material according to the formula; (2) Spinosad, an emulsifier, a dispersant, a wetting agent, a thickener, a defoaming agent, an antifreeze agent, a coating agent, and 100 g of water were uniformly mixed to obtain an aqueous suspension. The aqueous suspension was ground in a sand mill at 25°C ± 5°C for 60 minutes, and then sheared in a shearing machine for 10 minutes to prepare a spinosad suspension concentrate.

[0078] Example 4: A spinosad suspension concentrate comprises the following raw materials: 2g of spinosad, 5g of an emulsifier, 1g of a dispersant, 1g of a wetting agent, 0.1g of a thickener, 0.1g of a defoaming agent, 2g of an antifreeze agent, and 6g of a coating agent.

[0079] The emulsifiers are calcium dodecylbenzenesulfonate and castor oil polyoxyethylene ether; the mass ratio of calcium dodecylbenzenesulfonate to castor oil polyoxyethylene ether is 2:1.

[0080] The dispersant is polyethylene glycol 200.

[0081] The wetting agent is Morwet EFW.

[0082] The thickener is magnesium aluminum silicate.

[0083] The defoaming agent is tributyl phosphate.

[0084] The antifreeze agent is ethylene glycol.

[0085] The coating agent is prepared according to Preparation Example 7.

[0086] A method for preparing a spinosad suspension concentrate, comprising the following steps: (1) Weigh each raw material according to the formula; (2) Spinosad, an emulsifier, a dispersant, a wetting agent, a thickener, a defoaming agent, an antifreeze agent, a coating agent, and 100 g of water were uniformly mixed to obtain an aqueous suspension. The aqueous suspension was ground in a sand mill at 25°C ± 5°C for 60 minutes, and then sheared in a shearing machine for 10 minutes to prepare a spinosad suspension concentrate.

[0087] Example 5: A spinosad suspension concentrate comprises the following raw materials: 15 g of spinosad, 15 g of an emulsifier, 3 g of a dispersant, 3 g of a wetting agent, 0.5 g of a thickener, 0.5 g of a defoaming agent, 6 g of an antifreeze agent, and 10 g of a coating agent.

[0088] The emulsifiers are calcium dodecylbenzenesulfonate and castor oil polyoxyethylene ether; the mass ratio of calcium dodecylbenzenesulfonate to castor oil polyoxyethylene ether is 2:1.

[0089] The dispersant is polyethylene glycol 200.

[0090] The wetting agent is Morwet EFW.

[0091] The thickener is magnesium aluminum silicate.

[0092] The defoaming agent is tributyl phosphate.

[0093] The antifreeze agent is ethylene glycol.

[0094] The coating agent is prepared according to Preparation Example 8.

[0095] A method for preparing a spinosad suspension concentrate, comprising the following steps: (1) Weigh each raw material according to the formula; (2) Spinosad, an emulsifier, a dispersant, a wetting agent, a thickener, a defoaming agent, an antifreeze agent, a coating agent, and 100 g of water were uniformly mixed to obtain an aqueous suspension. The aqueous suspension was ground in a sand mill at 25°C ± 5°C for 60 minutes, and then sheared in a shearing machine for 10 minutes to prepare a spinosad suspension concentrate.

[0096] Example 6: The difference from Example 1 is that the added amount of the coating agent is 6 g.

[0097] Example 7: The difference from Example 1 is that the added amount of the coating agent is 10 g.

[0098] Comparative Example 1: The difference from Example 1 is that no coating agent is added.

[0099] Comparative Example 2: The difference from Example 1 is that the added amount of the coating agent is 5 g.

[0100] Comparative Example 3: The difference from Example 1 is that the added amount of the coating agent is 11 g.

[0101] Comparative Example 4: The difference from Example 1 is that when preparing the coating agent, the lignin nanoparticle / surfactant composite material is not added.

[0102] Performance testing: 1. Light stability test: The samples prepared in the above examples and comparative examples were subjected to a light irradiation test to detect the light stability of the spinosad suspension concentrate.

[0103] The samples of the preparations of the above examples and comparative examples were sampled and placed in 25 ml quartz tubes, marked and recorded as 7 treatments. Two quartz tubes were used for each treatment and divided into two groups. One group was directly sealed and the other group was sealed and wrapped with tin foil to avoid light. Then the two groups of quartz tubes were exposed to fluorescent lamp (wavelength range 400-700 nm, light intensity 5000 lux) and near-ultraviolet lamp (320-400 nm, irradiance 1.5 W / m 2 ) was repeated three times at a temperature of 25±1°C and a humidity of 60%±5%. Samples were taken on days 0, 3, 7 and 14 of treatment to determine the decomposition rate of the spinosad suspension concentrate.

[0104] Table 1 Decomposition rate of spinosad suspension concentrate According to the illumination test results in Table 1, the spinosad suspension prepared by the method of the present application (Examples 1-7) has good light stability, indicating that the spinosad suspension with the addition of a coating agent is stable to light. Under 14 days of illumination, the decomposition rate is less than 4.0%, which effectively solves the problem of spinosad decomposition under light conditions.

[0105] Combining the data results of Example 1 and Comparative Example 1, it can be seen that the test results of Example 1 are better than those of Comparative Example 1, indicating that the addition of the coating agent effectively prevents spinosad from decomposing under light conditions, and the prepared spinosad suspension is light-stable.

[0106] Combined with the data results of Example 1, Example 6, Example 7, Comparative Example 2 and Comparative Example 3, it can be seen that the amount of coating agent added has an impact on the photostability test results of the spinosad suspension concentrate, and when the amount of coating agent added is 6-10g, the photostability effect of the spinosad suspension concentrate is best.

[0107] 2. Efficacy test: The samples prepared in the above examples and comparative examples were subjected to field efficacy tests for controlling pear psylla, respectively, with reference to the standard "Guidelines for Field Efficacy Tests of Pesticides" (GB / T 17980.21-2000).

[0108] (1) Test site requirements: Select pear orchards with serious psyllid infestation and uniform insect population density, with consistent varieties, tree ages, and cultivation and management measures.

[0109] (2) District division: The experiment set up 9 treatment groups (Example, Comparative Example and Clear Water Control Group), each group was repeated 4 times, with a total of 36 plots. The cultivation conditions were basically uniform and consistent. Random block arrangement was adopted, with 3 pear trees in each plot, 5 test points were selected for each pear tree, and the number of pear psylla was counted at fixed points.

[0110] (3) Application method: According to the duration of the drug, generally apply the drug 1-2 times, with an interval of 7-10 days.

[0111] Spray the entire plant: Focus on spraying the back of the leaves (the main habitat of pear psyllids) until the leaves are moist but not dripping.

[0112] (4) Drug efficacy investigation and record: Before applying the pesticide, investigate the base population of pear psyllids. After applying the pesticide, investigate the changes in the population 3, 7, and 15 days later. Count the number of live pear psyllids on the leaves. Calculate the pear psyllid population reduction rate and control effect. The pear psyllid population reduction rate and control effect are calculated according to the following formula: (5) Test results: Table 2 Results of drug efficacy test According to the test results in Table 2, the spinosad suspension prepared by the method of the present application (Examples 1-7) has a good control effect on pear psyllids, and has a prolonged effective period, improved the utilization rate of the active ingredients, can reduce the dosage, and save costs.

[0113] Combining the data results of Example 1 and Comparative Example 1, it can be seen that the test results of Example 1 are better than those of Comparative Example 1, indicating that the addition of the coating agent effectively prolongs the duration of the drug and improves the utilization rate of the active ingredients.

[0114] Combined with the data results of Example 1, Example 6, Example 7, Comparative Example 2 and Comparative Example 3, it can be seen that the amount of coating agent added has an impact on the prevention effect test results of the spinosad suspension concentrate, and when the amount of coating agent added is 6-10g, the prevention effect of the spinosad suspension concentrate is the best.

[0115] 3. Particle size stability: The particle size stability of the samples prepared in the above examples and comparative examples was tested as follows: The storage stability of the samples prepared in the above examples and comparative examples in different environments was tested according to the testing standards GB / T19137-2003 "Test method for low temperature stability of pesticides", NY / T1427-2016 "General rules for testing the stability of pesticides at room temperature", and GB / T19136-2003 "Test method for thermal storage stability of pesticides".

[0116] Three samples of the same content were weighed from each example and comparative example and stored in quartz test tubes with tube stoppers. The samples were stored in thermostats at 25°C, 54°C, and 65°C, respectively. The particle sizes of the samples were measured using a Malvern laser particle size analyzer. The samples in the 25°C treatment group were stored for 7 days, the 54°C treatment group were stored for 14 days, and the 65°C treatment group were stored for 60 days.

[0117] Table 3 Stability test results According to the test results in Table 3, the spinosad suspension prepared by the method of the present application (Examples 1-7) has good stability and temperature resistance and is easy to store.

[0118] Combining the data results of Example 1 and Comparative Example 1, it can be seen that the test result of Example 1 is better than the test result of Comparative Example 1, indicating that the addition of the coating agent effectively improves the stability and temperature resistance of the spinosad suspension concentrate.

[0119] Combined with the data results of Example 1, Example 6, Example 7, Comparative Example 2, and Comparative Example 3, it can be seen that the amount of coating agent added has an impact on the stability and temperature resistance test results of the spinosad suspension concentrate, and when the amount of coating agent added is 6-10g, the stability and temperature resistance of the spinosad suspension concentrate are best.

[0120] Combining the data of Example 1 and Comparative Example 4, it can be seen that the test result of Example 1 is better than the test result of Comparative Example 4, indicating that the added lignin nanoparticles / surfactant composite material effectively improves the stability and temperature resistance of the spinosad suspension concentrate.

Claims

1. A spinosad suspension concentrate, characterized in that: The invention comprises the following raw materials in parts by weight: 2-15 parts of spinosad, 5-15 parts of emulsifier, 1-3 parts of dispersant, 1-3 parts of wetting agent, 0.1-0.5 parts of thickener, 0.1-0.5 parts of defoaming agent, 2-6 parts of antifreeze agent and 6-10 parts of coating agent.

2. A spinosad suspension concentrate according to claim 1, characterized in that: The coating agent comprises the following raw materials in parts by mass: 10-15 parts of lignin nanoparticle / surfactant composite material, 5-10 parts of zein, 5-10 parts of gelatin, 1-3 parts of glycerol, 1-2 parts of glucose and 0.5-2 parts of acetic acid.

3. A spinosad suspension concentrate according to claim 2, characterized in that: The lignin nanoparticle / surfactant composite material comprises the following raw materials in parts by weight: 1-3 parts of alkali lignin, 4-8 parts of anionic surfactant, 2-5 parts of sodium chloride and 6-18 parts of nonionic surfactant.

4. A spinosad suspension concentrate according to claim 3, characterized in that: The anionic surfactant includes a first anionic surfactant and a second anionic surfactant; the mass ratio of the first anionic surfactant to the second anionic surfactant is (1-3):

1.

5. A spinosad suspension concentrate according to claim 4, characterized in that: The anionic surfactant is sodium α-olefin sulfonate.

6. A spinosad suspension concentrate according to claim 3, characterized in that: The nonionic surfactant is coconut oil fatty acid diethanolamide.

7. A spinosad suspension concentrate according to any one of claims 3 to 6, characterized in that: The preparation method of the lignin nanoparticle / surfactant composite material comprises the following steps: dissolving alkali lignin in a solvent, adding the first portion of anionic surfactant and mixing to obtain a lignin concentrate; The lignin concentrate is mixed with a second portion of anionic surfactant, nonionic surfactant and sodium chloride to obtain a lignin nanoparticle / surfactant composite material.

8. A spinosad suspension concentrate according to claim 2, characterized in that: The preparation method of the coating agent comprises the following steps: dissolving zein in a solvent, adding gelatin and mixing to obtain a composite solution; adding glycerol and glucose to the composite solution and mixing them to obtain a modified composite solution; The lignin nanoparticle / surfactant composite material is added to the modified composite solution and mixed to obtain a coating agent.

9. A spinosad suspension concentrate according to claim 1, characterized in that: The emulsifier is at least one of calcium dodecylbenzenesulfonate, phenylphenol polyoxyethylene ether phosphate, styrene polyoxyethylene ether ammonium sulfate, sorbitan trioleate, isomeric decanol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether and castor oil polyoxyethylene ether; The dispersant is at least one of polyethylene glycol, polyvinyl alcohol, polyvinyl pyrrolidone and Tersperse 2500; The wetting agent is at least one of fatty alcohol polyoxyethylene ether, Morwet EFW, isopropyl naphthalene sulfonate and polystyrene polyoxyethylene ether; The thickener is at least one of xanthan gum, carboxymethyl cellulose and magnesium aluminum silicate; The defoaming agent is at least one of an organosilicon defoaming agent, polyalkylsiloxane, mineral oil, fatty alcohol and tributyl phosphate; The antifreeze agent is at least one of ethylene glycol, propylene glycol, glycerol, polyethylene glycol and urea.

10. A method for preparing a spinosad suspension concentrate, characterized in that: The preparation steps are as follows: (1) Weigh the raw materials according to the formula; (2) Using water as a medium, spinosad, an emulsifier, a dispersant, a wetting agent, a thickener, a defoaming agent, an antifreeze agent, and a coating agent are uniformly mixed to obtain an aqueous suspension, and the obtained aqueous suspension is ground and sheared to prepare a spinosad suspension concentrate.

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