WO2023207923A1 - 一种含有苯嘧草唑的可分散油悬浮剂及其制备方法 - Google Patents

一种含有苯嘧草唑的可分散油悬浮剂及其制备方法 Download PDF

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WO2023207923A1
WO2023207923A1 PCT/CN2023/090406 CN2023090406W WO2023207923A1 WO 2023207923 A1 WO2023207923 A1 WO 2023207923A1 CN 2023090406 W CN2023090406 W CN 2023090406W WO 2023207923 A1 WO2023207923 A1 WO 2023207923A1
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dispersible oil
parts
methyl
oil suspension
wetting
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PCT/CN2023/090406
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English (en)
French (fr)
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王利
朱艳梅
董垒
赵泳
樊梅云
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南通江山农药化工股份有限公司
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Priority to CA3239234A priority Critical patent/CA3239234A1/en
Priority to AU2023263121A priority patent/AU2023263121A1/en
Publication of WO2023207923A1 publication Critical patent/WO2023207923A1/zh

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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
    • A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2

Definitions

  • the present invention relates to the technical field of A01P13/00, and more specifically, the present invention relates to a dispersible oil suspension containing adifenazole and a preparation method thereof.
  • the compounding of pyrazole and glyphosate has obvious synergistic effects and effectively improves the quick-acting and long-lasting effects. It can be made into dispersible oil suspensions, suspending agents, water emulsions, water-dispersible granules, granules, etc. dosage form. However, the addition of high levels of glyphosate can easily lead to pipe blockage during the production process, and at the same time, the dispersible suspension agent may become creamy and the original drug may decompose.
  • Chinese patent CN113491269A provides a herbicide composition, including acetate, glyphosate, surfactants, pH regulators, structural stabilizers, solvents and oil bases.
  • a herbicide composition including acetate, glyphosate, surfactants, pH regulators, structural stabilizers, solvents and oil bases.
  • the first aspect of the present invention provides a dispersible oil suspension containing acetozolin.
  • the ingredients include: 22-44 parts by weight of glyphosate ammonium salt, 0.5-1.5 parts of pyrazole, 3-8 parts of wetting and dispersing agent, 10-15 parts of emulsifier, 1-2 parts of structural regulator, and make up to 100 parts of solvent.
  • the weight ratio of the glyphosate ammonium salt and acetate is (28-38):1, preferably 33:1.
  • the wetting and dispersing agent is one or more of sulfonates, polycarboxylates, and sulfates.
  • the wetting and dispersing agent is selected from TSC- One or more of 930, SP-OF3498D, GY-EM05, WELOD 461.
  • the emulsifier is selected from one or more of OD21, ODE286, and TSC901.
  • the wetting and dispersing agent is selected from one or more of TSC-930, SP-OF3498D, and GY-EM05; when the emulsifier is ODE286, the wetting and dispersing agent is SP-OF3498D; when the emulsifier is TSC901, the wetting and dispersing agent is SP-OF3498D.
  • the weight ratio of the wetting and dispersing agent to the emulsifier is 5: (11-14), more preferably 5:12.
  • the applicant unexpectedly discovered during the experiment that by selecting a combination of specific types and proportions of emulsifiers and wetting and dispersing agents in this application, in the presence of fewer types of additives, the obtained dispersible oil suspension not only has better Good viscosity, no sanding process and no risk of creaming at room temperature. At the same time, the decomposition rate of pyrazole is reduced after hot and cold storage, which increases the storage period. The applicant believes that the possible reason is the specific wetting and dispersing agent.
  • the system formed with emulsifiers interacts with long carbon chains, and the polar groups carried by specific wetting and dispersing agents and emulsifiers make the comb-shaped structure of the wetting and dispersing agents increase the distance between the original drug molecules.
  • the excellent dispersion stability prevents the release of acetate molecules under extreme conditions.
  • the structure regulator is silica and/or organic bentonite.
  • the structure regulator is white carbon black and organic bentonite in a weight ratio of (1-3):1, more preferably (1-2):1.
  • Dispersed oil suspensions have good dilution stability and long-lasting foaming properties.
  • each molecule is controlled within a three-dimensional structural space, and large and small molecular chains can cooperate with each other to avoid migration between each other over time. With tighter winding, the overall system maintains a more stable viscosity.
  • the solvent in this application is not particularly limited, and those skilled in the art can make routine selections.
  • the solvent is methyl oleate.
  • the dispersible oil suspension containing mefenacet also includes 5-10 parts by weight of a synergist.
  • synergists in this application include anionic surfactants, such as fast penetrating agent T, dioctyl sulfosuccinate sodium salt, sodium isooctyl succinate sulfonate, etc.; anionic non-ionic twin structure sulfonates. ; Nonionic surfactants, such as fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether polyoxypropylene ether, Tween, etc.; decamide substances, etc.
  • anionic surfactants such as fast penetrating agent T, dioctyl sulfosuccinate sodium salt, sodium isooctyl succinate sulfonate, etc.
  • anionic non-ionic twin structure sulfonates such as fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether polyoxypropylene ether, Tween, etc.
  • decamide substances etc.
  • synergist brands in this application can be listed as 3075V, T-100, 245-LQ-(TH), L-1505-LQ-(AP), 4166, etc.
  • the second aspect of the present invention provides a method for preparing a dispersible oil suspension, which includes: mixing afenacetate, a wetting and dispersing agent, an emulsifier, a structural regulator, and a solvent to form an oil phase; adding the oil phase to sand In the mill, after the oil phase is circulated, glyphosate ammonium salt is added for sand grinding.
  • the preparation method of the dispersible oil suspension includes: dissolving azole in methyl oleate, then adding the remaining raw materials and shearing to form a uniform oil phase; passing the sand mill through After adding hot water at 0-50°C, add the oil phase. After the circulation of the oil phase is normal, add glyphosate ammonium salt and sand grind to get it.
  • the weight of glyphosate ammonium salt in the dispersible oil suspension in this application is relatively large.
  • the glyphosate ammonium salt is easy to settle, agglomerate, etc., causing the circulation pipeline to be blocked, and the application People unexpectedly discovered that first, after mixing acetaminophen, specific wetting and dispersing agents, emulsifiers, structural regulators, and solvents in this application, and then after the oil phase is circulated, glufosinate ammonium salt is added. This avoids the need for The problem of pipeline clogging caused by glyphosate ammonium salt, and the processability is good during later sand grinding, and the ideal particle size distribution can be obtained.
  • the present invention has the following beneficial effects:
  • the dispersible oil suspension agent in the present application solves the problem of decomposition of azole in the prior art, and the dispersible oil suspension agent does not have the problem of creaming, has better high and low temperature resistance, and has better dilution stability, long-lasting foaming and suspension rate.
  • Figure 1 is a diagram showing the effect of weed control (Ageratum, Setaria, and Polygonum) 3 days after using the dispersible oil suspension agent of Example 1 of the present application;
  • Figure 2 is a diagram showing the effect of weeding (Ageratum, Setaria, and Polygonum) 7 days after using the dispersible oil suspension agent of Example 1 of the present application;
  • Figure 3 shows the weeding (goosegrass, setaria, bulrush, Imperata, crabgrass, mugwort, annual, small fly, humulus, malan, and blackgrass) 3 days after using the dispersible oil suspension agent of Example 1 of the present application. Mold, root vegetables) renderings;
  • Figure 4 shows the weeding results of 15 days after using the dispersible oil suspension agent of Example 1 of the present application (goosegrass, setaria, reed, Imperata, crabgrass, mugwort, annual, small fly, humulus, malan, and blackgrass). Mold, root vegetables) renderings;
  • Figure 5 shows the weeding (goosegrass, setaria, bulrush, Imperata, crabgrass, mugwort, annual, small fly, humulus, malan, wormwood) 30 days after using the dispersible oil suspension agent of Example 1 of the present application. Mold and root vegetables) renderings.
  • a dispersible oil suspension containing pyrazole the specific ingredients in parts by weight are as follows:
  • the glyphosate ammonium salt is self-made by the company, with a purity of more than 96%; the azole is self-made by the company, with a purity of more than 92%; the wetting and dispersing agent TSC-930 was purchased from Zhuben Oil, and the emulsifier OD21 was purchased from Wuxi Yiyi Jingfeng Technology Co., Ltd.; silica was purchased from Nantong Yelu New Materials Sales Co., Ltd.; organic bentonite was purchased from Zhangjiagang Free Trade Zone Guangxing International Trading Co., Ltd.
  • the preparation method of the dispersible oil suspension is as follows:
  • the oil separation rate test environment was hot storage for 14 days; long-term storage at normal temperature; and no obvious oil separation was found after the hot storage was transferred to normal temperature.
  • the dispersible oil suspension obtained in this example was tested for efficacy:
  • the potted plants were removed from the greenhouse (28 ⁇ 5°C), and the stems and leaves were sprayed. There were three replicates, and a blank control was set up. After treatment, conventional culture is carried out in the greenhouse, and plant reaction symptoms are regularly observed. The fresh weight of the above-ground parts of the weeds is weighed 10 days after treatment, and the fresh weight control effect is calculated. The control effect of completely dead weeds is calculated as 100%.
  • nectar, purslane, goosegrass, crabgrass, and barnyard grass all reach over 90.0%.
  • a dispersible oil suspension containing pyrazole the specific ingredients are the same as in Example 1, the difference is that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent SP-OF3494D, purchased from Jiangsu Qingyu Chemical Technology Ltd.
  • the preparation method of the dispersible oil suspension containing pyrazole is the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent SP-OF3494D.
  • a dispersible oil suspension containing benzofen the specific ingredients are the same as in Example 1, except that 0.5 part of organic bentonite is used.
  • the preparation method of the dispersible oil suspension containing mefenacetate is the same as in Example 1.
  • a dispersible oil suspension containing pyrazole the specific ingredients are the same as in Example 1, except that 5 parts of the wetting and dispersing agent TSC-930 and 12 parts of the emulsifier OD21 are replaced with 17 parts of Huntsman WELOD 461 .
  • the preparation method of the dispersible oil suspension agent is the same as in Example 1, except that the wetting and dispersing agent TSC-930 and the emulsifier OD21 are replaced with 461.
  • a dispersible oil suspension containing pyrazole the specific ingredients are the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent SP-OF3498D.
  • the preparation method of the dispersible oil suspension is the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent SP-OF3498D, and in step (2), it is sanded until the particle size D97 is 2.824 ⁇ m.
  • a dispersible oil suspension containing pyrazole the specific ingredients are the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent SP-OF3498D, and the emulsifier OD21 is replaced by ODE286.
  • the preparation method of the dispersible oil suspension is the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent SP-OF3498D, and the emulsifier OD21 is replaced by ODE286.
  • a dispersible oil suspension containing pyrazole the specific ingredients are the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent SP-OF3498D, and the emulsifier OD21 is replaced by TSC901.
  • the preparation method of the dispersible oil suspension is the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent 3498D, the emulsifier OD21 is replaced by TSC901, and the particle size D97 is sanded to 2.577 ⁇ m.
  • a dispersible oil suspension containing pyrazole the specific ingredients are the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent GY-EM05.
  • the preparation method of the dispersible oil suspension agent is the same as in Example 1, except that the wetting and dispersing agent TSC-930 is replaced by the wetting and dispersing agent GY-EM05, and the particle size D97 is sanded to 2.458 ⁇ m.
  • a dispersible oil suspension containing pyrazole the specific ingredients are the same as in Example 1.
  • the preparation method of the dispersible oil suspension agent is the same as in Example 1, except that in step (2), it is sanded until D97 is 2.787 ⁇ m.
  • Example 4 The test results of Example 4 to Example 9 are shown in Table 2.
  • Example 1 the test methods of viscosity, dilution stability and long-lasting foaming property are the same as those in Example 1.
  • the suspension rate test method or test standard is to use standard hard water to prepare the test sample into a suspension of appropriate concentration. Under the specified conditions, let it stand in the measuring cylinder for a certain period of time, and measure the mass of the active ingredients in the bottom tenth of the suspension and sediment.
  • Example 9 During the test, the dilution stability of the dispersible oil suspension obtained in Example 5 and Example 9 was qualified, and the dispersibility of the dispersible oil suspension obtained in Example 9 was better than that of the dispersible oil suspension obtained in Example 5. , the dispersible oil suspension agent of Example 9 was dispersed in the form of cloud.
  • Embodiments 10-15 provide a dispersible oil suspension agent.
  • the specific ingredients are the same as in Embodiment 1.
  • the difference is that the contents of white carbon black and organic bentonite are different.
  • the specific implementation method of the preparation method is the same as in Embodiment 1.
  • the difference is that the particle size D97 is different, see Table 3 for details.
  • Examples 16-26 provide a dispersible oil suspension agent.
  • the specific ingredients are the same as those in Example 1. The difference is that the types of wetting and dispersing agents and emulsifiers are different. See Table 4 for details.
  • a dispersible oil suspension containing pyrazole The specific ingredients are the same as in Example 1. The difference is that the types of wetting and dispersing agents and emulsifiers are different. See Table 5 for details.
  • the preparation method and specific implementation are the same as those in Example 1, except that the corresponding wetting and dispersing agents and emulsifiers are added.
  • Example 5 The formulas of Example 5 and Example 28 of the present application are the same, the test results fluctuate within a reasonable range, and the test results are stable.
  • a dispersible oil suspension The specific ingredients are the same as those in Example 1. The difference is that the glyphosate ammonium salt is glyphosate acid, and the wetting and dispersing agents and emulsifiers are different.
  • the ingredients also include a stabilizer, sodium polyphosphate, See table for details 6.

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Abstract

本发明涉及A01P13/00技术领域，更具体地，本发明涉及一种含有苯嘧草唑的可分散油悬浮剂及其制备方法。含有苯嘧草唑的可分散油悬浮剂，按重量份计，成分包括：草甘膦铵盐22-44份，苯嘧草唑0.5-1.5份，润湿分散剂3-8份，乳化剂10-15份，结构调节剂1-2份，溶剂补足至100份。本申请中可分散油悬浮剂解决了现有技术中苯嘧草唑分解的问题，且该可分散油悬浮剂未出现膏化的问题，具有较好的耐高、低温性，且具有较佳的稀释稳定性、持久起泡性和悬浮率。

Description

一种含有苯嘧草唑的可分散油悬浮剂及其制备方法 技术领域
本发明涉及A01P13/00技术领域，更具体地，本发明涉及一种含有苯嘧草唑的可分散油悬浮剂及其制备方法。
背景技术
苯嘧草唑和草甘膦复配，具有明显的增效作用，有效提高速效性和持效性，可以制成可分散油悬浮剂、悬浮剂、水乳剂、水分散粒剂、颗粒剂等剂型。然而高含量的草甘膦的加入，在生产过程中容易出现管道堵塞，同时可分散悬浮剂出现膏化、原药分解的问题。
中国专利CN113491269A提供了一种除草剂组合物，包括苯嘧草唑、草甘膦、表面活性剂、pH调节剂、结构稳定剂、溶剂和油基，然而其在生产过程中的放大实验中其也存在膏化的风险，且其成分种类繁多，造成生产效率的下降，同时根据其原料和制备方法，会出现管道堵塞的问题。
因此，需要提供一种含有苯嘧草唑和草甘膦铵盐的可分散油悬浮剂，降低原料种类，解决膏化、管道堵塞等问题。
发明内容
针对现有技术中存在的一些问题，本发明第一个方面提供了一种含有苯嘧草唑的可分散油悬浮剂，按重量份计，成分包括：草甘膦铵盐22-44份，苯嘧草唑0.5-1.5份，润湿分散剂3-8份，乳化剂10-15份，结构调节剂1-2份，溶剂补足至100份。
在一种实施方式中，所述草甘膦铵盐和苯嘧草唑的重量比为(28-38)：1，优选为33：1。
在一种实施方式中，所述润湿分散剂为磺酸盐类、聚羧酸盐类、硫酸盐类分散剂中一种或多种，优选的，所述润湿分散剂选自TSC-930、SP-OF3498D、GY-EM05、WELOD 461中一种或多种。
在一种实施方式中，所述乳化剂选自OD21、ODE286、TSC901中一种或多种。
在一种实施方式中，当乳化剂为OD21时，润湿分散剂选自TSC-930、SP-OF3498D、GY-EM05中一种或多种；当乳化剂为ODE286时，润湿分散剂为 SP-OF3498D；当乳化剂为TSC901时，润湿分散剂为SP-OF3498D。
优选的，所述润湿分散剂和乳化剂的重量比为5：(11-14)，更优选为5:12。
申请人在实验中意外的发现，选择本申请中特定种类和配比的乳化剂和润湿分散剂的组合，在较少种类助剂存在的条件下，得到的可分散油悬浮剂不仅具有较好的粘度，无砂磨过程和常温下膏化的风险，同时热贮和冷贮后苯嘧草唑的分解率降低，提高了贮存期，申请人认为可能的原因是特定的润湿分散剂和乳化剂形成的体系，长碳链之间作用，且特定的润湿分散剂和乳化剂，其携带的极性基团使得其润湿分散剂的梳形结构增大了原药分子之间的分散稳定性，避免了在极端条件下，苯嘧草唑分子的脱出。
在一种实施方式中，所述结构调节剂为白炭黑和/或有机膨润土。
优选的，所述结构调节剂为重量比为(1-3)：1的白炭黑和有机膨润土，更优选为(1-2)：1。
申请人在实验中发现，在本申请中特定的助剂存在的条件下，得到的可分散油悬浮剂会有少量的固体聚集在底部，而添加有机膨润土后，仍有少量的固体聚集在底部，本领域技术人员为了解决固体聚集的情况下，往往通过调试加入的助剂，提高原药成分的分散性，而申请人发现，一旦调节本申请中特定的助剂，则会造成较高的析油率以及热贮、冷贮条件下的苯嘧草唑的分解问题，申请人在实验中意外的发现，当结构调节剂为重量比为(1-2)：1的白炭黑和有机膨润土时，和本申请中特定润湿分散剂和乳化剂助剂复合的条件下，得到的可分散油悬浮剂不仅无固体聚集底部，同时未能影响本申请中可分散油悬浮剂的析油性和耐冷、耐热性，避免了结构调节剂对析油、耐冷和耐热性的影响，申请人认为可能的原因是该特定重量比的白炭黑和有机膨润土，在本申请中特定的润湿分散剂和乳化剂存在的条件下，在油酸甲酯溶剂中形成的三维结构，维持一定的粘度，又不会有膏化的风险。
此外，申请人意外的发现，本申请中特定结构调节剂、润湿分散剂、乳化剂的结合，同时在本申请中特定制备方法，在单一溶剂油酸甲酯存在的条件下，得到的可分散油悬浮剂局具有较好的稀释稳定性和持久起泡性，申请人认为各个分子被控制在三维结构空间内，且大小分子链之间能够相互配合，避免随着时间的迁移彼此之间更为紧密的缠绕，整体的体系保持较为稳定的粘度。
此外，申请人意外的发现，即使不添加额外的快速渗透剂、其他的表面活性剂等，本申请中得到的可分散悬浮剂具有较佳的分散、渗透性、润湿性、粘附性、靶标附着性、抗蒸腾性、铺展性等。
本申请中溶剂不做特别限定，本领域技术人员可做常规选择。在一种优选的实施方式中，所述溶剂为油酸甲酯。
在一种实施方式中，所述含有苯嘧草唑的可分散油悬浮剂还包括5-10重量份增效剂。
本申请中增效剂可以列举的有阴离子表面活性剂，例如快速渗透剂T、磺化琥珀酸二辛酯钠盐、琥珀酸尔异辛酯磺酸钠等；阴非离子双生结构磺酸盐；非离子表面活性剂，例如脂肪醇聚氧乙烯醚、脂肪醇聚氧乙烯醚聚氧丙烯醚、吐温等；癸酰胺类物质等。
本申请中增效剂牌号可以列举的有3075V、T-100、245-LQ-(TH)、L-1505-LQ-(AP)、4166等。
本发明第二个方面提供了一种可分散油悬浮剂的制备方法，包括：将苯嘧草唑、润湿分散剂、乳化剂、结构调节剂、溶剂混合形成油相；将油相加入砂磨机中，油相循环后加入草甘膦铵盐，进行砂磨。
在一种实施方式中，所述可分散油悬浮剂的制备方法，包括：将苯嘧草唑溶解在油酸甲酯中，然后添加剩余的原料剪切后形成均匀油相；砂磨机通0-50℃热水后，加入油相，待油相循环正常后，加入草甘膦铵盐进行砂磨，即得。
申请人在实验中发现，在本申请中可分散油悬浮剂中草甘膦铵盐重量占比较多，在制备过程中，草甘膦铵盐容易沉降、结块等导致循环管道堵塞，而申请人意外的发现，首先将本申请中苯嘧草唑、特定的润湿分散剂、乳化剂、结构调节剂、溶剂混合后，待油相循环后，加入草铵膦铵盐，此时避免了草甘膦铵盐导致的管道堵塞的问题，且后期进行砂磨时加工性好，可得到理想的粒径分布，申请人认为可能的原因是在本申请中形成的油相中加入草甘膦铵盐，此时油相的流动性可以很好的将草甘膦铵盐在加入后的初期进行分散循环中，避免了局部的草甘膦铵盐的沉降导致管道堵塞，此外，该方法得到的可分散油悬浮剂倾倒后残余物少。
本发明与现有技术相比具有以下有益效果：
本申请中可分散油悬浮剂解决了现有技术中苯嘧草唑分解的问题，且该可分散油悬浮剂未出现膏化的问题，具有较好的耐高、低温性，且具有较佳的稀释稳定性、持久起泡性和悬浮率。
附图说明
图1为使用本申请实施例1可分散油悬浮剂药后3天的除草(藿香蓟、狗尾草、水蓼)效果图；
图2为使用本申请实施例1可分散油悬浮剂药后7天的除草(藿香蓟、狗尾草、水蓼)效果图；
图3为使用本申请实施例1可分散油悬浮剂药后3天的除草(牛筋草、狗尾草、芦苇、白茅、马唐、艾草、一年蓬、小飞蓬、葎草、马兰、乌蔹霉、扯根菜)效果图；
图4为使用本申请实施例1可分散油悬浮剂药后15天的除草(牛筋草、狗尾草、芦苇、白茅、马唐、艾草、一年蓬、小飞蓬、葎草、马兰、乌蔹霉、扯根菜)效果图；
图5为使用本申请实施例1可分散油悬浮剂药后30天的除草(牛筋草、狗尾草、芦苇、白茅、马唐、艾草、一年蓬、小飞蓬、葎草、马兰、乌蔹霉、扯根菜)效果图。
具体实施方式
以下通过具体实施方式说明本发明，但不局限于以下给出的具体实施例。
实施例1
一种含有苯嘧草唑的可分散油悬浮剂，按重量份计，具体成分如下：
草甘膦铵盐33份，苯嘧草唑1份，润湿分散剂TSC-930 5份，乳化剂OD21 12份，白炭黑1份，有机膨润土1份，油酸甲酯补足至100份。
其中，草甘膦铵盐为公司自制，纯度为96％以上；苯嘧草唑为公司自制，纯度为92％以上；润湿分散剂TSC-930购自竹本油脂，乳化剂OD21购自无锡颐景丰科技有限公司；白炭黑购自南通市叶律新材料销售有限公司；有机膨润土购自张家港保税区广兴国际贸易有限公司。
该可分散油悬浮剂的制备方法如下：
(1)将苯嘧草唑溶解在油酸甲酯中，然后添加剩余的原料，高速剪切机5 档剪切5min形成均匀油相备用。
(2)卧式砂磨机通50℃热水，按比例先将油相投入，循环正常后加入草甘膦铵盐，砂磨至粒径D97为6.235μm，D10为0.527μm，D50为1.090μm，D90为3.446μm。
对该实施例得到的可分散油悬浮剂进行测试，测试结果见表1。
表1
备注：析油率测试环境为热贮14天；常温长期放置；热贮转常温，均未见明显析油。
对该实施例得到的可分散油悬浮剂进行药效测试：
室内试验如下：
【试验杂草】茼麻、马齿觅、牛筋草、马唐、稗草
【试验单位】浙江农林大学绿色农药协同创新中心(陈杰)
【试验方法】
温室盆栽去(28±5℃),茎叶喷雾处理，设3次重复，另设空白对照。处理后置温室中进行常规培养，定时观察植株反应症状，并于药后10天称取杂草地上部分鲜重，计算鲜重防效，已完全枯死的杂草防效按100％计算。
【试验结果】
茼麻、马齿觅、牛筋草、马唐、稗草的除草性均达到90.0％以上。
田间试验如下：
试验1
【试验地点】临安市径山镇绿君衣庄
【试验单位】浙江农林大大学绿色农药协同创新中心(陈杰)
【试验时间】2021.07.06-2021.08.05
【制剂用量】190g/亩
【主要杂草】藿香蓟、狗尾草、水蓼，杂草处于成熟结果期，覆盖度80-100％。
【试验结果】
药后3天，显示一定的中毒症状，杂草叶片开始萎蔫，见图1，药后7天，成效显著，见图2。
试验2
【试验地点】江山公司东厂区空地(业务发展部内部人员完成)
【试验时间】2021.8.9-2021.9.8
【制剂用量】180g/亩
【主要杂草】牛筋草、狗尾草、芦苇、白茅、马唐、艾草、一年蓬、小飞蓬、葎草、马兰、乌蔹霉、扯根菜
【试验结果】
药后3天，显示一定的中毒症状，见图3，药后15天，成效显著，见图4，药后30天，杂草几乎除尽，见图5。
实施例2
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂SP-OF3494D，购自江苏擎宇化工科技有限公司。
含有苯嘧草唑的可分散油悬浮剂的制备方法同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂SP-OF3494D。
实施例3
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，有机膨润土0.5份。
含有苯嘧草唑的可分散油悬浮剂的制备方法同实施例1。
实施例2和实施例3的可分散油悬浮剂均未出现明显的析油现象。
实施例4
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂TSC-930 5份和乳化剂OD21 12份替换为亨斯迈WELOD 461 17份。
可分散油悬浮剂的制备方法同实施例1，不同之处在于，将润湿分散剂TSC-930和乳化剂OD21替换为461。
实施例5
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂SP-OF3498D。
可分散油悬浮剂的制备方法同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂SP-OF3498D，步骤(2)中砂磨至粒径D97为2.824μm。
实施例6
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂SP-OF3498D，乳化剂OD21替换为ODE286。
可分散油悬浮剂的制备方法同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂SP-OF3498D，乳化剂OD21替换为ODE286。
实施例7
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂SP-OF3498D，乳化剂OD21替换为TSC901。
可分散油悬浮剂的制备方法同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂3498D，乳化剂OD21替换为TSC901，砂磨至粒径D97为2.577μm。
实施例8
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂GY-EM05。
可分散油悬浮剂的制备方法同实施例1，不同之处在于，润湿分散剂TSC-930替换为润湿分散剂GY-EM05，砂磨至粒径D97为2.458μm。
实施例9
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1。
可分散油悬浮剂的制备方法同实施例1，不同之处在于，步骤(2)中砂磨至D97为2.787μm。
实施例4-实施例9的测试结果如表2。
表2
其中，粘度，稀释稳定性，持久起泡性的测试方法同实施例1。
悬浮率测试方法或测试标准为用标准硬水将待测试样配制成适当浓度的悬浮液。在规定的条件下，于量筒中静置一定时间，测定底部十分之一悬浮液和沉淀物中有效成分质量。
在测试过程中，实施例5和实施例9得到的可分散油悬浮剂的稀释稳定性合格，且实施例9得到的可分散油悬浮剂的分散性优于实施例5的可分散油悬浮剂，实施例9的可分散油悬浮剂呈云雾状分散。
实施例10-15
实施例10-15提供了一种可分散油悬浮剂，具体成分同实施例1，不同之处在于白炭黑和有机膨润土的含量不同，制备方法具体实施方式同实施例1，不同 之处在于粒径D97不同，具体见表3。
表3
实施例16-26
实施例16-26提供了一种可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂和乳化剂的种类不同，具体见表4。
表4

实施例27-33
一种含有苯嘧草唑的可分散油悬浮剂，具体成分同实施例1，不同之处在于，润湿分散剂和乳化剂的种类不同，具体见表5。
制备方法，具体实施方式同实施例1，不同之处在于，加入相应的润湿分散剂和乳化剂不同。
表5
本申请实施例5和实施例28配方相同，其测试结果波动在合理范围内，测试结果稳定。
实施例34-39
一种可分散油悬浮剂，具体成分同实施例1，不同之处在于，草甘膦铵盐为草甘膦酸，润湿分散剂、乳化剂不同，成分还包括稳定剂多聚磷酸钠，具体见表 6。
表6

Claims (10)

  1. 一种含有苯嘧草唑的可分散油悬浮剂，其特征在于，按重量份计，成分包括：草甘膦铵盐22-44份，苯嘧草唑0.5-1.5份，润湿分散剂3-8份，乳化剂10-15份，结构调节剂1-2份，溶剂补足至100份。
  2. 根据权利要求1所述含有苯嘧草唑的可分散油悬浮剂，其特征在于，所述草甘膦铵盐和苯嘧草唑的重量比为(28-38)：1。
  3. 根据权利要求2所述含有苯嘧草唑的可分散油悬浮剂，其特征在于，所述润湿分散剂为磺酸盐类、聚羧酸盐类、硫酸盐类分散剂中一种或多种，优选的，所述润湿分散剂选自TSC-930、SP-OF3498D、GY-EM05、WELOD 461中一种或多种。
  4. 根据权利要求3所述含有苯嘧草唑的可分散油悬浮剂，其特征在于，所述乳化剂选自OD21、ODE286、TSC901中一种或多种。
  5. 根据权利要求4所述含有苯嘧草唑的可分散油悬浮剂，其特征在于，所述润湿分散剂和乳化剂的重量比为5：(11-14)。
  6. 根据权利要求1-5任一项所述含有苯嘧草唑的可分散油悬浮剂，其特征在于，所述结构调节剂为白炭黑和/或有机膨润土。
  7. 根据权利要求6所述含有苯嘧草唑的可分散油悬浮剂，其特征在于，所述结构调节剂为重量比为(1-3)：1的白炭黑和有机膨润土。
  8. 根据权利要求7所述含有苯嘧草唑的可分散油悬浮剂，其特征在于，所述可分散油悬浮剂还包括5-10重量份增效剂。
  9. 一种根据权利要求1-7任一项所述含有苯嘧草唑的可分散油悬浮剂的制备方法，其特征在于，包括：将苯嘧草唑、润湿分散剂、乳化剂、结构调节剂、溶剂、草甘膦铵盐混合后，进行砂磨。
  10. 根据权利要求9所述可分散油悬浮剂的制备方法，其特征在于，包括：将苯嘧草唑、润湿分散剂、乳化剂、结构调节剂、溶剂混合形成油相；将油相加入砂磨机中，油相循环后加入草甘膦铵盐，进行砂磨。
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CN113491269A (zh) 2020-03-20 2021-10-12 沈阳中化农药化工研发有限公司 一种除草剂组合物可分散油悬浮剂及其制备方法
CN113412840A (zh) * 2021-03-22 2021-09-21 南通江山农药化工股份有限公司 一种除草组合物、制剂及其应用
CN115281212A (zh) * 2022-04-27 2022-11-04 南通江山农药化工股份有限公司 一种含有苯嘧草唑的可分散油悬浮剂及其制备方法

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