A dispersible liquid agent and its preparation method and application
By using polymer emulsifiers and dispersants with hydrophobic and hydrophilic structures in dispersible liquids, the problem of the slippage of the traditional dispersible liquids is solved, and higher efficacy and pesticide utilization are achieved.
Patent Information
- Application Number
- CN202510065906.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-16
- Publication Date
- 2025-04-18
- Estimated Expiration
- 2045-01-16
AI Technical Summary
After dilution, the traditional dispersible liquid agent can easily bounce and slide off the crop leaves, affecting the efficacy of the medicine.
A dispersible liquid agent including a primary drug, a polymer emulsifier having a hydrophobic and hydrophilic structure, and a polymer dispersant are used. After dilution, the liquid agent is adsorbed and precipitated particles through hydrophobic groups, and the particles are suspended by the steric hindrance of the hydrophilic groups, reducing the dynamic surface tension of the drug solution.
It effectively prevents the liquid from bounced and slipped from crop leaves, improves the efficacy of the medicine, and maintains the long-term suspension of the original medicine particles, and improves the utilization rate of pesticides.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of aerial spraying, and in particular to a dispersible liquid agent and a preparation method and application thereof. Background Art
[0002] Dispersible liquid refers to a liquid dosage form in which the original drug that is insoluble or not easily soluble in water is dissolved in a water-soluble or semi-water-soluble solvent and processed in the presence of one or more surfactants / polymers. The diluent obtained after diluting the dosage form with water is neither a solution nor a suspension, but a dispersion with very fine crystals. After diluting with water, it is similar to the solid-liquid dispersion system of a suspension. At the same time, when the traditional dispersible liquid is diluted with water for application, the crystal particle size of the precipitated is 1~10μm, and due to the high density of the crystal, it precipitates quickly, and the supernatant quickly becomes transparent; at the same time, due to the characteristics and polarity of the original drug itself, the strongly polar and easily soluble organic solvent used has a relatively small surface tension, but the surface tension of water is very large. Therefore, when it is diluted with water for miscibility, the surface tension of the diluent will be greatly increased, and it is even greater than the critical surface tension of the crop, resulting in the liquid and the precipitated crystals to easily slide and bounce off the target (crop) surface during application, affecting the efficacy. Summary of the invention
[0003] In view of this, the object of the present invention is to provide a dispersible liquid agent and a preparation method and application thereof. The dispersible liquid agent of the present invention can avoid the problem that the diluted liquid medicine bounces and slides off the crop leaves, thereby affecting the efficacy of the medicine.
[0004] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0005] The present invention provides a dispersible liquid preparation, which comprises, by weight percentage, 2-30% of the original drug, 1-10% of the polymer emulsifier, 1-10% of the polymer dispersant and the balance of an organic solvent;
[0006] The polymer dispersant includes a methacrylic acid main chain with a hydrophobic structure and a polycarboxylate compound with a PEG comb-like structure with a hydrophilic structure;
[0007] The polymer emulsifier includes a block polyether compound of a polyoxypropylene group having a hydrophobic structure and a polyoxyethylene group having a hydrophilic structure.
[0008] Preferably, the mass percentage of the polymer emulsifier is 3-5%, and / or the mass percentage of the polymer dispersant is 3-5%.
[0009] Preferably, the model of the polymer emulsifier is one or more of Ethylan 324, Ethylan NS-500LQ, CEREWINBOP 591B, Tersperse5500, G-5000, PE / L101, B848, AL304, Emulsogen 3510 and Synergen 848.
[0010] Preferably, the polymer dispersant is one or more of Agrilan 755, Agrilan 855, Tersperse 2500, Atlox 4913, GCP01 and DA1349.
[0011] Preferably, the original drug includes neonicotinoid compounds and diprofil;
[0012] The mass ratio of the neonicotinoid compound to diprophyllin is (1-25): (1-5).
[0013] Preferably, the neonicotinoid compound includes one or more of imidacloprid, thiamethoxam, clothianidin, dinotefuran, acetamiprid, thiamethoxam, nitenpyram, chlorpyrifos, pheniramine and cycloheximide.
[0014] Preferably, the organic solvent includes one or more of dimethyl sulfoxide, amide organic solvents, acetone and pyrrolidone substances.
[0015] Preferably, the amide organic solvent includes one or more of dimethylformamide, dimethylacetamide, dimethylpropionamide, hexamethylphosphoramide and dimethylacrylamide;
[0016] The pyrrolidone substances include one or more of N-methylpyrrolidone, N-ethylpyrrolidone, N-butylpyrrolidone, N-octylpyrrolidone and alkane derivatives, and the models of the alkane derivatives include 8000M and / or 8000C.
[0017] The present invention also provides a method for preparing the dispersible liquid according to the above technical solution, comprising the following steps:
[0018] After the neonicotinoid compound, diprofil and an organic solvent are mixed under shear conditions, a polymer emulsifier and a polymer dispersant are added to obtain the dispersible liquid.
[0019] The present invention also provides the use of the dispersible liquid agent described in the above technical solution or the dispersible liquid agent prepared by the preparation method described in the above technical solution in the field of aerial spraying.
[0020] The invention provides a dispersible liquid preparation, which comprises, by weight percentage, 2-30% of a technical drug, 1-10% of a polymer emulsifier, 1-10% of a polymer dispersant and a balance of an organic solvent; the polymer dispersant comprises a methacrylic acid main chain having a hydrophobic structure and a polycarboxylate compound having a PEG comb-like structure having a hydrophilic structure; the polymer emulsifier comprises a block polyether compound of a polyoxypropylene group having a hydrophobic structure and a polyoxyethylene group having a hydrophilic structure.
[0021] The methacrylic acid main chain with a hydrophobic structure in the polymer dispersant and the polyoxypropylene group with a hydrophobic structure in the polymer emulsifier used in the present invention can be effectively adsorbed on the surface of the effective ingredient (that is, the original drug, which is mostly hydrophobic), and the comb-like structure of the PEG with a hydrophilic structure in the polymer dispersant and the polyoxyethylene group with a hydrophilic structure in the polymer emulsifier can provide steric hindrance and good water solubility; the original drug molecules can be dissolved in both organic solvents and water, and the emulsifier function is played at the preparation end (before dilution) to ensure that the physical and chemical indicators of the dispersible liquid are qualified. When diluted with water, the original drug particles are captured by the hydrophobic group during the precipitation process from the organic solvent and firmly adsorbed on the surface of the precipitated particles, and then the ions are dispersed by the steric hindrance of the hydrophilic group, and the function of the dispersant is played to prevent the particles from agglomerating and precipitating quickly, and the particles can be kept suspended for a long time without obvious precipitation. With the continuous precipitation of the original drug particles, the appearance of the diluted liquid gradually changes from transparent to translucent to opaque (the particle size of the original drug particles reaches the range of 500-700nm). At the same time, the present invention uses the above-mentioned polymer emulsifier with a polyether structure to accelerate the directional arrangement of the emulsifier on the oil-water interface and quickly reach the critical micelle concentration, which can significantly reduce the dynamic surface tension of the formed drug solution within 1000ms, and the polyoxypropylene group therein firmly adsorbs the precipitated original drug crystals and adheres to the surface of the target crop, making it easier to achieve the wetting and spreading effect, thereby improving the efficacy.
[0022] Compared with the prior art, the technical solution of the present invention also has the following beneficial effects:
[0023] 1) After dilution, the dispersible liquid of the present invention changes from transparent to translucent to opaque emulsion, the particle size reaches nanometer level, and can remain suspended for up to 24 hours, with higher pesticide utilization rate, while the traditional dispersible liquid will have floating oil or original drug particles naturally precipitated within a specified time;
[0024] 2) The dispersion stability and particle size of the dispersible liquid of the present invention are superior to similar products on the market. 90The particle size of the microparticles is 500~700nm, and the suspension rate is ≥99%. Because the physical suspension rate is higher, the long-term suspension of the original drug particles is more conducive to long-term continuous application of the drug, and the precipitation of the original drug crystals will not cause uneven application of the drug, affecting the efficacy or even causing drug damage;
[0025] 3) The dispersible liquid agent of the present invention can significantly reduce the dynamic surface tension value of the liquid medicine, making it easier to wet, spread and adhere to the surface of the target crop, thereby improving the control effect;
[0026] 4) The dispersible liquid agent of the present invention is more environmentally friendly and safer. The original drug particles of the diluted liquid are controlled at the nanometer level. It has higher prevention effect than the traditional dispersible liquid agent, is not easy to block the nozzle, and is more suitable for the field of aerial spraying. DETAILED DESCRIPTION
[0027] The present invention provides a dispersible liquid preparation, which comprises, by weight percentage, 2-30% of the original drug, 1-10% of the polymer emulsifier, 1-10% of the polymer dispersant and the balance of an organic solvent;
[0028] The polymer dispersant includes a methacrylic acid main chain with a hydrophobic structure and a polycarboxylate compound with a PEG comb-like structure with a hydrophilic structure;
[0029] The polymer emulsifier includes a block polyether compound of a polyoxypropylene group having a hydrophobic structure and a polyoxyethylene group having a hydrophilic structure.
[0030] In the present invention, unless otherwise specified, all preparation raw materials are commercially available products well known to those skilled in the art.
[0031] According to the percentage by mass, the dispersible liquid of the present invention comprises 2-30% of the original drug, more preferably 5-25%. In an embodiment of the present invention, the percentage by mass of the original drug may be 18%, 26%, 6% or 30%.
[0032] In the present invention, the technical drug preferably includes a neonicotinoid compound and abicyclopyrin, and the mass ratio of the neonicotinoid compound to abicyclopyrin is preferably (1-25): (1-5), more preferably (5-20): (2-4). In an embodiment of the present invention, the mass ratio of the neonicotinoid compound to abicyclopyrin may be 5:1, 25:1 or 1:5.
[0033] In the present invention, the neonicotinoid compound preferably includes one or more of imidacloprid, thiamethoxam, clothianidin, dimethoprim, acetamiprid, thiacloprid, nitenpyram, chlorothiazide, pyraclostrobin and cyclohexanil. In an embodiment of the present invention, the neonicotinoid compound may be imidacloprid, dimethoprim, nitenpyram, pyraclostrobin, clothianidin, acetamiprid, thiacloprid, chlorothiazide or cyclohexanil.
[0034] In the present invention, controlling the dosage of neonicotinoid compounds and diprofilin within the above range for combined use can further ensure the stability of physical and chemical indexes while achieving the purpose of insecticidal synergy.
[0035] According to the percentage by mass, the dispersible liquid of the present invention comprises 1-10%, preferably 2-8%, of a polymer emulsifier. The polymer emulsifier comprises a block polyether compound of a polyoxypropylene group having a hydrophobic structure and a polyoxyethylene group having a hydrophilic structure, and the HLB value of the polymer emulsifier is preferably 7-9. In the present invention, the model of the polymer emulsifier is preferably one or more of Ethylan 324 (purchased from Nouryon), Ethylan NS-500LQ (purchased from Nouryon), CEREWIN BOP 591B (purchased from Sasol), Tersperse5500 (purchased from Indorama), G-5000 (purchased from Croda), PE / L101 (purchased from Croda), B848 (purchased from Solvay), AL304 (purchased from Solvay), Emulsogen 3510 (purchased from Clariant) and Synergen 848 (purchased from Clariant). When the model of the high molecular weight emulsifier is two or more of the above specific options, the present invention has no special limitation on the ratio of the above specific substances, and they can be mixed in any ratio. In an embodiment of the present invention, the polymer emulsifier may be Sasol CEREWIN BOP 591B, Clariant Synergen 848 or Indorama Tersperse 5500. In an embodiment of the present invention, the mass percentage of the polymer emulsifier may be 4%, 5%, 3%, 10% or 1%.
[0036] According to the mass percentage, the dispersible liquid agent of the present invention includes 1-10% of the polymer dispersant, preferably 2-8%, and more preferably 3-5%. In the present invention, the polymer dispersant includes a methacrylic acid main chain with a hydrophobic structure and a polycarboxylate compound with a PEG comb structure with a hydrophilic structure. In the present invention, the model of the polymer dispersant is one or more of Agrilan 755 (purchased from Nouryon), Agrilan855 (purchased from Nouryon), Tersperse2500 (purchased from Indorama), Atlox4913 (purchased from Croda), GCP01 (purchased from Livago) and DA1349 (purchased from Solvay). When the polymer dispersant is two or more of the above-mentioned specific selections, the present invention does not have any special restrictions on the ratio of the above-mentioned specific substances, and can be mixed in any ratio. In an embodiment of the present invention, the polymer dispersant can be Nouryon Agrilan855 or Nouryon Agrilan755. In an embodiment of the present invention, the mass percentage of the polymer dispersant may be 10%, 1%, 5%, 3% or 4%.
[0037] In terms of mass percentage, the dispersible liquid of the present invention includes a balance of organic solvents. In the present invention, the organic solvent preferably includes one or more of dimethyl sulfoxide, amide organic solvents, acetone and pyrrolidone substances; the amide organic solvent preferably includes one or more of dimethylformamide, dimethylacetamide, dimethylpropionamide, hexamethylphosphoramide and dimethylacrylamide; the pyrrolidone substance preferably includes one or more of N-methylpyrrolidone, N-ethylpyrrolidone, N-butylpyrrolidone, N-octylpyrrolidone and alkane derivatives, and the model of the alkane derivative preferably includes 8000M and / or 8000C (purchased from Indorama); when the organic solvent is two or more of the above-mentioned specific selections, the present invention does not have any special restrictions on the ratio of the above-mentioned specific substances, and can be mixed in any ratio. In an embodiment of the present invention, the organic solvent may be N-butylpyrrolidone, dimethylacetamide, N-octylpyrrolidone, 8000C, 8000M or dimethylpropionamide.
[0038] In the present invention, the organic solvent is more environmentally friendly and safer.
[0039] In the present invention, the dispersible liquid is used for aerial spraying, and the D 90 The particle size of the microparticles is 500~700nm, and the suspension rate is ≥99%.
[0040] The present invention also provides a method for preparing the dispersible liquid according to the above technical solution, comprising the following steps:
[0041] After the neonicotinoid compound, diprofil and an organic solvent are mixed under shear conditions, a polymer emulsifier and a polymer dispersant are added to obtain the dispersible liquid.
[0042] The present invention does not have any special limitation on the shearing process, and the shearing process may be performed using a process well known to those skilled in the art.
[0043] The present invention does not have any special limitation on the process of adding the polymer emulsifier and the polymer dispersant, and the process well known to those skilled in the art can be used.
[0044] After adding the polymer emulsifier and the polymer dispersant, stirring is preferably also included. The stirring process of the present invention is not particularly limited. The process well known to those skilled in the art can be used to ensure that a transparent liquid is obtained.
[0045] The present invention also provides the use of the dispersible liquid agent described in the above technical solution or the dispersible liquid agent prepared by the preparation method described in the above technical solution in the field of aerial spraying.
[0046] In the present invention, the application field is preferably the field of controlling wheat aphids.
[0047] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0048] Example 1
[0049] Components of the dispersible liquid: calculated by mass percentage, including 15% imidacloprid, 3% acyclovir, 1% polymer emulsifier CEREWIN BOP 591B, 10% polymer dispersant Agrilan 855 and the balance dimethylacetamide;
[0050] Preparation method of dispersible liquid: put imidacloprid, cypermethrin and dimethylacetamide into a stirring tank and shear and mix them evenly until they are completely dissolved and transparent, then add polymer emulsifier CEREWIN BOP 591B and polymer dispersant Agrilan 855, stir until transparent, and obtain the dispersible liquid.
[0051] Example 2
[0052] Components of the dispersible liquid: calculated by mass percentage, including 25% imidacloprid, 1% dimethoate, 10% polymer emulsifier Clariant Synergen 848, 1% polymer dispersant Nouryon Agrilan755 and the balance dimethylacetamide;
[0053] The preparation method of the dispersible liquid is shown in Example 1.
[0054] Example 3
[0055] Components of the dispersible liquid: calculated by mass percentage, including 1% imidacloprid, 5% dimethoate, 5% polymer emulsifier Tersperse 5500, 5% polymer dispersant Agrilan 755, and the balance dimethylacetamide;
[0056] The preparation method of the dispersible liquid is shown in Example 1.
[0057] Example 4
[0058] Components of the dispersible liquid: calculated by mass percentage, including 15% of dinotefuran, 3% of abiprofen, 1% of Clariant Synergen 848, 1% of Nouryon Agrilan 855, and the balance of dimethylpropionamide;
[0059] The preparation method of the dispersible liquid is shown in Example 1.
[0060] Example 5
[0061] Components of the dispersible liquid: calculated by mass percentage, including 25% of dinotefuran, 1% of abiraterone, 10% of polymer emulsifier Tersperse 5500, 1% of polymer dispersant Agrilan 755 and the balance of dimethylpropionamide;
[0062] The preparation method of the dispersible liquid is shown in Example 1.
[0063] Example 6
[0064] Components of the dispersible liquid: calculated by mass percentage, including 1% of dinotefuran, 5% of abiprofen, 5% of polymer emulsifier CEREWIN BOP 591B, 5% of polymer dispersant Agrilan 755, and the balance of dimethylpropionamide;
[0065] The preparation method of the dispersible liquid is shown in Example 1.
[0066] Example 7
[0067] Components of the dispersible liquid: calculated by mass percentage, including 15% nitenpyram, 3% abipyridin, 3% polymer emulsifier CEREWIN BOP 591B, 3% polymer dispersant Agrilan 855, and the balance N-butylpyrrolidone;
[0068] The preparation method of the dispersible liquid is shown in Example 1.
[0069] Example 8
[0070] Components of the dispersible liquid: calculated by mass percentage, including 25% of bispyribac, 5% of dimethoate, 5% of Clariant Synergen 848, 5% of Nouryon Agrilan755, and the balance of N-octylpyrrolidone;
[0071] The preparation method of the dispersible liquid is shown in Example 1.
[0072] Example 9
[0073] The components of the dispersible liquid preparation include, by weight percentage, 25% clothianidin, 1% acyclovir, 4% high molecular weight emulsifier Tersperse 5500, 4% high molecular weight dispersant Agrilan 855, and the balance 8000M.
[0074] The preparation method of the dispersible liquid is shown in Example 1.
[0075] Example 10
[0076] Components of the dispersible liquid: calculated by mass percentage, including 25% acetamiprid, 1% acyclovir, 4% polymer emulsifier CEREWIN BOP 591B, 4% polymer dispersant Agrilan755 and the balance 8000C;
[0077] The preparation method of the dispersible liquid is shown in Example 1.
[0078] Embodiment 11
[0079] Components of the dispersible liquid: calculated by mass percentage, including 25% of thiamethoxam, 1% of dimethomorph, 4% of polymer emulsifier Tersperse 5500, 4% of polymer dispersant Agrilan 855, and the balance of N-butylpyrrolidone;
[0080] The preparation method of the dispersible liquid is shown in Example 1.
[0081] Example 12
[0082] Components of the dispersible liquid: calculated by mass percentage, including 25% of cycloheximide, 1% of dimethoate, 4% of polymer emulsifier CEREWIN BOP 591B, 4% of polymer dispersant Agrilan 755, and the balance of N-octyl pyrrolidone;
[0083] The preparation method of the dispersible liquid is shown in Example 1.
[0084] Example 13
[0085] Components of the dispersible liquid: calculated by mass percentage, including 25% of thiacloprid, 1% of abicyclopyrifos, 4% of Clariant Synergen 848, 4% of Nouryon Agrilan 855, and the balance of dimethylacetamide;
[0086] The preparation method of the dispersible liquid is shown in Example 1.
[0087] Embodiment 14
[0088] Components of the dispersible liquid: calculated by mass percentage, including 25% of chlorpyrifos, 1% of diprofen, 4% of polymer emulsifier Tersperse 5500, 4% of polymer dispersant Agrilan 755, and the balance of N-butylpyrrolidone;
[0089] The preparation method of the dispersible liquid is shown in Example 1.
[0090] Comparative Example 1
[0091] The components of the dispersible liquid preparation include, by weight percentage, 15% imidacloprid, 3% diprofen, 8% sodium dodecylbenzenesulfonate and the balance dimethylacetamide;
[0092] The preparation method of the dispersible liquid agent is as follows: imidacloprid, dicyclopentadien and dimethylacetamide are put into a stirring kettle for shear mixing until they are evenly dissolved and transparent, and sodium dodecylbenzene sulfonate is added and stirred until transparent to obtain the dispersible liquid agent.
[0093] Comparative Example 2
[0094] The components of the dispersible liquid preparation include, by weight percentage, 15% dinotefuran, 3% dimethoate, 8% Nongru 601# and the balance dimethylpropionamide;
[0095] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0096] Comparative Example 3
[0097] The components of the dispersible liquid preparation include, by weight percentage, 15% nitenpyram, 3% dimethoate, 8% Nongru 602# and the balance dimethylpropionamide;
[0098] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0099] Comparative Example 4
[0100] The components of the dispersible liquid preparation include, by weight percentage, 15% of bispyribac, 3% of dimethoate, 8% of Nongru 1601#, and the balance of N-butylpyrrolidone;
[0101] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0102] Comparative Example 5
[0103] The components of the dispersible liquid preparation include, by weight percentage, 15% clothianidin, 3% dimethoate, 8% Nongru 1602# and the balance N-butylpyrrolidone;
[0104] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0105] Comparative Example 6
[0106] The components of the dispersible liquid preparation include, by weight percentage, 15% acetamiprid, 3% diprofen, 8% sodium dodecylbenzenesulfonate and the balance N-octylpyrrolidone;
[0107] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0108] Comparative Example 7
[0109] The components of the dispersible liquid preparation include, by weight percentage, 15% thiamethoxam, 3% aprotinin, 8% Nongru 601# and the balance 8000M;
[0110] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0111] Comparative Example 8
[0112] The components of the dispersible liquid preparation include, by weight percentage, 15% of cycloheximide, 3% of dimethoate, 8% of Nongru 1602# and the balance of 8000C;
[0113] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0114] Comparative Example 9
[0115] The components of the dispersible liquid preparation include, by weight percentage, 15% of thiacloprid, 3% of dimethoate, 8% of sodium maleate sulfate, and the balance of 8000M;
[0116] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0117] Comparative Example 10
[0118] The components of the dispersible liquid preparation include, by weight percentage, 15% of chlorthiocarb, 3% of dimethoate, 8% of lauryl polyoxyethylene ether formaldehyde condensate sulfate and the balance of 8000C;
[0119] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0120] Comparative Example 11
[0121] The components of the dispersible liquid preparation include, by weight percentage, 15% imidacloprid, 3% dimethoate, 5% high molecular weight emulsifier CEREWIN BOP 591B and the balance dimethylacetamide;
[0122] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0123] Comparative Example 12
[0124] The components of the dispersible liquid preparation include, by weight percentage, 25% imidacloprid, 1% dimethoate, 5% high molecular weight dispersant Agrilan 755 and the balance dimethylacetamide;
[0125] The preparation method of the dispersible liquid is referred to Comparative Example 1.
[0126] Test Case
[0127] The dispersible liquids described in Examples 1 to 14 and Comparative Examples 1 to 12 were subjected to storage stability tests (including hot storage tests and cold storage tests): the hot storage test was stored at 54±2°C for 2 weeks; the cold storage test was stored at 0±2°C for 1 week; the test results showed that the dispersible liquids described in Examples 1 to 14 and Comparative Examples 1 to 12 of the present invention had uniform appearance, no crystals were precipitated at different temperatures, and the hot and cold storage stability was qualified;
[0128] The dispersible liquids described in Examples 1 to 14 and Comparative Examples 1 to 12 were diluted with water and then the particle size was measured using a laser particle size analyzer. The test results are shown in Table 1: The particle size D of the microparticles after dilution of the dispersible liquids described in Examples 1 to 14 90 The particles are evenly distributed between 500 and 700 nm, with a slightly blue transparent to translucent appearance, and finally a white emulsion, with a dispersion stability without obvious floating oil and crystallization; the particle size D of the dispersible liquid agent after dilution in Comparative Examples 1 to 12 is 90 The particle size is between 1 and 10 μm and the distribution is uneven. The appearance is transparent to translucent or white emulsion. The dispersion stability has obvious crystal precipitation or precipitated particles.
[0129] Table 1 Appearance of the dispersible liquid preparations described in Examples 1 to 14 and Comparative Examples 1 to 12 and their appearance after 50-fold dilution
[0130]
[0131] The dispersible liquids described in Examples 1 to 14 and Comparative Examples 1 to 12 were subjected to dispersion stability tests according to the Q / BASF I217-2022 standard. The test results are shown in Tables 2 to 3. As can be seen from Tables 2 to 3, the dispersible liquids described in Test Examples 1 to 14 showed no floating oil (cream) on the upper side and no precipitation on the lower side after the initial dispersion of 0.5 h and the redispersibility of 24.5 h; while the dispersible liquids described in Comparative Examples 1 to 12 showed some floating oil (cream) in the initial dispersion of 0.5 h and the redispersibility of 24.5 h, but both showed ≤2.0 mL of floating oil or precipitation (↓).
[0132] Table 2 Dispersion stability and particle size test results of the dispersible liquids described in Examples 1 to 14
[0133]
[0134] Table 3 Dispersion stability and particle size test results of the dispersible liquids described in Comparative Examples 1 to 12
[0135]
[0136] Dynamic surface tension test:
[0137] The dispersible liquids, diprofenoprene DC and flufenoxuron DC described in Examples 1 to 14 and Comparative Examples 1 to 12 were diluted 50 times for simulated aerial spraying in the field, and the dilutions were tested with a dynamic surface tension meter. The test results are shown in Table 4:
[0138] Table 4 Dynamic surface tension test results of the dispersible liquids described in Examples 1 to 14 and Comparative Examples 1 to 12
[0139]
[0140] As shown in Table 4, the dynamic surface tension values of the dilutions of the dispersible liquids described in Examples 1 to 14 are 35.0 to 39.0 mN / m, and the dynamic surface tension values of the dilutions of the dispersible liquids described in Comparative Examples 1 to 12 are 40 to 43 mN / m except for Comparative Example 11, and the critical surface tension value of wheat is 36.2 to 39.0 mN / m;
[0141] In summary, the polymer emulsifier and polymer dispersant of the dispersible liquid provided by the present invention can significantly inhibit the growth of crystals when the pesticide dispersible liquid is diluted with water for a period of time, no obvious crystal precipitation is observed, and the dynamic surface tension of the dilution can be reduced. All product indicators meet the national standards during storage at 54±2℃ for 2 weeks and at 0±2℃ for 1 week.
[0142] Application Examples
[0143] Test crop: wheat
[0144] Target: Aphids
[0145] Test reagents: The treatment reagents are the dispersible liquids described in Examples 1 to 14 (experimental groups) and Comparative Examples 1 to 12 (control groups) and an equal amount of water (blank control group);
[0146] Reference criteria: GB / T 17980.79-2004, Guidelines for Field Efficacy Tests of Pesticides (II), Part 79: Insecticides for Control of Wheat Aphids;
[0147] Test method: In April 2024, the test was conducted in Huixian County, Xinxiang City, Henan Province. At the beginning of the outbreak of wheat aphids, the plant protection drone was used to spray the leaves of wheat plants once (the dosage of the active ingredient is shown in Table 5). The dosage of the liquid was 30 liters / hectare. Each treatment was repeated once, and the area of the plot was 3335m 2 . At 3, 7 and 14 days after application, the diagonal five-point sampling method was used to investigate the number of aphids in 10 wheat plants with aphids at each point. The base number of aphids in each plot before treatment should not be less than 500. The insect population base was investigated before the application, and the insect population reduction rate and control effect were calculated after the application. Finally, the statistical test results were analyzed and the difference significance analysis was performed. The test results are shown in Table 5:
[0148] Table 5 Results of field efficacy test on control of wheat aphids in experimental group, control group and blank control group
[0149]
[0150] As shown in Table 5, the control effects of the dispersible liquids of Examples 1 to 14 on wheat aphids are higher than those of the corresponding comparative examples 1 to 12. The main reason is that the particle size D 90In the range of 500-700nm, more drug particles are deposited on the leaves per unit area compared with the corresponding control (particle size: 1-10μm). At the same time, with the addition of polymer emulsifiers, the dynamic surface tension of the liquid medicine is within the critical surface tension range of wheat, which reduces the bounce of the liquid medicine and increases the amount of liquid medicine deposited on the surface of wheat leaves. Therefore, under the conditions of aerial spraying, its control effect has been significantly improved, indicating that when the dispersible liquid agent is sprayed by aerial spraying, the particle size reaches the nanometer level and the dynamic surface tension of the liquid medicine is reduced, which can significantly improve its own control effect.
[0151] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.
Claims
1. A dispersible liquid preparation, characterized in that: According to the percentage by mass, it includes 2-30% of the original drug, 1-10% of the polymer emulsifier, 1-10% of the polymer dispersant and the balance of the organic solvent; The original drugs are neonicotinoid compounds and diprofil; The mass ratio of the neonicotinoid compound to diprofil is (1-25): (1-5); The neonicotinoid compound is imidacloprid, dinotefuran, nitenpyram, bispyribac, clothianidin, thiacloprid, chlorothiazolin or cycloheximide; The model of the polymer emulsifier is CEREWIN BOP 591B, Synergen 848 or Tersperse 5500; The polymer dispersant model is Agrilan855 or Agrilan755; The organic solvent includes one or more of dimethylformamide, dimethylacetamide, dimethylpropionamide, N-methylpyrrolidone, N-ethylpyrrolidone, N-butylpyrrolidone and N-octylpyrrolidone.
2. The method for preparing the dispersible liquid according to claim 1, characterized in that: The following steps are involved: After the neonicotinoid compound, diprofil and an organic solvent are mixed under shear conditions, a polymer emulsifier and a polymer dispersant are added to obtain the dispersible liquid.
3. Use of the dispersible liquid agent according to claim 1 or the dispersible liquid agent prepared by the preparation method according to claim 2 in the field of aerial spraying.
Citation Information
Patent Citations
Synergistic insecticidal composition containing afidopyropen and application of synergistic insecticidal composition
CN111280174A