TWI772416B - A pyraclostrobin water dispersible solid composition and the process for preparing the same - Google Patents

A pyraclostrobin water dispersible solid composition and the process for preparing the same Download PDF

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TWI772416B
TWI772416B TW107115522A TW107115522A TWI772416B TW I772416 B TWI772416 B TW I772416B TW 107115522 A TW107115522 A TW 107115522A TW 107115522 A TW107115522 A TW 107115522A TW I772416 B TWI772416 B TW I772416B
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pyraclostrobin
solid composition
mixture
pulverization
water
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TW201900025A (en
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吳一凡
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大陸商江蘇龍燈化學有限公司
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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
    • 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
    • A01N25/08—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 solids as carriers or diluents
    • 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
    • A01N25/12—Powders or granules
    • A01N25/14—Powders or granules wettable
    • 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
    • A01N25/22—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 ingredients stabilising the active ingredients
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/34—Nitriles
    • 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
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • 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
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The present invention provides a pyraclostrobin water dispersible solid composition comprising the following components by weight percent: 5~50% of pyraclostrobin, 0.1~15% of alkyl sulfonate, 5~80% of porous carrier and 1~45% of functional additives. The present invention also provides a process for preparing the composition, which comprises; firstly proportionately mixing pyraclostrobin with alkyl naphthalene sulfonate; and then roughly comminuting the obtained mixture below 35℃ to obtain a homogeneous mixture; adding a porous carrier and a functional additive in the obtained homogenous mixture; and proceeding a finely comminution to obtain the pyraclostrobin water dispersible solid composition. The pyraclostrobin water dispersible solid composition prepared by the present application has the advantages of good thermal and normal storage stability, no aggregation, no agglomeration, and no blockage of sprayer filter or spray head, thereby it is convenient for users to apply and improve the pesticide efficacy.

Description

一種吡唑醚菌酯水分散固體組合物及其製備方法 A kind of pyraclostrobin water-dispersed solid composition and preparation method thereof

本申請案主張於2017年5月10日提交中國專利局，申請號為201710324705.2，發明名稱為“一種吡唑醚菌酯水分散固體組合物及其製備方法”的中國專利申請的優先權，其全部內容通過引用結合在本申請中。 This application claims the priority of the Chinese patent application filed on May 10, 2017, with the application number of 201710324705.2 and the invention titled "A water-dispersed solid composition of pyraclostrobin and its preparation method". The entire contents of this application are incorporated by reference.

本發明涉及農業化學領域，具體涉及一種水分散固體組合物及其製備方法，尤其涉及一種吡唑醚菌酯水分散固體組合物及其製備方法。 The invention relates to the field of agricultural chemistry, in particular to a water-dispersed solid composition and a preparation method thereof, in particular to a water-dispersed solid composition of pyraclostrobin and a preparation method thereof.

吡唑醚菌酯是由德國巴斯夫公司於1993年開發的兼具吡唑結構的甲氧基丙烯酸酯類殺菌劑，是一種線粒體呼吸抑制劑。它藉由阻止細胞色素b和c1間電子傳遞而抑制線粒體呼吸作用，使線粒體不能產生和提供細胞正常代謝所需要的能量(ATP)，最終導致細胞死亡。 Pyraclostrobin is a methoxyacrylate fungicide with a pyrazole structure developed by BASF in Germany in 1993. It is a mitochondrial respiration inhibitor. It inhibits mitochondrial respiration by preventing electron transfer between cytochrome b and c1, so that mitochondria cannot produce and provide the energy (ATP) required for normal cell metabolism, eventually leading to cell death.

吡唑醚菌酯(pyraclostrobin)化學名稱為：N-[2-[[1-(4-氯苯基)吡唑-3-基]氧甲基]苯基]-N-甲氧基胺基甲酸甲酯，屬於甲氧基丙烯酸酯類廣譜殺菌劑。吡唑醚菌酯可用於小麥、花生、水稻、蔬菜、果樹、煙草、茶樹、觀賞植物、草坪等各種作物，防治子囊菌、擔子菌、半知菌和卵菌綱真菌引 起的葉枯病、銹病、白粉病、霜黴病、疫病、炭疽病、瘡痂病、褐斑病、立枯病等多種病害。目前市面上主要以吡唑醚菌酯乳油、水乳劑產品來使用。然而這些劑型都具有一個共同的缺點，即乳油製劑中含有大量的有機溶劑，其對生態環境和水生生物危害極大。隨著人們對環境保護的意識逐步加強，這類產品必將逐步淘汰。現在各個農化公司都在朝著環保型劑型水劑化、顆粒化產品加大研發力度，逐步開發吡唑醚菌酯的懸浮劑、種衣劑、顆粒劑等劑型，以減少使用有機溶劑對環境的危害。 The chemical name of pyraclostrobin is: N-[2-[[1-(4-chlorophenyl)pyrazol-3-yl]oxymethyl]phenyl]-N-methoxyamino Methyl formate belongs to methoxyacrylate broad-spectrum fungicides. Pyraclostrobin can be used in various crops such as wheat, peanuts, rice, vegetables, fruit trees, tobacco, tea trees, ornamental plants, lawns, etc. to prevent and control Ascomycetes, Basidiomycetes, Deuteromycetes and Oomycetes. Leaf blight, rust, powdery mildew, downy mildew, blight, anthracnose, scab, brown spot, blight and other diseases caused by it. At present, pyraclostrobin EC and water emulsion products are mainly used on the market. However, these formulations all have a common disadvantage, that is, the emulsifiable concentrate formulations contain a large amount of organic solvents, which are extremely harmful to the ecological environment and aquatic organisms. With the gradual strengthening of people's awareness of environmental protection, such products will be phased out. At present, various agrochemical companies are increasing their research and development efforts towards environmentally friendly formulations of water-based and granulated products, and gradually developing pyraclostrobin suspensions, seed coating agents, granules and other formulations to reduce the use of organic solvents. environmental hazards.

但是水分散劑型中，固體製劑例如可濕性粉劑(WP)、水分散顆粒劑(WDG)的粒徑對製劑的穩定性和懸浮率有很大的影響。為了得到粒徑在1~15μm的固體製劑，各種方式的粉碎是必須的。但由於活性物熔點低，尤其是熔點不超過70℃時，直接粉碎是比較困難的，因為在粉碎過程中，活性物很容易被熔化或軟化，最終會導致產品理化品質存在風險，熱貯穩定性和懸浮率不合格等問題。 However, in the water dispersion dosage form, the particle size of solid preparations such as wettable powder (WP) and water dispersible granule (WDG) has a great influence on the stability and suspension rate of the preparation. In order to obtain a solid preparation with a particle size of 1 to 15 μm, various methods of pulverization are necessary. However, due to the low melting point of the active substance, especially when the melting point does not exceed 70°C, it is difficult to directly pulverize it, because during the pulverization process, the active substance is easily melted or softened, which will eventually lead to risks in the physical and chemical quality of the product and stable thermal storage. Sex and suspension rate unqualified and other issues.

吡唑醚菌酯的熔點較低，僅為56~64℃，因而製備成的吡唑醚菌酯組合物存在熱貯後容易團聚結塊的問題。對於長期貯存後的製劑，在農藥噴霧使用時，也會因為團聚結塊的問題導致堵塞過濾器和噴頭，從而給用戶使用帶來不便，且影響了植物對吡唑醚菌酯活性物的吸收，降低了藥效。這些技術困難，使得吡唑醚菌酯水分散製劑沒有得到廣泛使用。 The melting point of pyraclostrobin is relatively low, only 56-64 °C, so the prepared pyraclostrobin composition has the problem of easy agglomeration and agglomeration after thermal storage. For formulations that have been stored for a long time, when the pesticide is used for spraying, the filter and nozzle will be blocked due to agglomeration and agglomeration, which will bring inconvenience to users and affect the absorption of pyraclostrobin by plants. , reducing the efficacy of the drug. These technical difficulties have prevented the widespread use of pyraclostrobin aqueous dispersions.

CN102469775A公開一種製備吡唑醚菌酯的含水懸浮液的方法，該方法藉由大量的吡唑醚菌酯以無定型液滴形式分散在水相中，然後加入少量吡唑醚菌酯單一晶型顆粒的懸浮液，誘導吡唑醚菌酯無定型液滴快速結晶形成最終的顆粒水分散懸浮液。該方法需要熔融吡唑醚菌酯並且在加熱水相超過吡唑醚菌酯活性物熔點以上的溫度下進行。因此該方法實際生產加工能耗比較大，可操作性比較複雜，對設備要求也很高。因此如何提供一種熱貯和常貯穩定性好，不易聚集和結塊，且製備簡便的組合物是目前迫切 需要的。 CN102469775A discloses a method for preparing an aqueous suspension of pyraclostrobin. In the method, a large amount of pyraclostrobin is dispersed in an aqueous phase in the form of amorphous droplets, and then a small amount of pyraclostrobin is added to a single crystal form The suspension of particles induces rapid crystallization of pyraclostrobin amorphous droplets to form the final aqueous dispersion of particles. The process requires melting pyraclostrobin and is carried out at a temperature that heats the aqueous phase above the melting point of the pyraclostrobin active. Therefore, the actual production and processing energy consumption of this method is relatively large, the operability is relatively complicated, and the equipment requirements are also very high. Therefore, how to provide a composition with good thermal storage and normal storage stability, not easy to aggregate and agglomerate, and easy to prepare is an urgent need at present. needs.

發明人意外發現：採用吡唑醚菌酯、烷基磺酸鹽、多孔性載體以及功能性助劑的組合，可以得到具有改進熱貯穩定性，避免團聚結塊的吡唑醚菌酯的水分散固體組合物。 The inventor unexpectedly found that: using a combination of pyraclostrobin, alkyl sulfonates, porous carriers and functional additives, it is possible to obtain pyraclostrobin water with improved thermal storage stability and avoiding agglomeration and agglomeration. Disperse the solid composition.

基於上述發現，本發明提供以下技術方案： Based on the above findings, the present invention provides the following technical solutions:

第一方面，本發明提供一種吡唑醚菌酯水分散固體組合物，其按重量百分比包括以下組分：吡唑醚菌酯5~50%，烷基磺酸鹽0.1~15%，多孔性載體5~80%，功能性助劑1~45%。 In the first aspect, the present invention provides a water-dispersed solid composition of pyraclostrobin, which comprises the following components by weight: 5-50% of pyraclostrobin, 0.1-15% of alkyl sulfonate, porosity Carrier 5~80%, functional additives 1~45%.

本發明中，所述吡唑醚菌酯占組合物的重量百分比為5~50%，例如5%、8%、10%、12%、15%、20%、22%、25%、28%、30%、32%、35%、40%、42%、45%或50%。 In the present invention, the weight percentage of the pyraclostrobin in the composition is 5-50%, such as 5%, 8%, 10%, 12%, 15%, 20%, 22%, 25%, 28% , 30%, 32%, 35%, 40%, 42%, 45% or 50%.

本發明中，所述烷基磺酸鹽占組合物的重量百分比為0.1~15%，例如0.1%、0.5%、1%、2%、3%、3.5%、4%、5.2%、6%、7%、8.5%、9%、10%、11%、12%、13%、14%或15%。 In the present invention, the weight percentage of the alkyl sulfonate in the composition is 0.1-15%, for example, 0.1%, 0.5%, 1%, 2%, 3%, 3.5%, 4%, 5.2%, 6% , 7%, 8.5%, 9%, 10%, 11%, 12%, 13%, 14% or 15%.

本發明中，所述多孔性載體占組合物的重量百分比為5~80%，例如5%、8%、10%、12%、13%、15%、18%、20%、22%、25%、30%、35%、40%、48%、52%、60%、65%、72%、79%或80%。 In the present invention, the weight percentage of the porous carrier in the composition is 5-80%, for example, 5%, 8%, 10%, 12%, 13%, 15%, 18%, 20%, 22%, 25% %, 30%, 35%, 40%, 48%, 52%, 60%, 65%, 72%, 79%, or 80%.

本發明中，所述功能性助劑占組合物的重量百分比為1~45%，例如1%、2%、3%、5%、8%、10%、15%、20%、22%、25%、30%、35%、40%、42%、43%或45%。 In the present invention, the functional adjuvant accounts for 1 to 45% by weight of the composition, such as 1%, 2%, 3%, 5%, 8%, 10%, 15%, 20%, 22%, 25%, 30%, 35%, 40%, 42%, 43% or 45%.

本發明藉由對吡唑醚菌酯、烷基磺酸鹽、多孔性載體以及功能性助劑的含量進行選擇，其配製得到的吡唑醚菌酯水分散固體組合物具有熱貯和常貯穩定性好、不聚集、不結塊、無堵塞噴霧器過濾器或噴霧頭現象。 In the present invention, the content of pyraclostrobin, alkyl sulfonate, porous carrier and functional auxiliary is selected, and the prepared pyraclostrobin water-dispersed solid composition has the advantages of thermal storage and normal storage. Good stability, no agglomeration, no caking, no clogging of sprayer filter or spray head phenomenon.

該吡唑醚菌酯水分散固體組合物中，除了含有吡唑醚菌酯這一活性成分外，還可以含有其它活性成分，例如戊唑醇、呋蟲胺或氟唑環菌胺等，可以含有其中一種或多種，本發明不做特殊限定。 The pyraclostrobin water-dispersed solid composition, in addition to the active ingredient pyraclostrobin, may also contain other active ingredients, such as tebuconazole, dinotefuran or flufenoxam, etc. It contains one or more of them, which is not particularly limited in the present invention.

優選地，所述吡唑醚菌酯水分散固體組合物按重量百分比由如下組分組成： Preferably, the pyraclostrobin water-dispersed solid composition is composed of the following components by weight percentage:

吡唑醚菌酯6~30%，烷基磺酸鹽2~5%，多孔性載體10~70%，餘量為功能性助劑。 Pyraclostrobin 6~30%, alkyl sulfonate 2~5%, porous carrier 10~70%, and the balance is functional additives.

優選地，所述烷基磺酸鹽選自烷基萘磺酸鹽、烷基萘磺酸鹽甲醛縮聚物、烷基苯磺酸鹽、烷基乙基磺酸鹽或第二烷基磺酸鹽中的任意一種或至少兩種的混合物，其中典型但非限制性的混合物為：烷基萘磺酸鹽和烷基萘磺酸鹽甲醛縮聚物的混合物，烷基萘磺酸鹽和烷基苯磺酸鹽的混合物，烷基乙基磺酸鹽和烷基萘磺酸鹽甲醛縮聚物的混合物，第二烷基磺酸鹽和烷基苯磺酸鹽的混合物；優選為烷基萘磺酸鹽甲醛縮聚物。 Preferably, the alkyl sulfonate is selected from alkyl naphthalene sulfonate, alkyl naphthalene sulfonate formaldehyde polycondensate, alkyl benzene sulfonate, alkyl ethyl sulfonate or second alkyl sulfonic acid Any one or a mixture of at least two of the salts, wherein typical but non-limiting mixtures are: a mixture of alkylnaphthalenesulfonate and alkylnaphthalenesulfonate formaldehyde polycondensate, alkylnaphthalenesulfonate and alkylnaphthalenesulfonate Mixtures of benzene sulfonates, mixtures of alkyl ethyl sulfonates and alkyl naphthalene sulfonate formaldehyde polycondensates, mixtures of second alkyl sulfonates and alkyl benzene sulfonates; preferably alkyl naphthalene sulfonates Acid formaldehyde polycondensate.

優選地，所述多孔性載體選自高嶺土、蒙脫黏土、綠坡縷石、合成矽、植物纖維、礦物纖維或矽酸鎂鋁中的任意一種或至少兩種的混合物，其中典型但非限制性的混合物為：高嶺土和蒙脫黏土的混合物，蒙脫黏土和綠坡縷石的混合物，合成矽和高嶺土的混合物，植物纖維、礦物纖維和合成矽的混合物，矽酸鎂鋁和蒙脫黏土的混合物。 Preferably, the porous carrier is selected from any one or a mixture of at least two of kaolin, montmorillonite, attapulgite, synthetic silicon, plant fiber, mineral fiber or magnesium aluminum silicate, among which typical but not limited The natural mixtures are: a mixture of kaolin and montmorillonite, a mixture of montmorillonite and attapulgite, a mixture of synthetic silica and kaolin, a mixture of vegetable fibers, mineral fibers and synthetic silica, magnesium aluminum silicate and montmorillonite clay mixture.

優選地，所述高嶺土選自高嶺石、迪開石、珍珠陶土、富矽高嶺石、多水高嶺石或多水埃洛石中的任意一種或至少兩種的混合物，其中典型但非限制性的混合物為：高嶺石和迪開石的混合物，珍珠陶土和富矽高嶺石的混合物，多水埃洛石和珍珠陶土的混合物；所述蒙脫黏土選自貝得石、鋰蒙脫石、皂石或斑脫土中的任意一種或至少兩種的混合物，其中典型但非限制性的混合物為：貝得石和鋰蒙脫石的混合物，皂石和斑脫土的混合物，鋰蒙脫石和皂石的混合物；所述綠坡縷石選自漂白土和/或海泡石；所 述合成矽選自白炭黑和/或氣相白炭黑。 Preferably, the kaolin is selected from any one or a mixture of at least two of kaolinite, dicite, nacre, silicon-rich kaolinite, halloysite or halloysite, wherein typical but non-limiting The mixture is: a mixture of kaolinite and dicite, a mixture of pearl clay and silicon-rich kaolinite, a mixture of halloysite and pearl clay; the montmorillonite is selected from beidellite, hectorite, saponite Or any one of bentonite or a mixture of at least two, wherein typical but non-limiting mixtures are: a mixture of beidellite and hectorite, a mixture of saponite and bentonite, a mixture of hectorite and saponite mixture; said attapulgite is selected from fuller's earth and/or sepiolite; all The synthetic silicon is selected from silica and/or fumed silica.

優選地，所述功能性助劑選自分散劑、潤濕劑、消泡劑或惰性載體中的任意一種或至少兩種的混合物，即所述吡唑醚菌酯水分散固體組合物中，可以含有其中任意一種功能性助劑，也可以採用兩種或多種的混合形式。 Preferably, the functional adjuvant is selected from any one or a mixture of at least two of dispersing agents, wetting agents, defoaming agents or inert carriers, that is, in the water-dispersed solid composition of pyraclostrobin, it can be It contains any one of the functional adjuvants, or a mixture of two or more of them can be used.

優選地，所述分散劑選自木質素磺酸鹽、聚羧酸鹽、脂肪醇聚氧乙烯醚或環氧乙烷環氧丙烷嵌段共聚物中的任意一種或至少兩種的混合物，其中典型但非限制性的混合物為：木質素磺酸鹽和聚羧酸鹽的混合物，聚羧酸鹽和脂肪醇聚氧乙烯醚的混合物，環氧乙烷環氧丙烷嵌段共聚物和木質素磺酸鹽的混合物。 Preferably, the dispersant is selected from any one or a mixture of at least two of lignosulfonates, polycarboxylates, fatty alcohol polyoxyethylene ethers or ethylene oxide propylene oxide block copolymers, wherein Typical but non-limiting mixtures are: mixtures of lignosulfonates and polycarboxylates, mixtures of polycarboxylates and fatty alcohol polyoxyethylene ethers, ethylene oxide propylene oxide block copolymers and lignin A mixture of sulfonates.

優選地，所述潤濕劑選自壬基酚聚氧乙烯醚、K12或聚氧乙烯脂肪醇醚中的任意一種或至少兩種的混合物，其中典型但非限制性的混合物為壬基酚聚氧乙烯醚和K12的混合物，K12和聚氧乙烯脂肪醇醚的混合物。 Preferably, the wetting agent is selected from any one or a mixture of at least two of nonylphenol polyoxyethylene ether, K12 or polyoxyethylene fatty alcohol ether, wherein a typical but non-limiting mixture is nonylphenol polyoxyethylene A mixture of oxyethylene ether and K12, a mixture of K12 and polyoxyethylene fatty alcohol ether.

優選地，所述消泡劑選自矽氧烷類消泡劑，至於具體的矽氧烷類消泡劑種類，本領域技術人員可以根據實際需要進行常規選擇，本發明不做特殊限定。 Preferably, the defoaming agent is selected from siloxane-based defoaming agents. As for the specific types of siloxane-based defoaming agents, those skilled in the art can make routine selections according to actual needs, which are not particularly limited in the present invention.

優選地，所述惰性載體選自玉米澱粉、滑石粉、蔗糖、硫酸鉀、高嶺土或矽藻土中的任意一種或至少兩種的混合物，其中典型但非限制性的混合物為：玉米澱粉和滑石粉的混合物，蔗糖和硫酸鉀的混合物，高嶺土和玉米澱粉的混合物。 Preferably, the inert carrier is selected from any one or a mixture of at least two of corn starch, talc, sucrose, potassium sulfate, kaolin or diatomaceous earth, wherein a typical but non-limiting mixture is: corn starch and talc A mixture of flour, a mixture of sucrose and potassium sulfate, a mixture of kaolin and cornstarch.

本發明所述的吡唑醚菌酯水分散固體組合物，其製劑為可濕性粉劑或水分散顆粒劑。 The pyraclostrobin water-dispersed solid composition of the present invention is formulated as wettable powder or water-dispersed granule.

進一步，本發明提供了所述吡唑醚菌酯水分散固體組合物的製備方法，，包括以下步驟：(1)按配比將吡唑醚菌酯與烷基磺酸鹽混合； (2)將得到的混合物在35℃以下進行粗粉碎，得到均質混合物；(3)在得到的均質混合物中，加入多孔性載體和功能性助劑，進行細粉碎，得到所述吡唑醚菌酯水分散固體組合物。 Further, the present invention provides a method for preparing the water-dispersed solid composition of pyraclostrobin, comprising the following steps: (1) mixing pyraclostrobin and alkyl sulfonate according to the ratio; (2) coarsely pulverizing the obtained mixture below 35° C. to obtain a homogeneous mixture; (3) adding a porous carrier and a functional auxiliary to the obtained homogeneous mixture, and performing fine pulverization to obtain the pyraclostrobin Ester water dispersed solid composition.

不同於以往公開的製備方法，本發明在步驟(1)中首先只將吡唑醚菌酯與烷基磺酸鹽進行混合，而不採用將所有組分或者連同分散劑和消泡劑以及載體進行一塊混合的形式。 Different from the preparation method disclosed in the past, the present invention firstly only mixes pyraclostrobin and alkyl sulfonate in step (1), instead of using all components or together with dispersant and defoamer and carrier Carry out a piece of mixed form.

本發明藉由在步驟(1)中先將吡唑醚菌酯與烷基磺酸鹽混合，經第一次粗粉碎使得吡唑醚菌酯與烷基磺酸鹽混合更充分，烷基磺酸鹽更有效地在吡唑醚菌酯顆粒表面附著吸附，有效阻止了在存儲過程中顆粒與顆粒之間的接觸聚集。 In the present invention, the pyraclostrobin and the alkyl sulfonate are mixed firstly in step (1), and the first coarse pulverization makes the pyraclostrobin and the alkyl sulfonate more fully mixed, and the alkyl sulfonate The acid salt is more effectively attached and adsorbed on the surface of pyraclostrobin particles, which effectively prevents the contact aggregation between particles during storage.

發明人還意外發現，當只將吡唑醚菌酯與烷基磺酸鹽進行先混合時，藉由採用在35℃以下進行粗粉碎，其能夠使吡唑醚菌酯呈現為膏狀物，具有軟化現象，從而更進一步有助於後面水分散固體顆粒物成品避免團聚結塊問題。 The inventors also unexpectedly found that when only pyraclostrobin and alkyl sulfonate are mixed first, the pyraclostrobin can be made into a paste by coarsely pulverizing at below 35°C, It has a softening phenomenon, which further helps to avoid the problem of agglomeration and agglomeration of the finished water-dispersed solid particles.

對於將吡唑醚菌酯與烷基磺酸鹽混合後得到的混合物，本發明採用在低溫下進行粉碎，其具體採用的是在35℃以下的低溫下進行，例如溫度為0℃、4℃、8℃、10℃、12℃、15℃、20℃、22℃、25℃、28℃、30℃或35℃，當然也可以在0度以下進行。 For the mixture obtained by mixing pyraclostrobin and alkyl sulfonate, the present invention adopts pulverization at low temperature, which is specifically adopted at low temperature below 35°C, for example, the temperature is 0°C, 4°C , 8°C, 10°C, 12°C, 15°C, 20°C, 22°C, 25°C, 28°C, 30°C or 35°C, of course, it can also be performed below 0°C.

吡唑醚菌酯原藥熔點為56~64℃，如果採用常規條件下直接粉碎，原藥會發生軟化現象，影響粉碎效率。而採用在本發明的低溫下粉碎可有效解決吡唑醚菌酯原藥在粉碎過程中顆粒碰撞而軟化現象，同時使得烷基磺酸鹽充分均勻並緊密附著在吡唑醚菌酯顆粒表面，解決後續二次氣流粉碎對吡唑醚菌酯顆粒的影響。 The melting point of pyraclostrobin is 56~64℃. If it is directly pulverized under normal conditions, the original drug will soften and affect the pulverization efficiency. The pulverization at the low temperature of the present invention can effectively solve the phenomenon of particle collision and softening of the pyraclostrobin original drug during the pulverization process, and at the same time, the alkyl sulfonate is sufficiently uniform and tightly attached to the surface of the pyraclostrobin particles, Solve the effect of subsequent secondary airflow pulverization on pyraclostrobin particles.

本發明採用在粗粉碎後得到的均質混合物中，再加入多孔性載體和功能性助劑，這樣的操作能夠使粉碎的溫度相對寬鬆，其可以採用相對較高 的溫度下進行，此時功能性助劑能起到一定的保護作用，進一步起到對最終形成的吡唑醚菌酯水分散固體組合物避免團聚和結塊產生促進作用。 The present invention adopts the homogeneous mixture obtained after coarse pulverization, and then adds porous carriers and functional additives. Such an operation can make the pulverization temperature relatively loose, and it can adopt a relatively high temperature. At this time, the functional additives can play a certain protective role, and further play a role in promoting the formation of the final pyraclostrobin water-dispersed solid composition to avoid agglomeration and agglomeration.

本發明的製備方法中，採用了低溫下粗粉碎結合細粉碎的操作方式，藉由將粉碎分成粗粉碎和細粉碎兩步操作，烷基磺酸鹽與吡唑醚菌酯的混合更充分，更有效地在吡唑醚菌酯顆粒表面附著吸附，進一步有效阻止了在儲存過程中顆粒與顆粒之間的接觸團聚現象。 In the preparation method of the present invention, the operation mode of coarse pulverization combined with fine pulverization at low temperature is adopted. The adhesion and adsorption on the surface of the pyraclostrobin particles is more effective, and the contact agglomeration phenomenon between the particles during the storage process is further effectively prevented.

本發明在製備不同形式的水分散固體組合物時，例如製備可濕性粉劑時，上述製備方法中在步驟(3)進行細粉碎後，直接可以得到該可濕性粉劑；而當製備水分散顆粒劑時，在步驟(3)進行細粉碎後，還需經造粒烘乾步驟，才可得到該水分散顆粒劑。對於造粒烘乾技術，本領域技術人員應當明瞭，其可以採用例如擠壓造粒、噴霧造粒、旋轉造粒、流化床造粒等多種操作方式，本發明對其不做特殊限定。 When the present invention prepares different forms of water-dispersed solid compositions, such as wettable powder, the wettable powder can be directly obtained after finely pulverizing step (3) in the above preparation method; In the case of granules, after the fine pulverization in step (3), the water-dispersed granules can be obtained only after the step of granulation and drying. For the granulation drying technology, those skilled in the art should understand that it can adopt various operation modes such as extrusion granulation, spray granulation, rotary granulation, fluidized bed granulation, etc., which is not particularly limited in the present invention.

本發明中，步驟(2)所述粗粉碎採用氣流粉碎，其具體操作為：將混合料以一定的速度藉由高速氣流，使得顆粒與顆粒、顆粒與內壁之間產生強烈碰撞而達到破損的效果，其最終使得粉碎後粒徑D90

Figure 107115522-A0305-02-0009-8
20μm。 In the present invention, the coarse pulverization in step (2) adopts airflow pulverization, and the specific operation is as follows: the mixture is subjected to high-speed airflow at a certain speed, so that the particles and particles, particles and the inner wall are strongly collided to achieve damage. effect, which finally makes the particle size D90 after pulverization
Figure 107115522-A0305-02-0009-8
20μm.

至於上述氣流粉碎所採用的具體氣流速度，本領域技術人員可以根據實際要粉碎後的粒徑大小進行調整，本發明不做特殊限定。 As for the specific airflow velocity used in the above-mentioned airflow pulverization, those skilled in the art can adjust the particle size according to the actual particle size to be pulverized, which is not particularly limited in the present invention.

本發明採用氣流粉碎能夠實現吡唑醚菌酯與烷基磺酸鹽的均勻混合，提高混合的均勻度和散熱效果。 The invention can realize the uniform mixing of pyraclostrobin and the alkyl sulfonate by adopting the jet pulverization, and improve the uniformity of mixing and the heat dissipation effect.

本發明中，步驟(3)所述細粉碎採用二次氣流粉碎，其可以調整粉碎壓力和進料速度，以使粉碎後粒徑達到1~15μm。 In the present invention, the fine pulverization in step (3) adopts secondary airflow pulverization, which can adjust the pulverization pressure and the feeding speed, so that the particle size after pulverization reaches 1-15 μm.

至於二次氣流粉碎所採用的具體氣流速度、粉碎壓力以及進料速度，本領域技術人員也是可以根據實際要達到的粉碎後粒徑大小進行調整的。 As for the specific airflow velocity, pulverization pressure and feed velocity used in the secondary jet pulverization, those skilled in the art can also adjust it according to the actual particle size after pulverization.

本發明的吡唑醚菌酯水分散固體組合物可以是可濕性粉劑或者水分散顆粒劑。該吡唑醚菌酯水分散固體組合物具有熱貯和常貯穩定性好、不聚 集、不結塊、不堵塞過濾器或噴霧頭等優點，從而方便了貯存和用戶使用，並提高了吡唑醚菌酯的藥效。 The pyraclostrobin water-dispersed solid composition of the present invention may be a wettable powder or a water-dispersible granule. The pyraclostrobin water-dispersed solid composition has good thermal storage and normal storage stability, no polymerization The advantages of collection, no caking, no clogging of filters or spray heads, etc., are convenient for storage and use by users, and improve the efficacy of pyraclostrobin.

與現有技術相比，本發明至少具有以下有益效果： Compared with the prior art, the present invention at least has the following beneficial effects:

(1)本發明的吡唑醚菌酯水分散固體組合物，具有熱貯和常貯穩定性好、不聚集、不結塊、不堵塞過濾器或噴霧頭等優點，流動性好；(2)本發明製備吡唑醚菌酯水分散固體組合物的方法操作簡便，經濟成本低，可實現性強。 (1) The pyraclostrobin water-dispersed solid composition of the present invention has the advantages of good thermal storage and normal storage stability, no aggregation, no caking, no clogging of filters or spray heads, etc., and good fluidity; (2) ) The method for preparing the pyraclostrobin water-dispersed solid composition of the present invention is easy to operate, low in economic cost and strong in realizability.

為便於理解本發明，本發明列舉實施例如下。本領域技術人員應該明瞭，所述實施例僅僅是幫助理解本發明，不應視為對本發明的具體限制。以下「%」均指重量百分比。 In order to facilitate the understanding of the present invention, examples of the present invention are as follows. It should be understood by those skilled in the art that the embodiments are only for helping the understanding of the present invention, and should not be regarded as a specific limitation of the present invention. The following "%" all refer to weight percentage.

實施例1：20%吡唑醚菌酯 可濕性粉劑 Example 1: 20% pyraclostrobin WP

Figure 107115522-A0305-02-0010-1
Figure 107115522-A0305-02-0010-1

配製過程：將吡唑醚菌酯原藥與Morwet D425(烷基萘磺酸鹽甲醛縮聚物)按重量比例混合，攪拌均勻後，在溫度為30℃下進行第一次粗粉碎，得到均質混合物；然後將氣相白炭黑、Soap L(牛脂酸鈉)和玉米澱粉按重量比例加入到上述粗粉碎混料中，進行第二次細粉碎，直到粒徑D90<10μm， 即得最終產品。 Preparation process: mix the original drug of pyraclostrobin with Morwet D425 (alkylnaphthalene sulfonate formaldehyde polycondensate) in a proportion by weight, after stirring evenly, carry out the first rough pulverization at a temperature of 30 ° C to obtain a homogeneous mixture ; Then add fumed silica, Soap L (sodium tallow) and corn starch in the above-mentioned coarsely pulverized mixture by weight, carry out the second fine pulverization, until particle size D90<10 μm, That is the final product.

實施例2：50%吡唑醚菌酯 水分散粒劑 Example 2: 50% pyraclostrobin water dispersible granules

Figure 107115522-A0305-02-0011-2
Figure 107115522-A0305-02-0011-2

配製過程：將吡唑醚菌酯原藥與Morwet EFW(烷基萘磺酸鹽)按重量比例混合，攪拌均勻後，在溫度為25℃下進行第一次粗粉碎，得到均質混合物；然後將白炭黑、EO/PO嵌段共聚物、Soap L(牛脂酸鈉)和矽藻土按重量比例加入到上述粗粉碎混料中，進行第二次細粉碎，得到粒徑D90<10μm的母粉，該母粉加入適量的水捏合後，經過擠壓造粒烘乾得到最終產品。 Preparation process: mix the original drug of pyraclostrobin and Morwet EFW (alkylnaphthalene sulfonate) according to the weight ratio, after stirring evenly, carry out the first coarse pulverization at a temperature of 25 ° C to obtain a homogeneous mixture; Silica, EO/PO block copolymer, Soap L (sodium tallowate) and diatomaceous earth are added to the above-mentioned coarsely pulverized mixture in proportion by weight, and then finely pulverized for the second time to obtain a mother with particle size D90<10 μm The master powder is kneaded by adding an appropriate amount of water, and then extruded, granulated and dried to obtain the final product.

實施例3：10%吡唑醚菌酯 可濕性粉劑 Example 3: 10% pyraclostrobin WP

Figure 107115522-A0305-02-0011-3
Figure 107115522-A0305-02-0011-3

配製過程：將吡唑醚菌酯原藥與十二烷基磺酸鈉按重量比例混合，攪拌均勻後，在溫度為22℃下進行第一次粗粉碎，得到均質混合物；然後將煅燒高嶺土、壬基酚聚氧乙烯醚磷酸酯、Soap L(牛脂酸鈉)和硫酸鉀按重量 比例加入到上述粗粉碎混料中，進行第二次細粉碎，直到粒徑D90<10μm，即得最終產品。 Preparation process: mix the original drug of pyraclostrobin and sodium dodecyl sulfonate in a proportion by weight, and after stirring evenly, carry out the first coarse pulverization at a temperature of 22 ° C to obtain a homogeneous mixture; then calcined kaolin, Nonylphenol Ethoxylate Phosphate, Soap L (Sodium Tallow) and Potassium Sulfate by Weight The proportion is added to the above-mentioned coarsely pulverized mixture, and the second fine pulverization is carried out until the particle size D90<10 μm, that is, the final product is obtained.

實施例4：5%吡唑醚菌酯+10%啶醯菌胺 可濕性粉劑 Embodiment 4: 5% pyraclostrobin + 10% pyraclostrobin WP

Figure 107115522-A0305-02-0012-4
Figure 107115522-A0305-02-0012-4

配製過程：將吡唑醚菌酯原藥與烷基乙基磺酸鹽按重量比例混合，攪拌均勻後，在溫度35℃下進行第一次粗粉碎，得到均質混合物；然後將啶醯菌胺、植物纖維、脂肪醇聚氧乙烯醚、Soap L(牛脂酸鈉)和滑石粉按重量比例加入到上述粗粉碎混料中，進行第二次細粉碎，直到粒徑D90<10μm，即得最終產品。 Preparation process: mix the original drug of pyraclostrobin and alkyl ethyl sulfonate according to the weight ratio, after stirring evenly, carry out the first coarse pulverization at the temperature of 35 ℃ to obtain a homogeneous mixture; then the pyraclostrobin is mixed , vegetable fiber, fatty alcohol polyoxyethylene ether, Soap L (sodium tallowate) and talc are added to the above-mentioned coarsely pulverized mixture in proportion by weight, and the second fine pulverization is carried out until the particle size D90<10 μm, that is, the final product.

實施例5：5%吡唑醚菌酯+40%百菌清 水分散顆粒劑 Example 5: 5% pyraclostrobin+40% chlorothalonil water dispersible granules

Figure 107115522-A0305-02-0012-5
高嶺土 23%
Figure 107115522-A0305-02-0012-5
 Kaolin 23%

配製過程：將吡唑醚菌酯原藥與烷基萘磺酸鹽甲醛縮聚物按重量比例混合，攪拌均勻後，在溫度為10℃下進行第一次粗粉碎，得到均質混合物；然後將百菌清、礦物纖維、聚羧酸鹽、琥珀酸磺酸鈉、Soap L(牛脂酸鈉)和高嶺土按重量比例加入到上述粗粉碎混料中，進行第二次細粉碎，得到粒徑D90<10μm的母粉，該母粉加入適量的水捏合後，經過擠壓造粒烘乾得到最終產品。 Preparation process: mix the original drug of pyraclostrobin and the alkylnaphthalene sulfonate formaldehyde polycondensate according to the weight ratio, stir evenly, and carry out the first coarse pulverization at a temperature of 10 ℃ to obtain a homogeneous mixture; Bacterial clear, mineral fiber, polycarboxylate, sodium succinate sulfonate, Soap L (sodium tallowate) and kaolin are added in the above-mentioned coarsely pulverized mixture by weight, carry out the second fine pulverization, obtain particle diameter D90＜ 10μm master powder, the master powder is kneaded by adding an appropriate amount of water, and then extruded, granulated and dried to obtain the final product.

對比例1 Comparative Example 1

與實施例1相比，除配製過程不同外，其它與實施例1相同。 Compared with Example 1, except the preparation process is different, other parts are the same as Example 1.

配製過程：將吡唑醚菌酯原藥與Morwet D425、氣相白炭黑、Soap L和玉米澱粉按重量比例在溫度為30℃下進行混合，只經粗粉碎，使得D90達到20μm，即得最終產品。 Preparation process: Mix the original drug of pyraclostrobin with Morwet D425, fumed silica, Soap L and corn starch by weight at a temperature of 30 ° C, and only coarsely pulverize to make D90 reach 20 μm, that is, Final product.

對比例2 Comparative Example 2

與實施例1相比，除配製過程不同外，其它與實施例1相同。 Compared with Example 1, except the preparation process is different, other parts are the same as Example 1.

配製過程：將吡唑醚菌酯原藥與Morwet D425、氣相白炭黑、Soap L和玉米澱粉按重量比例在溫度為30℃下進行混合，只經細粉碎，使得D90<10μm，即得最終產品。 Preparation process: Mix the original drug of pyraclostrobin with Morwet D425, fumed silica, Soap L and corn starch by weight at a temperature of 30 ° C, and only finely pulverize so that D90 < 10 μm, that is, Final product.

對比例3 Comparative Example 3

與實施例1相比，除配製過程不同外，其它與實施例1相同。 Compared with Example 1, except the preparation process is different, other parts are the same as Example 1.

配製過程：將吡唑醚菌酯原藥與Morwet D425、氣相白炭黑、Soap L和玉米澱粉按重量比例進行混合，先在溫度為30℃下經粗粉碎，使得D90達到20μm，再經細粉碎，直到粒徑D90<10μm，即得最終產品。 Preparation process: Mix the original drug of pyraclostrobin with Morwet D425, fumed silica, Soap L and corn starch according to the weight ratio, firstly coarsely pulverize at a temperature of 30 °C to make D90 reach 20 μm, and then pass Finely pulverize until the particle size D90<10μm to obtain the final product.

對比例4 Comparative Example 4

與實施例1相比，除配製過程不同外，其它與實施例1相同。 Compared with Example 1, except the preparation process is different, other parts are the same as Example 1.

配製過程：將吡唑醚菌酯原藥與Morwet D425、氣相白炭黑、Soap L和玉米澱粉按重量比例進行混合，先在溫度為40℃下經粗粉碎，使得D90達到20μm，再經細粉碎，直到粒徑D90<10μm，即得最終產品。 Preparation process: Mix the original drug of pyraclostrobin with Morwet D425, fumed silica, Soap L and corn starch in proportion by weight, firstly grind at 40℃ to make D90 reach 20μm, Finely pulverize until the particle size D90<10μm to obtain the final product.

對比例5 Comparative Example 5

與實施例2相比，除配製過程不同外，其它與實施例2相同。 Compared with Example 2, except the preparation process is different, other parts are the same as Example 2.

配製過程：吡唑醚菌酯原藥與Morwet EFW、白炭黑、EO/PO嵌段共聚物、Soap L和矽藻土按重量比例進行混合，經氣流粉碎，得到粒徑D90<10μm的母粉，該母粉加入適量的水捏合後，經過擠壓造粒烘乾得到最終產品。 Preparation process: The original drug of pyraclostrobin is mixed with Morwet EFW, white carbon black, EO/PO block copolymer, Soap L and diatomaceous earth according to the weight ratio, and it is pulverized by air flow to obtain the mother with particle size D90<10μm The master powder is kneaded by adding an appropriate amount of water, and then extruded, granulated and dried to obtain the final product.

對比例6 Comparative Example 6

與實施例2相比，採用CN102726379A公開的製備方法進行。 Compared with Example 2, the preparation method disclosed in CN102726379A was adopted.

配製過程：吡唑醚菌酯原藥與Morwet D425、氣相白炭黑、Soap L和玉米澱粉按重量比例混合均勻得到混合物，經氣流粉碎機將以上混合物進行超微粉碎後得到母粉；將超微粉碎後得到的母粉稱取一定的量放入旋化流化床；開啟旋化流化床並慢慢往其加入粘結劑的水溶液進行造粒；等造粒完成後進行烘乾；將烘乾的粒狀物進行篩分、分析檢驗後即得到吡唑醚菌酯水分散粒劑。 Preparation process: the original drug of pyraclostrobin and Morwet D425, fumed silica, Soap L and corn starch are uniformly mixed by weight to obtain a mixture, and the above mixture is ultrafinely pulverized by a jet mill to obtain a mother powder; The master powder obtained after ultrafine pulverization is weighed into a certain amount and put into the swirling fluidized bed; the swirling fluidized bed is opened and the aqueous solution of the binder is slowly added to it for granulation; after the granulation is completed, drying is carried out ; The pyraclostrobin water dispersible granules are obtained after sieving and analyzing the dried granules.

上述實施例1~5和對比例1~6製備的樣品測試熱貯穩定性。熱貯穩定性試驗是在54℃烘箱中進行。 The samples prepared in the above Examples 1 to 5 and Comparative Examples 1 to 6 were tested for thermal storage stability. The heat storage stability test was carried out in a 54°C oven.

在54℃的烘箱中熱貯後，將樣品從烘箱中取出。冷卻至室溫，將各測試樣品倒出，觀察樣品流動性。然後將可濕性粉劑樣品直接過325目篩子；水分散顆粒劑樣品用水稀釋後，過325目篩子。測試的結果如表1所示。 After heat storage in an oven at 54°C, the samples were removed from the oven. After cooling to room temperature, each test sample was poured out and the flowability of the sample was observed. Then, the wettable powder sample was directly passed through a 325-mesh sieve; the water-dispersible granule sample was diluted with water, and then passed through a 325-mesh sieve. The test results are shown in Table 1.

Figure 107115522-A0305-02-0015-6
Figure 107115522-A0305-02-0015-6
Figure 107115522-A0305-02-0016-7
Figure 107115522-A0305-02-0016-7

表1中的測試結果表明，根據本發明製備的吡唑醚菌酯水分散固體組合物熱貯流動性好，無結塊，無堵塞篩網，因此具有更方便用戶使用和提高吡唑醚菌酯藥效的突出優勢。 The test results in Table 1 show that the pyraclostrobin water-dispersed solid composition prepared according to the present invention has good heat storage fluidity, no caking, and no clogging of the screen, so it is more convenient for users to use and improves the efficiency of pyraclostrobin. The outstanding advantages of ester efficacy.

申請人聲明，本發明藉由上述實施例來說明本發明的詳細工藝設備和工藝流程，但本發明並不局限於上述詳細的技術方案，即不意味著本發明必須依賴上述詳細的技術方案才能實施。所屬技術領域的技術人員應該明瞭，對本發明的任何改進，對本發明產品各原料的等效替換及輔助成分的添加、具體方式的選擇等，均落在本發明的保護範圍和公開範圍之內。 The applicant declares that the present invention illustrates the detailed process equipment and process flow of the present invention by the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed technical solutions, that is, it does not mean that the present invention must rely on the above-mentioned detailed technical solutions. implement. Those skilled in the art should understand that any improvement of the present invention, the equivalent replacement of each raw material of the product of the present invention, the addition of auxiliary components, the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims (4)

一種吡唑醚菌酯水分散固體組合物的製備方法，其特徵在於，包括以下步驟：(1)按配製比例將吡唑醚菌酯與磺酸鹽混合；(2)將得到的混合物在35℃以下進行粗粉碎，得到均質混合物；(3)在得到的均質混合物中，加入多孔性載體和功能性助劑，進行細粉碎，得到所述吡唑醚菌酯水分散固體組合物，其中所述吡唑醚菌酯水分散固體組合物按重量百分比包括以下組分：吡唑醚菌酯5~50%，磺酸鹽0.1~15%，多孔性載體5~80%，功能性助劑1~45%；其中所述磺酸鹽選自烷基萘磺酸鹽、烷基萘磺酸鹽甲醛縮聚物、烷基苯磺酸鹽、烷基乙基磺酸鹽或二級烷基磺酸鹽中的任意一種或至少兩種的混合物。 A preparation method of pyraclostrobin water-dispersed solid composition, characterized in that, comprising the following steps: (1) mixing pyraclostrobin and sulfonate according to the preparation ratio; (2) mixing the obtained mixture at 35 Perform coarse pulverization below ℃ to obtain a homogeneous mixture; (3) adding a porous carrier and a functional auxiliary to the obtained homogeneous mixture, and performing fine pulverization to obtain the pyraclostrobin water-dispersed solid composition, wherein the The pyraclostrobin water-dispersed solid composition comprises the following components in percentage by weight: pyraclostrobin 5-50%, sulfonate 0.1-15%, porous carrier 5-80%, functional additive 1 ~45%; wherein the sulfonate is selected from alkylnaphthalenesulfonate, alkylnaphthalenesulfonate formaldehyde polycondensate, alkylbenzenesulfonate, alkylethylsulfonate or secondary alkylsulfonic acid Any one or a mixture of at least two of the salts. 如請求項1所述的方法，其特徵在於，步驟(3)所述細粉碎後，經造粒烘乾，得到吡唑醚菌酯水分散顆粒劑。 The method according to claim 1, characterized in that, after the fine pulverization in step (3), granulation and drying are performed to obtain pyraclostrobin water-dispersible granules. 如請求項1或2所述的方法，其特徵在於，步驟(2)所述粗粉碎採用氣流粉碎，並使粉碎後粒徑D90
Figure 107115522-A0305-02-0017-9
20μm。 The method according to claim 1 or 2, characterized in that, the coarse pulverization in step (2) adopts jet pulverization, and the particle size after pulverization is D90
Figure 107115522-A0305-02-0017-9
20μm. 一種如請求項1-3中任一項之一所述的方法製備得到的吡唑醚菌酯水分散固體組合物。 A pyraclostrobin water-dispersed solid composition prepared by the method according to any one of claims 1-3.
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