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TWI843864B - Solid preparation for controlling rice pests containing flupyridine - Google Patents

Solid preparation for controlling rice pests containing flupyridine Download PDF

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TWI843864B
TWI843864B TW109120819A TW109120819A TWI843864B TW I843864 B TWI843864 B TW I843864B TW 109120819 A TW109120819 A TW 109120819A TW 109120819 A TW109120819 A TW 109120819A TW I843864 B TWI843864 B TW I843864B
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aforementioned
rice
solid preparation
pests
controlling rice
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TW109120819A
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TW202114521A (en
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堀越亮
武內晴香
小野保道
佐藤篤志
薮崎光之
尾山和彦
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日商三井化學植保股份有限公司
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/08Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/12Powders or granules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/26Biocides, 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 in coated particulate form
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P17/00Pest repellants
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P7/00Arthropodicides
    • A01P7/04Insecticides

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Environmental Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Agronomy & Crop Science (AREA)
  • Dentistry (AREA)
  • Toxicology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical & Material Sciences (AREA)
  • Insects & Arthropods (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

本發明為一種水稻害蟲防除用固形製劑,其係含有選自由下述式(1)表示之氟吡嘧(flupyrimin)及其鹽所成之群組中之至少1種的有效成分、固體載體、界面活性劑、以及結合劑, 且為被覆型粒劑或擠出型粒劑。The present invention is a solid preparation for controlling rice pests, which contains at least one active ingredient selected from the group consisting of flupyrimin and its salts represented by the following formula (1), a solid carrier, a surfactant, and a binder. And it is a coated granule or an extruded granule.

Description

含有氟吡嘧(flupyrimin)之水稻害蟲防除用固形製劑Solid preparation for controlling rice pests containing flupyridine

本發明係關於含有氟吡嘧之水稻害蟲防除用固形製劑,更詳細而言,係關於被覆型粒劑或擠出型粒劑之水稻害蟲防除用固形製劑,及使用其之水稻害蟲防除方法、以及前述水稻害蟲防除用固形製劑之製造方法。The present invention relates to a solid preparation for controlling rice pests containing fluopyrazine, and more specifically, to a solid preparation for controlling rice pests in the form of coated granules or extruded granules, a method for controlling rice pests using the same, and a method for producing the solid preparation for controlling rice pests.

亞洲地域的主食之稻米,90%以上為在亞洲所生產,尤其是中國、印度、印尼3國的生產量佔有全世界之60%(非專利文獻1)。在此等之地域的稻米栽培(水稻栽培),因攝食損害地上部之蝶蛾目害蟲,及吸汁莖葉部之半翅目害蟲的損害導致之收量降低已成為問題,尤其是蝶蛾目害蟲之二化螟類、半翅目害蟲之飛蝨類帶來莫大的損害。因病害蟲導致之稻米的生產量損害約高達45%(非專利文獻2),為了提昇稻米的生產量,此等水稻害蟲的防除變必須。More than 90% of rice, the staple food in Asia, is produced in Asia, especially in China, India, and Indonesia, which account for 60% of the world's production (Non-patent Document 1). In such regions, rice cultivation (rice cultivation) has become a problem due to the damage caused by butterfly moth pests that damage the aboveground parts and hemiptera pests that suck the sap stems and leaves, resulting in reduced yields. In particular, the butterfly moth pests, the Chilo suppressalis, and the hemiptera pests, the flies, bring great damage. The loss of rice production due to diseases and pests is as high as 45% (Non-patent Document 2). In order to increase rice production, the prevention and control of these rice pests has become necessary.

現在,對於不同時期所發生之此等之水稻害蟲,藉由對各害蟲分別或是混合使用有效之藥劑,來進行防除(體系防除),進行複數次之處理時,耗費有關藥劑處理之人事費或勞力。又,對於既存藥劑之感受性降低之害蟲的發生成為問題(非專利文獻3、4)外,有機磷、苯基胺基甲酸酯(Carbamate)、合成除蟲菊酯等之既存藥劑,由於對非目標生物的不利影響而限制使用。據此,期望防除活性之通用性廣泛且其持續期間長,與既存藥劑未顯示交差耐藥性,進而對環境的影響亦低之新穎製劑的創出。At present, for these rice pests that occur at different times, effective pesticides are used for each pest separately or in combination to control them (systemic control). When multiple treatments are performed, the personnel costs and labor related to the pesticide treatment are consumed. In addition, the occurrence of pests with reduced sensitivity to existing pesticides has become a problem (non-patent documents 3 and 4). Existing pesticides such as organophosphates, carbamates, and synthetic pyrethroids are restricted in use due to their adverse effects on non-target organisms. Therefore, it is desired to create a novel formulation that has a wide range of control activity and a long duration, does not show cross-resistance with existing pesticides, and has low impact on the environment.

已報告氟吡嘧作為有害生物防除劑,對於水稻(Rice等)所發生之飛蝨類等之半翅目害蟲或二化螟類等之蝶蛾目害蟲,具有殺蟲效力,或與既存藥劑未顯示交差耐藥性,且對環境的影響低(專利文獻1),又,亦報告有於飛蝨類、二化螟類等之防除用,可混合其他殺蟲劑或殺菌劑來使用(專利文獻2)。然而,針對在稻米之生產的實用場面之具體的製劑形態或使用方法,尤其是防除活性的持續期間,研究仍然不足。 [先前技術文獻] [專利文獻]Flupyralid has been reported as a pest control agent, which has insecticidal effects on Hemiptera pests such as flies or Butterfly pests such as striped stem borers that occur on rice (Rice, etc.), or does not show cross-resistance with existing drugs, and has low impact on the environment (Patent Document 1). It has also been reported that it can be mixed with other insecticides or fungicides for the control of flies and striped stem borers (Patent Document 2). However, there is still a lack of research on the specific formulation form or method of use in practical scenarios of rice production, especially the duration of the control activity. [Prior Art Document] [Patent Document]

[專利文獻1]國際公開第2012/029672號 [專利文獻2]國際公開第2013/129688號 [非專利文獻][Patent Document 1] International Publication No. 2012/029672 [Patent Document 2] International Publication No. 2013/129688 [Non-Patent Document]

[非專利文獻1]AMIS Market Database,2018年9月20日檢索,網際網路,<URL:http://statistics.amis-outlook.org/data/ index.html> [非專利文獻2]India Crop Protection Chemicals (Pesticides) Market-Growth,Trends and Forecast(2017-2022), Mordor Intelligence報告(2017年12月) [非專利文獻3]Pest Management Science,Vol.73(6), 1169-1178(2017) [非專利文獻4]Scientific Reports,(2018)8:4586|DOI:10.1038/s41598-018-22906-5[Non-patent document 1] AMIS Market Database, retrieved on September 20, 2018, Internet, <URL: http://statistics.amis-outlook.org/data/index.html> [Non-patent document 2] India Crop Protection Chemicals (Pesticides) Market-Growth, Trends and Forecast (2017-2022), Mordor Intelligence Report (December 2017) [Non-patent document 3] Pest Management Science, Vol. 73(6), 1169-1178(2017) [Non-patent document 4] Scientific Reports, (2018) 8: 4586|DOI: 10.1038/s41598-018-22906-5

[發明欲解決之課題][Problems to be solved by the invention]

本發明係鑑於這般的狀況而完成者,以提供一種用以防除有害生物,尤其是水稻害蟲之防除活性的持續期間非常長之嶄新的固形製劑,及使用其之水稻害蟲防除方法、以及前述水稻害蟲防除用固形製劑之製造方法作為目的。 [用以解決課題之手段]The present invention was completed in view of such a situation, and aims to provide a novel solid preparation for controlling harmful organisms, especially rice pests, with a very long duration of control activity, a rice pest control method using the same, and a method for producing the solid preparation for controlling rice pests. [Means for solving the problem]

本發明者們為了解決前述課題進行努力研究時,發現作為固形製劑,藉由於選自由氟吡嘧及其鹽所成之群組中之至少1種的有效成分,組合特定之固體載體、界面活性劑及結合劑,並成為特定之被覆型粒劑或擠出型粒劑,對水稻害蟲顯示優異之防除活性,且前述防除活性特別長期間持續,而終至完成本發明。亦即,本發明係提供以下者。The inventors of the present invention have made great efforts to solve the above-mentioned problems and have found that as a solid preparation, at least one active ingredient selected from the group consisting of fluopyridine and its salts is combined with a specific solid carrier, a surfactant and a binder to form a specific coated granule or extruded granule, which exhibits excellent control activity against rice pests, and the control activity lasts particularly long, and finally the present invention is completed. That is, the present invention provides the following.

[1] 一種水稻害蟲防除用固形製劑,其係含有選自由下述式(1)表示之氟吡嘧及其鹽所成之群組中之至少1種的有效成分、固體載體、界面活性劑、以及結合劑,[1] A solid preparation for controlling rice pests, comprising at least one active ingredient selected from the group consisting of fluazifop and its salts represented by the following formula (1), a solid carrier, a surfactant, and a binder.

並為被覆型粒劑或擠出型粒劑。The granules are coated granules or extruded granules.

[2] 如[1]所記載之水稻害蟲防除用固形製劑,其係被覆型粒劑,前述固體載體包含核粒子及增量劑。[2] The solid preparation for controlling rice pests as described in [1] is a coated granule, wherein the solid carrier comprises core particles and an extender.

[3] 如[2]所記載之水稻害蟲防除用固形製劑,其中,前述核粒子的粒徑為63μm~6mm。[3] The solid preparation for controlling rice pests as described in [2], wherein the particle size of the core particles is 63μm~6mm.

[4] 如[2]或[3]所記載之水稻害蟲防除用固形製劑,其中,前述核粒子係選自由矽砂、粒狀碳酸鈣、矽藻土粒、粒狀黏土及浮石所成之群組中之至少1種。[4] A solid preparation for controlling rice pests as described in [2] or [3], wherein the core particles are at least one selected from the group consisting of silica sand, granular calcium carbonate, diatomaceous earth particles, granular clay and pumice.

[5] 如[2]~[4]中任一項所記載之水稻害蟲防除用固形製劑,其中,前述增量劑係選自由黏土、碳酸鈣、高嶺土及二氧化矽所成之群組中之至少1種。[5] A solid preparation for controlling rice pests as described in any one of [2] to [4], wherein the extender is at least one selected from the group consisting of clay, calcium carbonate, kaolin and silicon dioxide.

[6] 如[2]~[5]中任一項所記載之水稻害蟲防除用固形製劑,其中,前述結合劑係選自由流動石蠟、植物油脂、聚乙二醇及聚丙二醇所成之群組中之至少1種。[6] A solid preparation for controlling rice pests as described in any one of [2] to [5], wherein the binder is at least one selected from the group consisting of liquid paraffin, vegetable oil, polyethylene glycol and polypropylene glycol.

[7] 如[1]所記載之水稻害蟲防除用固形製劑,其係擠出型粒劑,前述固體載體包含增量劑,前述界面活性劑包含造粒性改良劑及崩壞・分散劑。[7] The solid preparation for controlling rice pests as described in [1] is an extruded granule, the solid carrier comprises an extender, and the surfactant comprises a granulation improver and a disintegrating/dispersing agent.

[8] 如[7]所記載之水稻害蟲防除用固形製劑,其中,前述增量劑係選自由黏土、滑石、碳酸鈣、高嶺土、二氧化矽及膨潤土所成之群組中之至少1種。[8] A solid preparation for controlling rice pests as described in [7], wherein the extender is at least one selected from the group consisting of clay, talc, calcium carbonate, kaolin, silicon dioxide and bentonite.

[9] 如[7]或[8]所記載之水稻害蟲防除用固形製劑,其中,前述造粒性改良劑係選自由月桂基硫酸鈉、二烷基磺基琥珀酸鈉及烷基苯磺酸鈉所成之群組中之至少1種。[9] A solid preparation for controlling rice pests as described in [7] or [8], wherein the granulation improving agent is at least one selected from the group consisting of sodium lauryl sulfate, sodium dialkyl sulfosuccinate and sodium alkylbenzene sulfonate.

[10] 如[7]~[9]中任一項所記載之水稻害蟲防除用固形製劑,其中,前述崩壞・分散劑係選自由木質素磺酸鈉、木質素磺酸鈣、萘磺酸鈉福爾馬林縮合物、聚丙烯酸鈉、聚氧乙烯烷基醚硫酸鈉、聚氧化烯苯乙烯苯基醚硫酸鈉、聚氧化烯苯乙烯苯基醚磷酸鈉,及聚氧乙烯・聚氧丙烯聚合物硫酸鈉所成之群組中之至少1種。[10] A solid preparation for controlling rice pests as described in any one of [7] to [9], wherein the disintegrating/dispersing agent is at least one selected from the group consisting of sodium lignin sulfonate, calcium lignin sulfonate, sodium naphthalene sulfonate formalin condensate, sodium polyacrylate, polyoxyethylene alkyl ether sodium sulfate, polyoxyalkylene styrene phenyl ether sodium sulfate, polyoxyalkylene styrene phenyl ether sodium phosphate, and polyoxyethylene/polyoxypropylene polymer sodium sulfate.

[11] 如[7]~[10]中任一項所記載之水稻害蟲防除用固形製劑,其中,前述結合劑係選自由聚乙烯醇、糊精、糖類、羧基甲基纖維素鈉、羥基丙基甲基纖維素及甲基纖維素所成之群組中之至少1種。[11] A solid preparation for controlling rice pests as described in any one of [7] to [10], wherein the binder is at least one selected from the group consisting of polyvinyl alcohol, dextrin, sugar, sodium carboxymethylcellulose, hydroxypropylmethylcellulose and methylcellulose.

[12] 一種水稻害蟲防除方法,其係包含將如[1]~[11]中任一項所記載之水稻害蟲防除用固形製劑的有效量,施用在選自由水稻害蟲、水稻、土壤及田水面所成之群組中之至少1種的步驟。[12] A method for controlling rice pests comprises the step of applying an effective amount of a solid preparation for controlling rice pests as described in any one of [1] to [11] to at least one selected from the group consisting of rice pests, rice, soil and field water surface.

[13] 如[12]所記載之水稻害蟲防除方法,其中,前述水稻害蟲係選自由飛蝨類及二化螟類所成之群組中之至少1種。[13] A rice pest control method as described in [12], wherein the rice pest is at least one selected from the group consisting of flies and rice stem borers.

[14] 如[12]或[13]所記載之水稻害蟲防除方法,其中,前述水稻害蟲為藥劑抵抗性害蟲。[14] A rice pest control method as described in [12] or [13], wherein the rice pest is a pesticide-resistant pest.

[15] 如[12]~[14]中任一項所記載之水稻害蟲防除方法,其中,前述水稻害蟲防除用固形製劑的有效量,以前述有效成分量為耕地每10公畝1g~1kg。[15] A rice pest control method as described in any one of [12] to [14], wherein the effective amount of the solid preparation for rice pest control is 1g to 1kg of the active ingredient per 10 hectares of cultivated land.

[16] 一種水稻害蟲防除用固形製劑之製造方法,其係如[2]~[6]中任一項所記載之水稻害蟲防除用固形製劑之製造方法,其特徵為包含: 於前述核粒子加入前述結合劑,或前述結合劑及前述界面活性劑,使其濕潤,而得到濕潤核粒子之濕潤步驟、與 混合前述有效成分、前述界面活性劑及前述增量劑,或前述有效成分及前述增量劑並粉碎,而得到第1混合粉碎物之混合粉碎步驟、與 混合前述濕潤核粒子與第1混合粉碎物,而得到前述濕潤核粒子的表面以第1混合粉碎物被覆的被覆型粒劑之步驟。[16] A method for producing a solid preparation for controlling rice pests, which is a method for producing a solid preparation for controlling rice pests as described in any one of [2] to [6], and is characterized by comprising: a wetting step of adding the aforementioned binder, or the aforementioned binder and the aforementioned surfactant, to the aforementioned core particles to make them wet, thereby obtaining wet core particles; a mixing and grinding step of mixing the aforementioned active ingredient, the aforementioned surfactant and the aforementioned extender, or the aforementioned active ingredient and the aforementioned extender and grinding them to obtain a first mixed and ground product; and a step of mixing the aforementioned wet core particles with the first mixed and ground product to obtain a coated granule in which the surface of the aforementioned wet core particles is coated with the first mixed and ground product.

[17] 一種水稻害蟲防除用固形製劑之製造方法,其係如[7]~[11]中任一項所記載之水稻害蟲防除用固形製劑之製造方法,其特徵為包含: 混合前述有效成分、前述增量劑及前述結合劑並粉碎,或混合前述有效成分、前述增量劑及前述結合劑與前述造粒性改良劑及/或前述崩壞・分散劑並粉碎,而得到第2混合粉碎物之混合粉碎步驟、與 捏合第2混合粉碎物及水,或捏合第2混合粉碎物及水與前述造粒性改良劑及/或前述崩壞・分散劑,而得到捏合物之捏合步驟、與 將前述捏合物以擠出型造粒機成型,而得到擠出型粒劑之步驟。 [發明效果][17] A method for producing a solid preparation for controlling rice pests, which is a method for producing a solid preparation for controlling rice pests as described in any one of [7] to [11], characterized in that it comprises: a mixing and pulverizing step of obtaining a second mixed pulverized product by mixing and pulverizing the aforementioned active ingredient, the aforementioned extender and the aforementioned binder, or mixing and pulverizing the aforementioned active ingredient, the aforementioned extender and the aforementioned binder with the aforementioned granulation improving agent and/or the aforementioned disintegrating/dispersing agent to obtain a mixed pulverized product, and a kneading step of obtaining a kneaded product by kneading the second mixed pulverized product with water, or kneading the second mixed pulverized product with water and the aforementioned granulation improving agent and/or the aforementioned disintegrating/dispersing agent, and a step of molding the mixed pulverized product with an extrusion granulator to obtain an extruded granule. [Invention Effect]

根據本發明,使得提供一種用以防除有害生物,尤其是水稻害蟲之防除活性的持續期間非常長之嶄新的固形製劑,及使用其之水稻害蟲防除方法、以及前述水稻害蟲防除用固形製劑之製造方法變可能。According to the present invention, it is possible to provide a novel solid formulation for controlling harmful organisms, especially rice pests, having a very long duration of control activity, a rice pest control method using the same, and a method for producing the solid formulation for controlling rice pests.

又,氟吡嘧及/或其鹽(較佳為酸加成鹽),與其他藥劑未顯示交差耐藥性,對非目標生物之安全性高,且以低濃度發揮充分優異之防除活性,但根據本發明,此等皆可特別持續長期間。例如,藉由將含有有效成分之氟吡嘧及/或其酸加成鹽的本發明之固形製劑進行1次處理,包含不同時期所發生,且對水稻帶來莫大損害之二化螟類及飛蝨類之2種類以上的水稻害蟲,亦可長期間抑制在低密度。因此,根據本發明,有望提昇稻米的收穫量,變成可解決藥劑感受性的降低、對環境的影響、效果的持續性、對非目標生物的影響、農作業從事者的勞力減低化之既存藥劑所面臨的課題。Furthermore, fluopyridine and/or its salts (preferably acid addition salts) do not show cross-resistance with other drugs, are highly safe against non-target organisms, and exert sufficiently excellent control activity at low concentrations, but according to the present invention, these can be particularly sustained for a long period of time. For example, by treating once with the solid preparation of the present invention containing fluopyridine and/or its acid addition salt as an active ingredient, two or more types of rice pests, including the rice stem borer and the flying lice, which occur at different times and cause great damage to rice, can also be suppressed at a low density for a long period of time. Therefore, according to the present invention, it is expected that the rice yield will be increased, and the problems faced by existing pesticides, such as reduction of pesticide sensitivity, impact on the environment, sustainability of effects, impact on non-target organisms, and reduction of labor for farmers, can be solved.

以下,將本發明根據其合適之實施形態進行詳細說明。Hereinafter, the present invention will be described in detail according to its suitable implementation forms.

<固形製劑> 本發明係提供一種水稻害蟲防除用固形製劑(以下視情況單稱為「固形製劑」),其係含有選自由下述式(1)表示之氟吡嘧及其鹽所成之群組中之至少1種的有效成分、固體載體、界面活性劑、以及結合劑,<Solid preparation> The present invention provides a solid preparation for controlling rice pests (hereinafter referred to as "solid preparation" as the case may be), which contains at least one active ingredient selected from the group consisting of fluopyridine and its salts represented by the following formula (1), a solid carrier, a surfactant, and a binder.

為被覆型粒劑或擠出型粒劑。It is a coated granule or an extruded granule.

根據本發明之固形製劑的一種態樣,提供一種固形製劑(以下視情況單稱為「被覆型粒劑」),其係被覆型粒劑,前述固體載體包含核粒子及增量劑。又,根據本發明之固形製劑的其他態樣,提供一種固形製劑(以下視情況單稱為「擠出型粒劑」),其係擠出型粒劑,前述固體載體包含增量劑,前述界面活性劑包含造粒性改良劑及崩壞・分散劑。According to one aspect of the solid preparation of the present invention, a solid preparation (hereinafter referred to as "coated granules" as appropriate) is provided, which is a coated granule, and the solid carrier comprises core particles and an extender. In addition, according to another aspect of the solid preparation of the present invention, a solid preparation (hereinafter referred to as "extruded granules" as appropriate) is provided, which is an extruded granule, the solid carrier comprises an extender, and the surfactant comprises a granulation improver and a disintegrating/dispersing agent.

尚,在本發明,於「水稻害蟲防除用固形製劑」,除了用以殺蟲或衰弱下述之水稻害蟲的劑之外,包含用以從下述之水稻排除水稻害蟲之劑、用以防治水稻害蟲對水稻的寄生之劑、用以保護水稻免受水稻害蟲侵害之劑。In the present invention, the "solid preparation for controlling rice pests" includes, in addition to agents for killing or weakening the following rice pests, agents for eliminating rice pests from the following rice, agents for preventing and controlling the parasitism of rice pests on rice, and agents for protecting rice from being attacked by rice pests.

(氟吡嘧) 有關本發明之有效成分之氟吡嘧,為上述式(1)所示之化合物,亦即為N-[1-((6-氯吡啶-3-基)甲基)吡啶-2(1H)-亞基]-2,2,2-三氟乙醯胺。氟吡嘧例如可依照國際公開第2012/029672號(專利文獻1)所記載之製造方法合成。(Fluoropyridine) The active ingredient of the present invention, Fluoropyridine, is a compound represented by the above formula (1), that is, N-[1-((6-chloropyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2,2-trifluoroacetamide. Fluoropyridine can be synthesized according to the production method described in International Publication No. 2012/029672 (Patent Document 1), for example.

又,作為有關本發明之有效成分的氟吡嘧之鹽,較佳為酸加成鹽,作為氟吡嘧之酸加成鹽,更佳為農藥上可容許的酸加成鹽。作為前述酸加成鹽,可列舉鹽酸鹽、硝酸鹽、硫酸鹽、磷酸鹽或乙酸鹽等。Furthermore, the salt of fluopyridine as the active ingredient of the present invention is preferably an acid addition salt, and the acid addition salt of fluopyridine is more preferably an acid addition salt acceptable for pesticides. Examples of the acid addition salt include hydrochlorides, nitrates, sulfates, phosphates, and acetates.

作為有關本發明之有效成分,可單獨為氟吡嘧及前述氟吡嘧之鹽當中的1種,亦可為2種以上的組合。The active ingredient of the present invention may be either fluazifop or a salt of fluazifop or a combination of two or more thereof.

(水稻害蟲) 所謂本發明之固形製劑顯示防除活性之水稻害蟲,係表示可食水稻之葉、莖、根、穗的害蟲;可從水稻之葉、莖、穗吸汁之害蟲。作為這般的水稻害蟲,雖並非被特別限定者,但例如作為農園藝上之害蟲,可列舉鱗翅目(蝶蛾目)害蟲(分秘夜蛾(Mythimna Separata)、瘤野螟、Cnaphalocrocis patnalis(Marasmia patnalis)、紅帶黃夜蛾(Naranga aenescens)、稻弄蝶(Parnara guttata)、鱗翅夜蛾(Plusia festucae)、勞氏黏蟲(Mythimna loreyi)、稻尺蠖(Protodeltote distinguenda)、斜紋夜蛾(Spodoptera depravata)、隱紋穀弄蝶(Pelopidas mathias)等;二化螟(二化螟蟲、Chilo suppressalis)、三化螟(三化螟蟲、Scirpophaga incertulas)、盜污陰夜蛾(Sesamia inferens)、Scirphophaga innotata、Chilo polychrysus、Chilo auricilius等之二化螟類)、半翅目(半翅目)害蟲(稻麥蚜、長角麥蚜、稻根蚜蟲、粗長毛禾根蚜等之蚜蟲類;黑尾葉蟬、電光葉蟬等之葉蟬類;灰飛蝨、褐飛蝨、白背飛蝨等之飛蝨類;紅條盲椿、稻黑椿象、中華稻緣椿、白星蝽、長肩棘緣椿象、白星椿象、稻綠蝽、水稻葉蝽等之椿象類等)、鞘翅目害蟲(水稻水象鼻蟲、稻象鼻蟲、豆芫菁、稻負泥蟲、稻鐵甲蟲(Dicladispa armigera)等)、蜱蟎亞綱(Steneotarsonemus spinki等)、膜翅目害蟲、直翅目害蟲(小翅稻蝗、黑頸鉤額螽類、螻蛄等)、雙翅目害蟲(水稻潛葉蠅、稻稈潛蠅、稻癭蚊(Orseolia oryzae)等)、纓翅目害蟲(稻薊馬、稻管薊馬等)、植物寄生性線蟲(貝西滑刃線蟲、水稻根瘤線蟲((Meloidogynae graminicola)等)等,可為此等當中之1種單獨,亦可為2種以上的組合。其中,較佳可列舉蝶蛾目害蟲、半翅目害蟲、纓翅目害蟲、雙翅目害蟲,及鞘翅目害蟲,更佳為飛蝨類、二化螟類及葉蟬類,更佳可列舉二化螟、三化螟、灰飛蝨、褐飛蝨、白背飛蝨、黑尾葉蟬、電光葉蟬,再更佳可列舉此等當中之飛蝨類及二化螟類。(Rice pests) The rice pests that the solid preparation of the present invention shows control activity against are pests that can feed on the leaves, stems, roots and ears of rice; and pests that can suck sap from the leaves, stems and ears of rice. Although such rice pests are not specifically limited, for example, as pests in agriculture, there are Lepidoptera (Order Butterflies) pests (Mythimna Separata, Cnaphalocrocis patnalis (Marasmia patnalis), Naranga aenescens, Parnara guttata, Plusia festucae, Mythimna loreyi, Protodeltote distinguenda, Spodoptera depravata, Pelopidas mathias, etc.); Chilo suppressalis (Chilo suppressalis, suppressalis), yellow stem borer (Scirpophaga incertulas), soil thief moth (Sesamia inferens), Scirphophaga innotata, Chilo polychrysus, Chilo auricilius, etc.), Hemiptera (aphids such as rice aphid, long-horned wheat aphid, rice root aphid, thick long-haired grass root aphid, etc.; leaf hoppers such as black-tailed leaf hopper, electric leaf hopper, etc.; flies such as gray fly, brown fly, white-backed fly, etc.; stink bugs such as red-striped blind tree, black rice stink bug, Chinese rice edge tree, white-spotted stink bug, long-shouldered spiny edge stink bug, white-spotted stink bug, rice green stink bug, rice leaf bug, etc.), Coleoptera (rice water weevil, rice weevil, bean sedge, rice mudworm, rice iron beetle (Dicladispa armigera), etc.), ticks (Steneotarsonemus spinki, etc.), Hymenoptera pests, Orthoptera pests (small-winged rice grasshoppers, black-necked hooked grasshoppers, crickets, etc.), Diptera pests (rice leaf miners, rice stem miners, rice gall midges (Orseolia oryzae), etc.), Lycoptera pests (rice weevils, rice pipe weevils, etc.), plant parasitic nematodes (Besse nematodes, rice root knot nematodes (Meloidogynae graminicola), etc., and may be one of them alone or a combination of two or more thereof. Among them, preferably, pests of the order Butterflies, Hemiptera, Leptera, Diptera, and Coleoptera can be listed, more preferably, flies, striped stem borers, and leaf crickets can be listed, more preferably, striped stem borers, yellow stem borers, gray flies, brown flies, white-backed flies, black-tailed leaf crickets, and electric leaf crickets can be listed, and more preferably, flies and striped stem borers among these can be listed.

又,作為前述水稻害蟲,可為對於益達胺(Imidacloprid)等之尼古丁性乙醯膽鹼受體作用藥;芬普尼、益斯普等之GABA受體作用性化合物;剋安勃等之二醯胺化合物等之既存藥劑,降低感受性之藥劑抵抗性害蟲。In addition, the rice pests mentioned above may be pests resistant to existing drugs that reduce the sensitivity of the drugs to nicotine acetylcholine receptors such as imidocloprid, GABA receptor-acting compounds such as fipronil and isaprol, and diamide compounds such as cyproconazole.

(其他有害生物防除劑) 作為本發明之固形製劑,由於有效成分之氟吡嘧及其鹽為以其本身對於上述水稻害蟲顯示優異之防除活性者,雖若含有該氟吡嘧及/或其鹽即可,但由於藉由與其他有害生物防除劑混合使用,亦可對更多之害蟲顯示更為優異之防除活性,故可進一步含有其他有害生物防除劑。作為可含有之其他有害生物防除劑,可列舉殺蟲劑(包含殺蟎劑及殺線蟲劑)、殺菌劑、除草劑及植物成長調節劑等,作為具體的藥劑,例如可列舉農藥手冊(The Pesticide Manual,第17版 The British Crop Protection Council 發行)及(SHIBUYA INDEX,2014年,SHIBUYA INDEX RESEARCH GROUP發行)所記載者。此等當中,作為前述其他有害生物防除劑較佳者為殺蟲劑及殺菌劑。(Other pest control agents) As the solid preparation of the present invention, since the active ingredients fluopyram and its salts show excellent control activity against the above-mentioned rice pests by themselves, although it is sufficient to contain the fluopyram and/or its salts, it can also show more excellent control activity against more pests by mixing with other pest control agents, so other pest control agents can be further contained. As other pest control agents that may be contained, insecticides (including miticides and nematicides), fungicides, herbicides and plant growth regulators can be listed. As specific agents, for example, those listed in the Pesticide Manual (17th edition, published by The British Crop Protection Council) and (SHIBUYA INDEX, 2014, published by SHIBUYA INDEX RESEARCH GROUP) can be listed. Among these, insecticides and fungicides are preferred as the other pest control agents mentioned above.

作為前述其他有害生物防除劑的較佳之例,例如可列舉有機磷酸酯系化合物、苯基胺基甲酸酯系化合物、沙蠶毒素衍生物、有機氯系化合物、除蟲菊酯系化合物、苯甲醯脲系化合物、保幼激素樣化合物、蛻皮酮樣化合物、類尼古丁系化合物、神經細胞之鈉通道阻滯劑、殺蟲性大環狀內酯、γ-胺基丁酸(GABA)拮抗劑、蘭諾定受體(Ryanodine receptor)作用性化合物、殺蟲性尿素類、BT劑、昆蟲病原病毒劑、聚醚系抗生物質、硫胺素拮抗藥,及磺胺(Sulfa)劑・葉酸拮抗藥摻合劑等。Preferred examples of the aforementioned other pest control agents include, for example, organophosphate compounds, phenylcarbamate compounds, worm toxin derivatives, organochlorine compounds, pyrethroid compounds, benzoylurea compounds, juvenile hormone-like compounds, scutellaria-like compounds, nicotine-like compounds, sodium channel blockers of nerve cells, insecticidal macrolides, γ-aminobutyric acid (GABA) antagonists, ryanodine receptor-active compounds, insecticidal ureas, BT agents, insect pathogenic virus agents, polyether antibiotics, thiamine antagonists, and sulfa (sulfa) agent and folic acid antagonist mixtures.

更具體而言,作為殺蟲劑,可列舉如歐殺松(acephate)、二氯松(dichlorvos)、EPN、撲滅松(fenitrothion)、芬滅松(fenamifos)、普硫松(prothiofos)、佈飛松(profenofos)、白克松(pyraclofos)、甲基毒死蜱(chlorpyrifos-methyl)、大利松(diazinon)、福賽絕(fosthiazate)、依米塞松(imicyafos)、褔瑞松(phorate)之有機磷酸酯系化合物;如納乃得(methomyl)、硫敵克(thiodicarb)、得滅克(aldicarb)、歐殺滅(oxamyl)、安丹(propoxur)、加保利(carbaryl)、丁基滅必蝨(fenobucarb)、乙硫苯威(ethiofencarb)、芬硫克(fenothiocarb)、比加普(pirimicarb)、加保扶(carbofuran)、丁基加保扶(carbosulfan)、免扶克(benfuracarb)之苯基胺基甲酸酯系化合物;如培丹(cartap)、硫賜安(thiocyclam)之沙蠶毒素衍生物;如大克蟎(dicofol)、四氯殺蟎碸(tetradifon)之有機氯系化合物;如百滅靈(permethrin)、七氟菊酯(tefluthrin)、賽滅寧(cypermethrin)、第滅靈(deltamethrin)、三氟氯氰菊酯(cyhalothrin)、芬化利(fenvalerate)、氟氰胺菊酯(fluvalinate)、依芬寧(ethofenprox)、矽護芬(silafluofen)、三氟氯氰菊酯(cyhalothrin)之除蟲菊酯系化合物;如二福隆(diflubenzuron)、得福隆(teflubenzuron)、二福隆(flufenoxuron)、克福隆(chlorfluazuron)之苯甲醯脲系化合物;如美賜平(methoprene)之保幼激素樣化合物;如可芬諾(Chromafenozide)之蛻皮酮樣化合物;如益達胺(imidacloprid)、可尼丁(clothianidin)、噻蟲嗪(thiamethoxam)、亞滅培(acetamiprid)、烯啶蟲胺(nitenpyram)、噻蟲啉(thiacloprid)、達特南(dinotefuran)、速殺氟(sulfoxaflor)、氟吡呋喃酮(flupyradifurone)、二克滅(dicloromezotiaz)、三氟苯嘧啶(triflumezopyrim)之尼古丁性乙醯膽鹼受體作用藥;如氟蟲胺(flubendiamide)、剋安勃(chlorantraniliprole)、氰蟲醯胺(cyantraniliprole)、環溴蟲醯胺(cyclaniliprole)、氟氰蟲醯胺(tetraniliprole)之二醯胺化合物;如益斯普(ethiprole)、芬普尼(fipronil)、吡蟲腈(pyrafluprole)、吡瑞蟲腈(pyriprole)、溴氟苯胺(broflanilide)、氟米塔麥(fluxametamide)之GABA受體作用性化合物;如嗒蟎酮(pyridaben)、芬普蟎(fenpyroxymate)、嘧蟎醚(pyrimidifen)、吡蟎胺(tebufenpyrad)、唑蟲醯胺(tolfenpyrad)之呼吸鏈電子傳達系複合體I抑制化合物;如丁氟蟎酯(cyflumetofen)、塞比芬(cyenopyrafen)、氟他胺(pyflbumide)之呼吸鏈電子傳達系複合體II抑制化合物;如嘧蟎酯(fluacrypyrim)、亞醌蟎(acequinocyl)、氟米克(flometoquin)之呼吸鏈電子傳達系複合體III抑制化合物;如賜派芬(spirodiclofen)、螺甲蟎酯(spiromesifen)、螺蟲乙酯(spirotetramat)之ACCase抑制化合物;如賜諾殺(spinosad)、阿維菌素(avermectin)、倍脈心(milbemycin)、司平托列(spinetoram)、列比美汀(lepimectin)、因滅汀苯甲酸鹽(emamectin benzoate)之大環內酯(Macrolide)化合物。More specifically, as insecticides, there can be mentioned acephate, dichlorvos, EPN, fenitrothion, fenamifos, prothiofos, profenofos, pyraclofos, chlorpyrifos-methyl, diazinon, fosthiazate, imicyafos, phorate ) organic phosphate compounds; such as methomyl, thiodicarb, aldicarb, oxamyl, propoxur, carbaryl, fenobucarb, ethiofencarb, fenothiocarb, pirimicarb, carbofuran, carbosulfan, benfuracarb, b) phenylcarbamate compounds; sandworm toxin derivatives such as cartap and thiocyclam; organochlorine compounds such as dicofol and tetradifon; such as permethrin, tefluthrin, cypermethrin, deltamethrin, cyhalothrin, fenvalerate, fluvalinate , ethofenprox, silafluofen, cyhalothrin; benzoylurea compounds such as diflubenzuron, teflubenzuron, flufenoxuron, chlorfluazuron; juvenile hormone-like compounds such as methoprene; dermatophenone-like compounds such as chromafenozide; imidacl Nicotine acetylcholine receptor-acting drugs such as oprid, clothianidin, thiamethoxam, acetamiprid, nitenpyram, thiacloprid, dinotefuran, sulfoxaflor, flupyradifurone, dicloromezotiaz, and triflumezopyrim; such as flubendiamide, diamide compounds such as ubendiamide, chlorantraniliprole, cyantraniliprole, cyclaniliprole, and tetraniliprole; GA such as ethiprole, fipronil, pyrafluprole, pyriprole, broflanilide, and fluxametamide BA receptor-active compounds; respiratory chain electron transport complex I inhibitory compounds such as pyridaben, fenpyroxymate, pyrimidifen, tebufenpyrad, tolfenpyrad; respiratory chain electron transport complex II inhibitory compounds such as cyflumetofen, cyenopyrafen, pyflbumide; respiratory chain electron transport complex II inhibitory compounds such as fluacrypyrim, ace Respiratory chain electron transport system complex III inhibitory compounds such as quinocyl and flometoquin; ACCase inhibitory compounds such as spirodiclofen, spiromesifen, and spirotetramat; Macrolide compounds such as spinosad, avermectin, milbemycin, spinetoram, lepimectin, and emamectin benzoate.

進而,作為其他化合物,可列舉布酚淨(buprofezin)、噻蟎酮(hexythiazox)、三亞蟎(amitraz)、殺蟲脒(chlordimeform)、依殺蟎(ethoxazole)、派滅淨(pymetrozine)、聯苯肼(bifenazate)、氟尼胺(flonicamid)、蟲蟎腈(chlorfenapyr)、百利普芬(pyriproxyfen)、茚蟲威(indoxacarb)、三氟甲吡醚(pyridalyl)、哌氟喹腙(pyrifluquinazon)、氰氟蟲腙(metaflumizone)、愛美松(hydramethylnon)、唑蚜威(triazamate)、雙丙環蟲酯(afidopyropen)、瑞那富寧(renofluthrin)、氯普亞列寧(chloroprallethrin)、氯氟氰蟲醯胺(cyhalodiamide)、氟吲哚辛(fluazaindolizine)、ε-甲氧苄氟菊酯(epsilon-metofluthrin)、ε-沒氟菊酯(epsilon-momfluorothrin)、κ-畢芬寧(kappa-bifenthrin)、κ-七氟菊酯(kappa-tefluthrin)、氟殺逢(fluhexafon)、替奧沙芬(tioxazafen)、沒氟菊酯(momfluorothrin)、右旋七氟甲醚菊酯(heptafluthrin)、嘧蟎胺(pyriminostrobin)、環氧蟲啶(cycloxaprid)、異環賽蘭(isocycloseram)、歐賽菲(oxazosulfyl)、替克樂比薩佛(tyclopyrazoflor)、賜派酮(spiropidion)、阿克那比(acynonapyr)、敵普派達(dimpropyridaz)、有機金屬系化合物、二硝基系化合物、有機硫化合物、尿素系化合物、三嗪系化合物、肼系化合物,亦可列舉如BT劑、昆蟲病原病毒劑等之微生物農藥。又,作為前述殺蟲劑,亦可列舉此等之農藥上可容許的酸加成鹽。Further, as other compounds, there can be listed buprofezin, hexythiazox, amitraz, chlordimeform, ethoxazole, pymetrozine, bifenazate, flonicamid, chlorfenapyr, pyriproxyfen, indoxacarb, trifluoromethylpyrifos, and chlorfenapyr. pyridalyl), pyrifluquinazon, metaflumizone, hydramethylnon, triazamate, afidopyropen, renofluthrin, chloroprallethrin, cyhalodiamide, fluazaindolizine, ε-methobenzyl Epsilon-metofluthrin, epsilon-momfluorothrin, kappa-bifenthrin, kappa-tefluthrin, fluhexafon, tioxazafen, momfluorothrin, heptafluthrin, pyriminostrobin ), cycloxaprid, isocycloseram, oxazosulfyl, tyclopyrazoflor, spiropidion, acynonapyr, dimpropyridaz, organometallic compounds, dinitro compounds, organosulfur compounds, urea compounds, triazine compounds, hydrazine compounds, and microbial pesticides such as BT agents and insect pathogenic virus agents. In addition, as the aforementioned pesticides, the acid addition salts of these pesticides that are allowed.

作為前述殺蟲劑,雖可為上述當中之1種單獨,亦可為2種以上的組合,但其中,作為較佳之殺蟲劑,可列舉培丹(cartap)、硫賜安(thiocyclam)、褔瑞松(phorate)、氟蟲胺(flubendiamide)、剋安勃(chlorantraniliprole)、氰蟲醯胺(cyantraniliprole)、加保扶(carbofuran)、芬普尼(fipronil)。The aforementioned insecticide may be one of the above-mentioned insecticides alone or a combination of two or more thereof. Among them, preferred insecticides include cartap, thiocyclam, phorate, flubendiamide, chlorantraniliprole, cyantraniliprole, carbofuran, and fipronil.

又,更具體而言,作為殺菌劑,例如可列舉如嘧菌酯(azoxystrobin)、克收欣(kresoxym-methyl)、三氟敏(trifloxystrobin)、苯氧菌胺(metominostrobin)、肟醚菌胺(orysastrobin)等之甲氧基丙烯酸酯(strobilurin)系化合物;滅派林(mepanipyrim)、嘧黴胺(pyrimethanil)、賽普洛(cyprodinil)之苯胺嘧啶(anilinopyrimidine)系化合物;如三泰芬(triadimefon)、比多農(bitertanol)、氟菌唑(triflumizole)、滅特座(metoconazole)、丙環唑(propiconazole)、戊菌唑(penconazole)、氟矽唑(flusilazole)、邁克尼(myclobutanil)、環克唑(cyproconazole)、戊唑醇(tebuconazole)、己唑醇(hexaconazole)、咪鮮安(prochloraz)、矽氟唑(simeconazole)之唑系化合物;如滅蟎猛(quinomethionate)之喹喔啉系化合物;如代森猛(maneb)、代森鋅(zineb)、代森錳鋅(mancozeb)、聚苯基胺基甲酸酯(polycarbamate)、丙森鋅(propineb)之二硫代苯基胺基甲酸酯系化合物;如乙黴威(diethofencarb)之苯基苯基胺基甲酸酯系化合物;如四氯異苯(chlorothalonil)、五氯硝基苯(quintozene)之有機氯系化合物;如苯菌靈(benomyl)、甲基硫菌靈(thiophanate-methyl)、卡苯達唑(carbendazole)之苯并咪唑系化合物;如甲霜靈(metalaxyl)、悉霜靈(oxadixyl)、甲呋醯胺(ofurase)、苯霜靈(benalaxyl)、呋霜靈(furalaxyl)、酯菌胺(cyprofuram)之苯基醯胺系化合物;如苯氟醯胺(dichlofluanid)之次磺酸系化合物;如氫氧化銅(copper hydroxide)、快得寧(oxine-copper)之銅系化合物;如羥基異噁唑(hydroxyisoxazole)之異噁唑系化合物;如福賽得(fosetyl-aluminium)、脫克松(tolclofos-methyl)之有機磷系化合物;如克菌丹(captan)、四氯丹(captafol)、滅菌丹(folpet)之N-鹵素硫代烷基系化合物;如二甲菌核利(procymidone)、異菌脲(iprodione)、乙烯菌核利(vinchlozolin)之二碳二亞胺(Dicarboximide)系化合物;如福多寧(flutolanil)、滅普寧(mepronil)、福拉比(furametpyr)、噻呋醯胺(thifluzamide)、白克列(boscalid)、平硫瑞(penthiopyrad)之羧基苯胺系化合物;如丁基嗎啉(fenpropimorph)、烯醯嗎啉(dimethomorph)之嗎啉系化合物;如三苯基氫氧化錫(fenthin hydroxide)、三苯基乙酸錫(fenthin acetate)之有機錫系化合物;如咯菌腈(fludioxonil)、拌種咯(fenpiclonil)之氰基吡咯系化合物。More specifically, as fungicides, for example, strobilurin compounds such as azoxystrobin, kresoxym-methyl, trifloxystrobin, metominostrobin, orysastrobin, etc.; anilinopyrimidine compounds such as mepanipyrim, pyrimethanil, cyprodinil, etc.; ne compounds; such as triadimefon, bitertanol, triflumizole, metoconazole, propiconazole, penconazole, flusilazole, myclobutanil, cyproconazole, tebuconazole, hexaconazole, prochloraz ), simeconazole; quinoxaline compounds such as quinomethionate; dithiophenylcarbamate compounds such as maneb, zineb, mancozeb, polycarbamate, and propineb; phenylphenylcarbamate compounds such as diethofencarb; chlorothalonil, quintozene, and pentachloronitrobenzene; e) organochlorine compounds; benzimidazole compounds such as benomyl, thiophanate-methyl, and carbendazole; phenylamide compounds such as metalaxyl, oxadixyl, ofurase, benalaxyl, furaxyl, and cyprofuram; sulfenic acid compounds such as dichlofluanid; copper hydroxide compounds such as Copper compounds such as hydroxide and oxine-copper; isoxazole compounds such as hydroxyisoxazole; organophosphorus compounds such as fosetyl-aluminium and tolclofos-methyl; N-halogen sulfide alkyl compounds such as captan, captafol, and folpet; procymidone, iprodione, and ethylenediamine; Dicarboximide compounds such as vinchlozolin; carboxyaniline compounds such as flutolanil, mepronil, furametpyr, thifluzamide, boscalid and penthiopyrad; morpholine compounds such as fenpropimorph and dimethomorph; organotin compounds such as fenthin hydroxide and fenthin acetate; cyanopyrrole compounds such as fludioxonil and fenpiclonil.

進而,作為其他化合物,可列舉三環唑(tricyclazole)、咯喹酮(pyroquilon)、環丙醯菌胺(carpropamid)、雙氯氰菌胺(diclocymet)、氰菌胺(fenoxanil)、四氯苯酞(fthalide)、扶吉胺(fluazinam)、霜脲氰(cymoxanil)、賽福寧(triforine)、比芬諾(pyrifenox)、氯苯嘧啶醇(fenarimol)、苯銹啶(fenpropidin)、戊菌隆(pencycuron)、富米綜(ferimzone)、賽座滅(cyazofamid)、丙森鋅(iprovalicarb)、苯噻菌胺(benthiavalicarb-isopropyl)、雙胍苯磺酸鹽(iminoctadin-albesilate)、賽芬胺(cyflufenamid)、嘉賜徵素(kasugamycin)、井岡黴素(validamycin)、鏈黴素(streptomycin)、噁喹酸(oxolinic-acid)、特布弗喹(tebufloquin)、烯丙苯噻唑(probenazole)、噻醯菌胺(tiadinil)、亞汰尼(isotianil)、亞賜圃(isoprothiolane)、托普洛卡(tolprocarb)、氟唑菌醯羥胺(pydiflumetofen)、皮卡布西(picarbutrazox)、杏仁菌酯(mandestrobin)、大芬滅替松(dipymetitrone)、必記福敏(pyraziflumid)、奧賽普林(oxathiapiprolin)、平氟芬(penflufen)、fluoxapiprolin、吡啶醯菌胺(florylpicoxamid)、氟醚菌醯胺(fluopimomide)、ipfenoquin、氟因菌唑(fluindapyr)、異氟西波(isoflucypram)、昆諾浮美林(quinofumelin)、methyltetraprole、必噠克緹(pyridachlometyl)、吡普洛潑尼(pyrapropoyne)、胺基吡芬(aminopyrifen)、inpyrifluxam、二氯苯賽鐸(dichlobentiazox)等。又,作為前述殺菌劑,亦可列舉此等之農藥上可容許的酸加成鹽。Further, as other compounds, tricyclazole, pyroquilon, carpropamid, diclocymet, fenoxanil, fthalide, fluazinam, cymoxanil, triforine, pyrifenox, fenarimol, fenpropidin, pencycuron, fumifenox, fenoxanil ... ferimzone, cyazofamid, iprovalicarb, benthiavalicarb-isopropyl, iminoctadin-albesilate, cyflufenamid, kasugamycin, validamycin, streptomycin, oxolinic-acid, tebufloquin, prothiazole benazole), tiadinil, isotianil, isoprothiolane, tolprocarb, pydiflumetofen, picarbutrazox, mandestrobin, dipymetitrone, pyraziflumid, oxathiapiprolin, penflufen, fluoxapiprol in, florylpicoxamid, fluopimomide, ipfenoquin, fluindapyr, isoflurane, quinofumelin, methyltetraprole, pyridachlometyl, pyrapropoyne, aminopyrifen, inpyrifluxam, dichlobentiazox, etc. In addition, as the aforementioned fungicides, the acid addition salts of these pesticides that are permitted can also be listed.

作為前述殺菌劑,雖可為上述當中之1種單獨,亦可為2種以上的組合,但其中,作為較佳之殺菌劑,可列舉嘧菌酯(azoxystrobin)、肟醚菌胺(orysastrobin)、噻呋醯胺(thifluzamide)、福拉比(furametpyr)、四氯苯酞(fthalide)、烯丙苯噻唑(probenazole)、阿拉酸式苯-S-甲基(acibenzolar-S-methyl)、噻醯菌胺(tiadinil)、亞汰尼(isotianil)、亞賜圃(isoprothiolane)、托普洛卡(tolprocarb)、環丙醯菌胺(carpropamid)、雙氯氰菌胺(diclocymet)、氰菌胺(fenoxanil)、三環唑(tricyclazole)、咯喹酮(pyroquilon)、富米綜(ferimzone)、特布弗喹(tebufloquin)、矽氟唑(simeconazole)、井岡黴素(validamycin)、嘉賜徵素(Kasugamycin)、戊菌隆(pencycuron)、平氟芬(penflufen)、二氯苯賽鐸(dichlobentiazox)。The aforementioned fungicide may be any one of the above or a combination of two or more thereof. Among them, preferred fungicides include azoxystrobin, orysastrobin, thifluzamide, furametpyr, fthalide, probenazole, acibenzolar-S-methyl, tiadinil, isotianil, isoprothiolane, toprolactone, and thiamethoxam. tolprocarb, carpropamid, diclocymet, fenoxanil, tricyclazole, pyroquilon, ferimzone, tebufloquin, simeconazole, validamycin, kasugamycin, pencycuron, penflufen, dichlobentiazox.

(添加劑) 本發明之固形製劑可藉由於有效成分之氟吡嘧使用添加劑(較佳為農藥上可容許之添加劑)來製造。作為其形態,可列舉粒劑,更具體而言,為含有固體載體、界面活性劑及結合劑之被覆型粒劑或擠出型粒劑。(Additives) The solid preparation of the present invention can be produced by using an additive (preferably an additive permitted for pesticides) with the active ingredient fluopyridine. As its form, granules can be listed, more specifically, coated granules or extruded granules containing a solid carrier, a surfactant and a binder.

[固體載體] 作為前述固體載體,可列舉滑石、膨潤土、黏土、高嶺土、矽藻土、蛭石、沸石、二氧化矽、碳酸鈣、硫酸銨、矽砂、矽石、浮石等。[Solid carrier] As the aforementioned solid carrier, there can be listed talc, bentonite, clay, kaolin, diatomaceous earth, vermiculite, zeolite, silicon dioxide, calcium carbonate, ammonium sulfate, silica sand, silica, pumice, etc.

本發明之被覆型粒劑係前述固體載體當中,含有核粒子及增量劑。又,本發明之擠出型粒劑係前述固體載體當中,含有增量劑,進而,較佳為未含有前述核粒子,亦即前述固體載體僅包含前述增量劑而成。The coated granules of the present invention are the solid carriers containing core particles and extenders. Furthermore, the extruded granules of the present invention are the solid carriers containing extenders, and preferably do not contain the core particles, that is, the solid carriers only contain the extenders.

在本發明,所謂「核粒子」,係表示粒徑為63μm以上之固體載體,作為前述粒徑,較佳為63μm~6mm的範圍內,更佳為75μm~2mm的範圍內,再更佳為106μm~2mm的範圍內。有關本發明之核粒子或固體載體的「粒徑」,係指將粒子對平面投影時之圓的直徑,投影面並非圓形的情況(粒子為平板狀、板狀等、棒狀、多角狀等之形狀時),係指其外接圓的直徑。作為這般的核粒子,若為滿足前述粒徑者雖並未特別限制,但可列舉粒狀之矽砂、矽藻土、浮石、黏土、碳酸鈣等,可為此等當中之1種單獨,亦可為2種以上的組合。又,在本發明,粒狀之碳酸鈣(粒狀碳酸鈣)及粒狀之黏土(粒狀黏土)中,除了各礦物之粉碎物的粒子之外,亦包含分別將粒徑小之礦物微粉與膨潤土或下述之結合劑等混合並進行捏合,並藉由擠出造粒或破碎造粒等,而成為粒狀之造粒物的粒子。In the present invention, the so-called "core particle" refers to a solid carrier with a particle size of 63 μm or more. The particle size is preferably in the range of 63 μm to 6 mm, more preferably in the range of 75 μm to 2 mm, and even more preferably in the range of 106 μm to 2 mm. The "particle size" of the core particle or solid carrier of the present invention refers to the diameter of the circle when the particle is projected onto a plane. When the projection plane is not circular (when the particle is in the shape of a flat plate, plate, rod, polygon, etc.), it refers to the diameter of its circumscribed circle. As such core particles, there are no particular limitations as long as they satisfy the aforementioned particle size, but examples thereof include granular silica sand, diatomaceous earth, pumice, clay, calcium carbonate, etc., and they may be one of them alone or a combination of two or more thereof. In the present invention, in addition to the particles of the crushed product of each mineral, the granular calcium carbonate (granular calcium carbonate) and the granular clay (granular clay) also include particles of granulated products obtained by mixing and kneading a mineral fine powder having a small particle size with bentonite or the following binder, etc., and then extruding or crushing the granulated products.

在本發明,所謂「增量劑」,係主要以稀釋有效成分為目的使用者,具體而言,係表示粒徑為未滿63μm之固體載體。作為這般的增量劑,若為滿足前述粒徑者,雖並未特別限制,但在前述被覆型粒劑較佳,從在下述之被覆型粒劑之製造方法的粉碎步驟變容易的觀點來看,係選自由黏土、碳酸鈣、高嶺土及二氧化矽所成之群組中之至少1種。又,在前述擠出型粒劑較佳,從同樣的觀點來看,係選自由黏土、滑石、碳酸鈣、高嶺土、二氧化矽及膨潤土所成之群組中之至少1種。In the present invention, the so-called "bulking agent" is mainly used for diluting the active ingredient, and specifically refers to a solid carrier with a particle size of less than 63 μm. As such a bulking agent, if it satisfies the aforementioned particle size, although there is no particular limitation, it is preferably the aforementioned coated granules, and from the viewpoint of facilitating the pulverization step in the following method for producing the coated granules, at least one of the group consisting of clay, calcium carbonate, kaolin and silicon dioxide. In addition, it is preferably the aforementioned extruded granules, and from the same viewpoint, at least one of the group consisting of clay, talc, calcium carbonate, kaolin, silicon dioxide and bentonite.

[界面活性劑] 作為前述界面活性劑,可列舉陰離子性界面活性劑、陽離子性界面活性劑及非離子性界面活性劑等。[Surfactant] As the aforementioned surfactant, there can be listed anionic surfactants, cationic surfactants, and nonionic surfactants.

作為本發明之被覆型粒劑所含有之界面活性劑,於上述當中,較佳為具有前述核粒子之濕潤作用者,具體而言,例如可列舉木質素磺酸鈉、月桂基硫酸鈉、萘磺酸鈉福爾馬林縮合物、聚氧化烯烷基醚硫酸鈉、烷基苯磺酸鈉、二烷基磺基琥珀酸鈉、聚氧化烯苯乙烯苯基醚硫酸鈉、聚氧化烯苯乙烯苯基醚磷酸鈉等之陰離子性界面活性劑;聚氧化烯山梨糖醇脂肪酸酯(聚氧化烯山梨糖醇單月桂酸酯等)、山梨糖醇脂肪酸酯、蔗糖脂肪酸酯、聚氧化烯蓖麻油、聚氧化烯硬化蓖麻油、聚氧化烯烷基醚、聚氧化烯烷基苯基醚、聚氧化烯苯乙烯基苯基醚、聚氧乙烯・聚氧丙烯嵌段聚合物、聚氧化烯烷基胺等之非離子性界面活性劑,可為此等當中之1種單獨,亦可為2種以上的組合。前述界面活性劑當中,前述非離子界面活性劑或其組合,在本發明之被覆型粒劑,可與下述之結合劑以相同目的使用。As the surfactant contained in the coated granules of the present invention, among the above, it is preferred that the surfactant has the wetting effect of the core particles mentioned above, and specifically, for example, anionic surfactants such as sodium lignin sulfonate, sodium lauryl sulfate, sodium naphthalene sulfonate formalin condensate, polyoxyalkylene alkyl ether sodium sulfate, sodium alkylbenzene sulfonate, sodium dialkyl sulfosuccinate, polyoxyalkylene styrene phenyl ether sodium sulfate, polyoxyalkylene styrene phenyl ether sodium phosphate, etc. can be listed; The nonionic surfactants such as oxyalkylene sorbitan fatty acid esters (polyoxyalkylene sorbitan monolaurate, etc.), sorbitan fatty acid esters, sucrose fatty acid esters, polyoxyalkylene castor oil, polyoxyalkylene hydrogenated castor oil, polyoxyalkylene alkyl ethers, polyoxyalkylene alkylphenyl ethers, polyoxyalkylene styrylphenyl ethers, polyoxyethylene-polyoxypropylene block polymers, polyoxyalkylene alkylamines, etc. may be used alone or in combination of two or more. Among the above-mentioned surfactants, the above-mentioned nonionic surfactants or their combination may be used in the coated particles of the present invention with the following binder for the same purpose.

尚,在本說明書,「聚氧化烯」係表示聚氧乙烯及聚氧丙烯當中之1種或此等之混合物。In the present specification, "polyoxyalkylene" means one of polyoxyethylene and polyoxypropylene or a mixture thereof.

本發明之擠出型粒劑係前述界面活性劑當中,含有造粒性改良劑及崩壞・分散劑。The extruded granules of the present invention contain a granulation improving agent and a disintegrating and dispersing agent in the aforementioned surfactant.

在本發明,所謂「造粒性改良劑」,係表示上述界面活性劑當中,在下述之製造方法之捏合步驟,具有提昇水與其他成分之相容的作用者,具體而言,表示定為0.1%水溶液時,在25℃,顯示10~35mN/m的表面張力值之界面活性劑。作為這般的造粒性改良劑,若為滿足上述表面張力者,雖並未特別限制,但在前述擠出型粒劑,較佳為選自由月桂基硫酸鈉、二烷基磺基琥珀酸鈉及烷基苯磺酸鈉所成之群組中之至少1種。In the present invention, the so-called "granulation improver" refers to the surfactants mentioned above, which have the function of improving the compatibility of water and other ingredients in the kneading step of the following production method. Specifically, it refers to the surfactants that show a surface tension value of 10 to 35 mN/m at 25° C. when it is set as a 0.1% aqueous solution. As such a granulation improver, as long as it satisfies the above surface tension, although it is not particularly limited, in the above extruded granules, it is preferably at least one selected from the group consisting of sodium lauryl sulfate, sodium dialkyl sulfosuccinate and sodium alkylbenzene sulfonate.

在本發明,所謂「崩壞・分散劑」,係表示上述界面活性劑當中,除了相當於前述造粒性改良劑者之外,具有提昇對前述有效成分之其他成分之分散性及崩壞性當中的至少任一個之作用者。作為這般的崩壞・分散劑,可列舉較佳為陰離子性界面活性劑,更佳為木質素磺酸鈉、木質素磺酸鈣、萘磺酸鈉福爾馬林縮合物、聚丙烯酸鈉、聚氧乙烯烷基醚硫酸鈉、聚氧化烯苯乙烯苯基醚硫酸鈉、聚氧化烯苯乙烯苯基醚磷酸鈉、聚氧乙烯・聚氧丙烯聚合物硫酸鈉,可為此等當中之1種單獨,亦可為2種以上的組合。In the present invention, the so-called "disintegrating and dispersing agent" means that among the above-mentioned surfactants, in addition to the above-mentioned granulation improving agent, it has the effect of improving at least one of the dispersibility and disintegration of other components of the above-mentioned active ingredients. As such a disintegrating and dispersing agent, preferably anionic surfactants can be listed, and more preferably sodium lignin sulfonate, calcium lignin sulfonate, sodium naphthalene sulfonate formalin condensate, sodium polyacrylate, polyoxyethylene alkyl ether sodium sulfate, polyoxyalkylene styrene phenyl ether sodium sulfate, polyoxyalkylene styrene phenyl ether sodium phosphate, polyoxyethylene and polyoxypropylene polymer sodium sulfate, and it can be one of them alone or a combination of two or more.

[結合劑] 在本發明,「結合劑」主要係以增加固形製劑的強度,及/或增強固體原料彼此之連接為目的來使用。作為這般的結合劑,可列舉羧基甲基纖維素鈉、羥基丙基甲基纖維素或甲基纖維素等之纖維素衍生物;聚丙烯酸鈉等之聚丙烯酸酯類;聚甲基丙烯酸甲酯等之聚甲基丙烯酸酯類;聚乙烯醇或聚乙烯吡咯烷酮等之聚乙烯衍生物;黃原膠、瓜爾膠、阿拉伯膠等之橡膠類(植物橡膠類等);澱粉;糊精;單糖類(果糖、葡萄糖、半乳糖等)或二糖類(蔗糖、麥芽糖、乳糖等)等之糖類;膠;酪蛋白;明膠;流動石蠟;大豆油或菜籽油等之植物油脂;聚乙二醇或聚丙二醇等之甘醇類,可為此等當中之1種單獨,亦可為2種以上的組合。[Binder] In the present invention, "binder" is mainly used to increase the strength of solid preparations and/or to strengthen the connection between solid raw materials. Examples of such binders include cellulose derivatives such as sodium carboxymethylcellulose, hydroxypropylmethylcellulose or methylcellulose; polyacrylates such as sodium polyacrylate; polymethacrylates such as polymethyl methacrylate; polyvinyl derivatives such as polyvinyl alcohol or polyvinyl pyrrolidone; rubbers (vegetable rubbers, etc.) such as xanthan gum, guar gum, and gum arabic; starch; dextrin; sugars such as monosaccharides (fructose, glucose, galactose, etc.) or disaccharides (sucrose, maltose, lactose, etc.); glue; casein; gelatin; liquid paraffin; vegetable oils such as soybean oil or rapeseed oil; glycols such as polyethylene glycol or polypropylene glycol. The binder may be any one of these alone or a combination of two or more thereof.

作為本發明之被覆型粒劑所含有之結合劑,上述當中,較佳為選自由流動石蠟、植物油脂、聚乙二醇及聚丙二醇所成之群組中之至少1種。又,作為本發明之擠出型粒劑所含有之結合劑,上述當中,較佳為選自由聚乙烯醇、糊精、糖類、羧基甲基纖維素鈉、羥基丙基甲基纖維素及甲基纖維素所成之群組中之至少1種。As the binder contained in the coated granules of the present invention, it is preferred that at least one of the above-mentioned binders is selected from the group consisting of fluidized paraffin, vegetable oils and fats, polyethylene glycol and polypropylene glycol. In addition, as the binder contained in the extruded granules of the present invention, it is preferred that at least one of the above-mentioned binders is selected from the group consisting of polyvinyl alcohol, dextrin, sugars, sodium carboxymethylcellulose, hydroxypropylmethylcellulose and methylcellulose.

[其他] 進而,作為本發明之固形製劑(較佳為被覆型粒劑),可進一步含有紅色色素或藍色色素等之著色劑。[Others] Furthermore, the solid preparation of the present invention (preferably coated granules) may further contain a coloring agent such as a red pigment or a blue pigment.

又,作為本發明之固形製劑,於不阻礙本發明之效果的範圍內,如有必要可進一步含有上述以外之界面活性劑、乳化劑、分散劑、崩壞劑、濕潤劑、展著劑、增黏劑、結合劑、防凍結劑、消泡劑、著色劑、防黴劑等之其他添加劑當中之至少1種。Furthermore, the solid preparation of the present invention may further contain at least one of other additives such as surfactants, emulsifiers, dispersants, disintegrants, wetting agents, spreaders, thickeners, binders, antifreeze agents, defoamers, colorants, anti-mold agents, etc. other than the above-mentioned additives, if necessary, within the range that does not hinder the effect of the present invention.

[組成] 作為本發明之固形製劑所含有之有效成分量(氟吡嘧或其鹽,含有2種以上的情況下,為該等之合計量,以下相同),由於亦為取決於使用目的或處理方法者,雖並未特別限定,但通常以氟吡嘧之自由體換算為0.1~80重量%,較佳為0.1~10重量%。[Composition] The amount of the effective ingredient contained in the solid preparation of the present invention (when two or more fluopyridine or its salts are contained, the total amount thereof, the same below) depends on the purpose of use or the method of treatment, and is not particularly limited, but is generally 0.1 to 80% by weight, preferably 0.1 to 10% by weight, based on the free form of fluopyridine.

作為本發明之固形製劑的較佳之態樣,可列舉以下者。 (1)含有氟吡嘧0.1~10重量%、核粒子(矽砂等之粒狀固體載體)20~98重量%、增量劑、界面活性劑及結合劑分別為0.2~30重量%(更佳為0.5~30重量%),合計成為100重量%之被覆型粒劑(Coated granule)、 (2)含有氟吡嘧0.1~10重量%、界面活性劑及結合劑分別為0.5~30重量%、增量劑(固體載體)20~98重量%,合計成為100重量%之擠出型粒劑(Extruded granule)、 (3)含有氟吡嘧0.1~10重量%、增量劑(固體載體)20~98重量%、造粒性改良劑0.1~2.0重量%、崩壞・分散劑0.5~5.0重量%、結合劑0.5~30重量%,合計成為100重量%之擠出型粒劑。As preferred embodiments of the solid preparation of the present invention, the following can be cited. (1) Coated granules containing 0.1-10% by weight of fluopyridine, 20-98% by weight of core particles (granular solid carrier such as silica sand), 0.2-30% by weight (preferably 0.5-30% by weight) of extender, surfactant and binder, and the total amount is 100% by weight. (2) Extruded granules containing 0.1-10% by weight of fluopyridine, 0.5-30% by weight of surfactant and binder, and 20-98% by weight of extender (solid carrier), and the total amount is 100% by weight. granule), (3) an extruded granule containing 0.1 to 10% by weight of fluopyridine, 20 to 98% by weight of a bulking agent (solid carrier), 0.1 to 2.0% by weight of a granulation improving agent, 0.5 to 5.0% by weight of a disintegrating and dispersing agent, and 0.5 to 30% by weight of a binder, the total amount of which is 100% by weight.

<固形製劑之製造方法> 本發明作為本發明之固形製劑之製造方法的一態樣,係提供一種製造方法(以下,視情況稱為「被覆型粒劑之製造方法」),其係包含: 於前述核粒子加入前述結合劑或前述結合劑及前述界面活性劑,使其濕潤,而得到濕潤核粒子之濕潤步驟、與 混合前述有效成分、前述界面活性劑及前述增量劑,或前述有效成分及前述增量劑並粉碎,而得到第1混合粉碎物之混合粉碎步驟、與 混合前述濕潤核粒子與第1混合粉碎物,而得到前述濕潤核粒子的表面以第1混合粉碎物被覆的被覆型粒劑之步驟、以及一種製造方法(以下,視情況稱為「擠出型粒劑之製造方法」),其係包含: 混合前述有效成分、前述增量劑及前述結合劑並粉碎,或混合前述有效成分、前述增量劑及前述結合劑與前述造粒性改良劑及/或前述崩壞・分散劑並粉碎,而得到第2混合粉碎物之混合粉碎步驟、與 捏合第2混合粉碎物及水,或捏合第2混合粉碎物及水與前述造粒性改良劑及/或前述崩壞・分散劑,而得到捏合物之捏合步驟、與 將前述捏合物以擠出型造粒機成型,而得到擠出型粒劑之步驟。<Method for producing solid preparation> The present invention, as one aspect of the method for producing the solid preparation of the present invention, provides a method for producing (hereinafter referred to as "method for producing coated granules" as the case may be), which comprises: adding the aforementioned binder or the aforementioned binder and the aforementioned surfactant to the aforementioned core particles to wet them, thereby obtaining a wetting step of obtaining a wet core particle, and mixing the aforementioned active ingredient, the aforementioned surfactant and the aforementioned extender, or the aforementioned active ingredient and the aforementioned extender and pulverizing them to obtain a first mixed pulverized product, and mixing the aforementioned wet core particles with the first mixed pulverized product to obtain a surface of the aforementioned wet core particles coated with the first mixed pulverized product. The invention relates to a step of preparing coated granules and a method for preparing the coated granules (hereinafter referred to as "method for preparing extruded granules"), which comprises: a mixing and pulverizing step of mixing the aforementioned active ingredient, the aforementioned extender and the aforementioned binder and pulverizing them, or mixing the aforementioned active ingredient, the aforementioned extender and the aforementioned binder with the aforementioned granulation improving agent and/or the aforementioned disintegrating/dispersing agent and pulverizing them to obtain a second mixed pulverized product, and a kneading step of kneading the second mixed pulverized product and water, or kneading the second mixed pulverized product and water with the aforementioned granulation improving agent and/or the aforementioned disintegrating/dispersing agent to obtain a kneaded product, and a step of molding the kneaded product with an extrusion granulator to obtain extruded granules.

[被覆型粒劑之製造方法] 本發明之被覆型粒劑係於前述核粒子表面,將前述有效成分及前述增量劑等以結合劑被覆而成為粒劑者。前述核粒子以容易被被覆的方式,於事前藉由前述結合劑使其濕潤(濕潤步驟)。在該濕潤步驟,可進一步加入前述界面活性劑(較佳為非離子界面活性劑)。作為這般的濕潤步驟,並未特別限制,雖可適當採用以往公知之方法或依照其之方法,但例如可列舉一邊對前述核粒子噴霧前述結合劑及如有必要之前述界面活性劑,一邊進行混合之方法。作為此時之結合劑,可藉由水或乙醇等之溶媒進行稀釋來使用。[Manufacturing method of coated granules] The coated granules of the present invention are granules formed by coating the active ingredient and the extender with a binder on the surface of the core particles. The core particles are wetted with the binder in advance in order to be easily coated (wetting step). In the wetting step, the surfactant (preferably a non-ionic surfactant) may be further added. There is no particular limitation to such a wetting step, and although a conventionally known method or a method in accordance therewith may be appropriately adopted, for example, a method of spraying the binder and, if necessary, the surfactant on the core particles while mixing them may be cited. As a binder at this time, it can be used by diluting with a solvent such as water or ethanol.

另外,被被覆之成分係於事前加入增量劑,均一進行混合並粉碎。亦即,混合前述有效成分、前述界面活性劑及前述增量劑,並粉碎(至少粉碎前述有效成分及前述增量劑),而得到第1混合粉碎物(混合粉碎步驟)。此時,在前述濕潤步驟,加入前述界面活性劑的情況下,混合前述有效成分及前述增量劑並粉碎,而得到第1混合粉碎物。作為前述界面活性劑,可分成濕潤步驟及混合粉碎步驟之兩步驟使用。作為這般的粉碎方法,並未特別限制,可適當採用以往公知之方法或依照其之方法,例如可列舉使用針磨機、錘磨機等之衝撃式粉碎機或射流粉碎機等之氣流式粉碎機之方法。In addition, the coated component is added with an extender in advance, uniformly mixed and crushed. That is, the aforementioned active ingredient, the aforementioned surfactant and the aforementioned extender are mixed and crushed (at least the aforementioned active ingredient and the aforementioned extender are crushed) to obtain the first mixed crushed product (mixing and crushing step). At this time, in the aforementioned wetting step, the aforementioned active ingredient and the aforementioned extender are mixed and crushed under the condition of adding the aforementioned surfactant to obtain the first mixed crushed product. As the aforementioned surfactant, it can be used in two steps, namely the wetting step and the mixing and crushing step. As such a crushing method, there is no particular limitation, and a previously known method or a method according to the method can be appropriately adopted, for example, a method using an impact mill such as a pin mill, a hammer mill or an air flow mill such as a jet mill can be cited.

前述濕潤步驟與混合粉碎步驟可任一者先進行,又,亦可為同時。接著,混合前述濕潤核粒子與第1混合粉碎物,而得到前述濕潤核粒子的表面以第1混合粉碎物被覆的被覆型粒劑。作為這般的混合方法,並未特別限制,可適當採用以往公知之方法或依照其之方法,例如可列舉使用混凝土攪拌機等之容器回轉型混合機;帶型攪拌機或圓錐型螺旋式混合機等之容器固定型混合機之方法。The aforementioned wetting step and the mixing and pulverizing step may be performed either first or simultaneously. Then, the aforementioned wet core particles are mixed with the first mixed and pulverized product to obtain coated granules in which the surface of the aforementioned wet core particles is coated with the first mixed and pulverized product. Such a mixing method is not particularly limited, and a conventionally known method or a method in accordance therewith may be appropriately adopted, for example, a method using a container rotary mixer such as a concrete mixer; a container fixed mixer such as a ribbon mixer or a conical screw mixer may be cited.

作為被覆型粒劑之製造方法,如有必要可進一步包含乾燥前述被覆型粒劑之乾燥步驟。作為這般的乾燥方法,並未特別限制,可適當採用以往公知之方法或依照其之方法。The method for producing the coated granules may further include a drying step of drying the coated granules, if necessary. Such a drying method is not particularly limited, and a conventionally known method or a method in accordance therewith may be appropriately adopted.

[擠出型粒劑之製造方法] 本發明之擠出型粒劑係於均一混合前述有效成分及前述增量劑等之成分並粉碎者加入水並進行捏合,將其成型而成為粒劑者。亦即,首先,混合前述有效成分、前述增量劑、前述造粒性改良劑、前述崩壞・分散劑及前述結合劑並粉碎(至少粉碎前述有效成分及前述增量劑),而得到第2混合粉碎物(混合粉碎步驟)。於該混合粉碎步驟,未加入前述造粒性改良劑及/或前述崩壞・分散劑,可於下一捏合步驟加入。作為這般的粉碎方法,可適當採用與被覆型粒劑之製造方法所列舉之粉碎方法相同的方法。又,作為此時之結合劑,可使用水或乙醇等之溶媒進行溶解而成為溶液狀來使用。[Manufacturing method of extruded granules] The extruded granules of the present invention are obtained by uniformly mixing and pulverizing the aforementioned active ingredient and the aforementioned extender, adding water and kneading, and molding them into granules. That is, first, the aforementioned active ingredient, the aforementioned extender, the aforementioned granulation improver, the aforementioned disintegrating/dispersing agent, and the aforementioned binder are mixed and pulverized (at least the aforementioned active ingredient and the aforementioned extender are pulverized) to obtain a second mixed pulverized product (mixing and pulverizing step). In the mixing and pulverizing step, the aforementioned granulation improver and/or the aforementioned disintegrating/dispersing agent are not added, but may be added in the next kneading step. As such a pulverizing method, the same method as the pulverizing method listed in the manufacturing method of the coated granules can be appropriately adopted. In this case, the binding agent may be dissolved in a solvent such as water or ethanol to be used in the form of a solution.

接著,未加入第2混合粉碎物及水,或是於前述粉碎步驟未加入前述造粒性改良劑及/或前述崩壞・分散劑的情況下,捏合(捏合)第2混合粉碎物及水與前述造粒性改良劑及/或前述崩壞・分散劑,而得到捏合物。又,作為前述造粒性改良劑及前述崩壞・分散劑,可分別獨立分成混合粉碎步驟及捏合步驟之兩步驟使用。作為這般的捏合方法,並未特別限制,可適當採用以往公知之方法或依照其之方法,例如可列舉使用帶型攪拌機、圓錐型螺旋式混合機、亨舍爾式攪拌機、雙腕型捏合機等之混合捏合機的方法。Next, without adding the second mixed pulverized product and water, or without adding the aforementioned granulation improving agent and/or the aforementioned disintegrating and dispersing agent in the aforementioned pulverizing step, the second mixed pulverized product and water are kneaded with the aforementioned granulation improving agent and/or the aforementioned disintegrating and dispersing agent to obtain a kneaded product. In addition, the aforementioned granulation improving agent and the aforementioned disintegrating and dispersing agent can be used in two steps of a mixing and pulverizing step and a kneading step, respectively. Such a kneading method is not particularly limited, and a conventionally known method or a method in accordance therewith can be appropriately adopted, for example, a method using a mixing and kneading machine such as a ribbon mixer, a conical screw mixer, a Henschel mixer, a double wrist kneading machine, etc. can be cited.

接著,將前述捏合物以擠出型造粒機成型,而得到擠出型粒劑。作為這般的成型方法,並未特別限制,可適當採用以往公知之方法或依照其之方法。例如,作為前述擠出型造粒機,可列舉藉由擠出之構造,對橫擠出型、前擠出型、堅型、滾筒擠出型,可列舉前述捏合物以螺絲或滾筒等施加壓力,從篩網或模具(Die)擠出之方法。Next, the kneaded product is molded by an extrusion granulator to obtain extruded granules. Such molding method is not particularly limited, and a conventionally known method or a method in accordance therewith can be appropriately adopted. For example, as the extrusion granulator, there can be listed a structure by extrusion, and for the horizontal extrusion type, the front extrusion type, the rigid type, and the drum extrusion type, there can be listed a method in which the kneaded product is extruded from a screen or a die by applying pressure with a screw or a drum.

前述擠出型粒劑之成型後,如有必要可進一步包含將此乾燥之乾燥步驟。作為這般的乾燥方法,並未特別限制,可適當採用以往公知之方法或依照其之方法。After the extrusion type granules are formed, if necessary, a drying step may be further included. Such a drying method is not particularly limited, and a conventionally known method or a method according to the method may be appropriately adopted.

根據本發明之另一較佳的態樣,作為組合之物,係提供本發明之固形製劑即第1組成物、與包含將其他有害生物防除劑作為有效成分而成之組成物即第2組成物的組合。此情況,第2組成物可加入適當之添加劑可成為任意之劑形。該組合之物可以藥劑套組等之形態提供。According to another preferred aspect of the present invention, a combination is provided of the solid preparation of the present invention, i.e., the first component, and a composition comprising other pest control agents as active ingredients, i.e., the second component. In this case, the second component may be added with appropriate additives to form any dosage form. The combination may be provided in the form of a drug set or the like.

根據本發明之又另一態樣,其係用以保護水稻免受水稻害蟲侵害之方法,提供一種包含將本發明之固形製劑、與其他有害生物防除劑的至少一種,同時或分別(較佳為同時適用各成分)適用在適用對象(應處理之區域)而成之方法。在此方法,「同時」適用亦包含將本發明之固形製劑與其他有害生物防除劑的至少一種施用在對象之前進行混合,適用其混合物。「分別」適用係包含不會預先混合該等,將本發明之固形製劑較其他成分優先適用、將本發明之固形製劑較其他成分更後適用。According to another aspect of the present invention, a method for protecting rice from rice pests is provided, which comprises applying the solid formulation of the present invention and at least one other pest control agent simultaneously or separately (preferably applying each component simultaneously) to the application object (area to be treated). In this method, "simultaneous" application also includes mixing the solid formulation of the present invention and at least one other pest control agent before applying them to the object, and applying the mixture. "Separately" application includes not mixing them in advance, applying the solid formulation of the present invention before other components, and applying the solid formulation of the present invention after other components.

<水稻害蟲防除方法> 本發明係提供一種水稻害蟲防除方法(以下,視情況單稱為「防除方法」),其係包含將上述之本發明之固形製劑施用在選自由前述水稻害蟲、水稻、土壤及田水面所成之群組中之至少1種之步驟。<Method for controlling rice pests> The present invention provides a method for controlling rice pests (hereinafter referred to as "control method" as the case may be), which comprises the step of applying the solid preparation of the present invention to at least one selected from the group consisting of the aforementioned rice pests, rice, soil and field water surface.

尚,在本發明,「水稻害蟲防除方法」中,除了殺蟲或衰弱前述水稻害蟲的方法之外,包含從下述之水稻排除水稻害蟲之方法、防止水稻害蟲對水稻之寄生之方法、保護水稻免受水稻害蟲侵害之方法。In addition, in the present invention, the "rice pest control method" includes, in addition to the method of killing or weakening the aforementioned rice pests, a method of eliminating rice pests from the following rice, a method of preventing rice pests from parasitizing rice, and a method of protecting rice from being attacked by rice pests.

[水稻] 作為可施用本發明之固形製劑的植物,雖並未特別限定,但較佳為水稻(Oryza sativa, Oryzaglaberrima)。水稻為禾本科水稻屬之植物,具體而言,分成粳稻種(O.sativa subsp.japonica)與秈稻種(O.sativa subsp.indica)的2種生態型,及藉由此等之雜交的中間性品種。爪哇稻米包含在粳稻種。[Rice] As a plant to which the solid preparation of the present invention can be applied, although not particularly limited, rice (Oryza sativa, Oryza glaberrima) is preferred. Rice is a plant of the genus Oryza in the family Gramineae, and is specifically divided into two ecotypes, japonica rice (O. sativa subsp. japonica) and ramie rice (O. sativa subsp. indica), and intermediate varieties obtained by hybridization of these. Java rice is included in japonica rice.

水稻係將亞洲之季風地帶為中心於非常廣泛範圍的地域,於各種氣候條件下栽培。栽培在北邊從俄羅斯與中國之國境的黑龍江河畔,南邊則渡過阿根廷。於尼泊爾、印度之山岳地帶;巴基斯坦、伊朗、埃及的砂漠地帶,已藉由灌溉栽培,而於亞洲的一部分與非洲、拉丁美洲,則未灌溉栽培。又,於亞洲之三角洲地帶,則作為浮稻栽培。Rice is cultivated in a wide range of regions, centered in the monsoon zone of Asia, under various climatic conditions. It is cultivated in the north from the banks of the Heilong River at the border between Russia and China, and in the south across Argentina. It is cultivated by irrigation in the mountainous areas of Nepal and India, and in the desert areas of Pakistan, Iran, and Egypt, but not in parts of Asia, Africa, and Latin America. Also, it is cultivated as floating rice in the delta areas of Asia.

藉由栽培方法,稻米被分成陸稻與水稻。陸稻係直接播種在田間,以田間狀態栽培。水稻雖亦有對水田直接播種之直播栽培,但於日本,一般是將幼苗移植至稻田(田種植)的栽培法。Rice is divided into land rice and paddy rice according to the cultivation method. Land rice is directly sown in the field and cultivated in the field. Although paddy rice can also be cultivated by direct seeding directly in paddy fields, in Japan, the general cultivation method is to transplant seedlings into rice fields (field planting).

通常可栽培的溫度為20℃以上,水稻係以湛水條件(水田)栽培。生育最低溫度為10~12℃,開花結實必須為23℃。反之,提高至35℃以上時,產生高溫障礙。The normal cultivation temperature is above 20℃. Rice is cultivated in waterlogged fields. The minimum growth temperature is 10~12℃, and the temperature for flowering and fruiting must be 23℃. On the contrary, when it is raised to above 35℃, high temperature barriers will occur.

原本為水生植物之水稻係水量要求大的作物之一,不灌水,土壤水分於表面層為水分10%以下,於下層土為12%以下時,則發生乾旱損害。惟,亦可於鹽類集積土壤、鹼或酸性土壤栽培。Rice, originally an aquatic plant, is one of the crops that requires a lot of water. Without irrigation, when the soil moisture is less than 10% at the surface layer and less than 12% at the subsoil layer, drought damage will occur. However, it can also be cultivated in salt-accumulating soils, alkaline or acidic soils.

本發明之固形製劑在米栽培,特佳為在水稻栽培,可施用在從播種(較佳為從移植後)至收穫為止的任意期間。例如,移植苗2~5週後,藉由將本發明之固形製劑對移植後之稻田(水稻稻田)的水面(田水面)施用,可一次防除不同時期所發生之前述水稻害蟲。尚,前述田水面中亦包含在瓦氏盆等之水耕栽培器材的水面。本發明之固形製劑除了前述田水面之外,可施用在包含移植前之栽培載體的土壤,或栽培前述陸稻等之土壤等,亦可直接施用在前述水稻害蟲或水稻(較佳為莖葉部)。此等當中,作為施用本發明之固形製劑之對象,較佳為前述土壤(移植前之栽培土壤及栽培載體、栽培陸稻等之土壤等)及前述田水面當中的至少1種。The solid preparation of the present invention can be applied to rice cultivation, particularly preferably paddy rice cultivation, at any time from sowing (preferably after transplanting) to harvesting. For example, 2 to 5 weeks after transplanting the seedlings, by applying the solid preparation of the present invention to the water surface (field water surface) of the transplanted rice field (paddy rice field), the aforementioned rice pests occurring at different times can be prevented at one time. In addition, the aforementioned field water surface also includes the water surface of hydroponic cultivation equipment such as a Vashvili pot. In addition to the aforementioned field water surface, the solid preparation of the present invention can be applied to the soil including the cultivation carrier before transplanting, or the soil for cultivating the aforementioned land rice, etc., and can also be directly applied to the aforementioned rice pests or rice (preferably the stem and leaf parts). Among these, the target to which the solid preparation of the present invention is applied is preferably at least one of the aforementioned soil (cultivation soil and cultivation carrier before transplantation, soil for cultivating rice, etc.) and the aforementioned field water surface.

又,在本發明之防除方法,可將本發明之固形製劑以成為有效量的方式,將前述固形製劑直接或是稀釋來施用。In the control method of the present invention, the solid preparation of the present invention can be applied directly or in a diluted form in an effective amount.

根據本發明之其他態樣,提供一種保護水稻免受水稻害蟲侵害之方法,其係包含將本發明之固形製劑的有效量,施用在選自由前述水稻害蟲、前述水稻(較佳為莖葉部)、前述土壤及前述田水面所成之群組中之至少1種之步驟。According to another aspect of the present invention, a method for protecting rice from rice pests is provided, comprising the step of applying an effective amount of the solid preparation of the present invention to at least one selected from the group consisting of the rice pests, the rice (preferably the stems and leaves), the soil, and the field water surface.

又,根據本發明之其他態樣,提供一種用以保護水稻免受水稻害蟲侵害之本發明之固形製劑的使用。Furthermore, according to another aspect of the present invention, a use of the solid preparation of the present invention for protecting rice from rice pests is provided.

作為將本發明之固形製劑施用在對象之手法,可列舉散布處理、田面水處理、土壤處理(散布、混和、灌注等)等,較佳可列舉田面水處理及土壤處理。As a method of applying the solid preparation of the present invention to an object, there can be listed spreading treatment, field water treatment, soil treatment (spreading, mixing, pouring, etc.), etc., preferably, field water treatment and soil treatment can be listed.

作為將本發明之固形製劑使用在田面水處理及土壤處理之方法,雖可直接將固形製劑散布在田水面或土壤表面,但於與肥料或砂混和後,可將任意的量散布在耕地(稻田)。作為藉由田面水處理及土壤處理施用時的處理量(亦即有效量),期望以本發明之固形製劑中之有效成分量(以氟吡嘧或其鹽之自由體換算的量,含有此等之2種以上的情況下,為該等之合計量,以下相同),耕地每10公畝為0.1g~10kg,較佳為1g~1kg。As a method of using the solid preparation of the present invention for field water treatment and soil treatment, the solid preparation can be directly spread on the field water surface or soil surface, but after mixing with fertilizer or sand, any amount can be spread on cultivated land (rice field). As the treatment amount (i.e., effective amount) when applied by field water treatment and soil treatment, it is expected that the amount of the effective ingredient in the solid preparation of the present invention (the amount converted as the free body of fluopyridine or its salt, when containing two or more of these, the total amount of these, the same below) is 0.1g~10kg per 10 acres of cultivated land, preferably 1g~1kg.

又,作為藉由本發明之固形製劑之土壤處理方法,雖並未特別限定,但較佳可列舉將本發明之固形製劑直接施用在土壤中或土壤表面上之方法。更佳之土壤處理方法為散布、帶、溝及種植穴適用法。Furthermore, as a soil treatment method using the solid preparation of the present invention, although not particularly limited, a method of directly applying the solid preparation of the present invention to the soil or on the soil surface can be preferably cited. More preferred soil treatment methods are scattering, belt, trench and planting hole application methods.

作為其他施用方法,可列舉對在如薄膜水耕(NFT)或輸液水耕(DFT)等之水耕栽培、如岩棉耕等之固體培養基耕栽培之養液栽培系統的養液之本發明之固形製劑的施用,或對包含蛭石之人工培土及包含育苗用人工墊之固體培養基的直接施用。又,從長期間持續防除活性的觀點來看,雖不佳,但本發明之固形製劑可藉由分散在水中,或是將經乳化或溶解之溶液灌注在土壤來施用。 [實施例]As other application methods, the solid preparation of the present invention can be applied to the nutrient solution of a hydroponic cultivation system such as thin-film hydroponics (NFT) or distilled-water hydroponics (DFT), or solid culture medium cultivation such as rock wool cultivation, or directly applied to artificial soil containing vermiculite and solid culture medium containing artificial mats for seedling cultivation. In addition, although it is not good from the perspective of long-term sustained control activity, the solid preparation of the present invention can be applied by dispersing in water or pouring the emulsified or dissolved solution into the soil. [Example]

以下,雖列舉實施例具體說明本發明,但本發明並非被限定於此等之實施例。尚,各製劑例之原料全部使用市售品。又,在各製劑例,僅粒徑為63μm以上之固體載體(核粒子)記為粒徑。Although the present invention is specifically described below by way of examples, the present invention is not limited to these examples. In addition, all raw materials in each formulation example are commercially available. In each formulation example, only solid carriers (core particles) with a particle size of 63 μm or more are recorded as particle sizes.

(製劑例) 製劑例1 [擠出型粒劑] 氟吡嘧                      2重量% 木質素磺酸鈉                 3重量% 月桂基硫酸鈉                0.5重量% 二氧化矽                    2重量% 聚乙烯醇                   1.5重量% 黏土                       91重量% 將上述成分均一混合粉碎,加入水充分捏合後,將此捏合物通過擠出型造粒機,進行造粒乾燥而得到粒劑。(Preparation Example) Preparation Example 1 [Extrusion Granules] Fluoropyrazine                      2 wt% Sodium lignin sulfonate                    3 wt% Sodium lauryl sulfate                    0.5 wt% Silicon dioxide                    2 wt% Polyvinyl alcohol                       1.5 wt% Clay                      91 wt% The above ingredients are uniformly mixed and pulverized, water is added and kneaded thoroughly, and the kneaded mixture is passed through an extrusion granulator, granulated and dried to obtain granules.

製劑例2 [擠出型粒劑] 氟吡嘧                    2重量% 木質素磺酸鈣               3重量% 烷基苯磺酸鈉              0.5重量% 二氧化矽                   2重量% 聚乙烯醇                   1重量% 黏土                    91.5重量% 將上述成分均一混合粉碎,加入水充分捏合後,將此捏合物通過擠出型造粒機,進行造粒乾燥而得到粒劑。Preparation Example 2 [Extrusion Granules] Fluoropyrazine                  2 wt% Calcium lignin sulfonate                  3 wt% Sodium alkylbenzene sulfonate                  0.5 wt% Silicon dioxide                       2 wt% Polyvinyl alcohol                  1 wt% Clay                      91.5 wt% The above ingredients are uniformly mixed and pulverized, water is added and kneaded thoroughly, and the kneaded mixture is passed through an extrusion granulator, granulated and dried to obtain granules.

製劑例3 [擠出型粒劑] 氟吡嘧                    2重量% 聚丙烯酸鈉                 2重量% 二烷基磺基琥珀酸鈉         0.3重量% 羧基甲基纖維素鈉           1.5重量% 碳酸鈣                  94.2重量% 排除聚丙烯酸鈉,並將上述之成分均一混合粉碎,對其加入聚丙烯酸鈉與水並充分捏合後,將此捏合物通過擠出型造粒機,進行造粒乾燥而得到粒劑。Preparation Example 3 [Extrusion Granules] Fluoropyrazine                    2 wt% Sodium polyacrylate                2 wt% Sodium dialkyl sulfosuccinate            0.3 wt% Sodium carboxymethylcellulose              1.5 wt% Calcium carbonate                  94.2 wt% Excluding sodium polyacrylate, the above ingredients are uniformly mixed and pulverized, sodium polyacrylate and water are added thereto and kneaded thoroughly, and the kneaded product is passed through an extrusion granulator, granulated and dried to obtain granules.

製劑例4 [擠出型粒劑] 氟吡嘧                    2重量% 木質素磺酸鈉               3重量% 烷基苯磺酸鈉              0.3重量% 糊精                     5重量% 高嶺土                   10重量% 黏土                   79.7重量% 將上述成分均一混合粉碎,加入水充分捏合後,將此捏合物通過擠出型造粒機,進行造粒乾燥而得到粒劑。Preparation Example 4 [Extrusion Granules] Fluoropyrazine                     2 wt% Sodium lignin sulfonate               3 wt% Sodium alkylbenzene sulfonate              0.3 wt% Dextrin                    5 wt% Kaolin                        10 wt% Clay                      79.7 wt% The above ingredients are uniformly mixed and pulverized, water is added and kneaded thoroughly, and the kneaded mixture is passed through an extrusion granulator, granulated and dried to obtain granules.

製劑例5 [擠出型粒劑] 氟吡嘧                    2重量% 萘磺酸鈉福爾馬林縮合物       3重量% 月桂基硫酸鈉              0.3重量% 羧基甲基纖維素鈉           1.5重量% 滑石                     30重量% 碳酸鈣                  63.2重量% 將上述成分均一混合粉碎,加入水充分捏合後,將此捏合物通過擠出型造粒機,進行造粒乾燥而得到粒劑。Preparation Example 5 [Extrusion Granules] Fluoropyrazine                    2 wt% Sodium naphthalenesulfonate formalin condensate       3 wt% Sodium lauryl sulfate              0.3 wt% Sodium carboxymethylcellulose           1.5 wt% Talc                                 30 wt% Calcium carbonate                  63.2 wt% The above ingredients are uniformly mixed and pulverized, water is added and kneaded thoroughly, and the kneaded mixture is passed through an extrusion granulator, granulated and dried to obtain granules.

製劑例6 [被覆型粒劑] 氟吡嘧                    2重量% 矽砂(粒狀:粒徑0.3~1.4mm)  95.55重量% 月桂基硫酸鈉              0.1重量% 二氧化矽                 0.5重量% 流動石蠟                 1.15重量% 紅色色素                 0.2重量% 高嶺土                   0.5重量% 將上述之矽砂及流動石蠟以外的成分均一混合粉碎,而得到粉碎物。於矽砂加入流動石蠟並使其均一濕潤後,加入前述粉碎物,進行均一混合,並於前述核粒子被覆前述粉碎物,而得到粒劑。Preparation Example 6 [Coated Granules] Fluoropyrazine                            2 wt% Silica sand (granular: particle size 0.3~1.4 mm)  95.55 wt% Sodium lauryl sulfate                  0.1 wt% Silicon dioxide                     0.5 wt% Liquid wax                     1.15 wt% Red pigment                 0.2 wt% Kaolin                       0.5 wt% The above-mentioned silica sand and ingredients other than the liquid wax are uniformly mixed and pulverized to obtain a pulverized product. After the liquid wax is added to the silica sand and uniformly wetted, the pulverized product is added and uniformly mixed, and the pulverized product is coated on the core particles to obtain granules.

製劑例7 [被覆型粒劑] 氟吡嘧                    2重量% 矽砂(粒狀:粒徑0.3~1.4mm)  95.85重量% 月桂基硫酸鈉              0.1重量% 二氧化矽                 0.75重量% 聚丙二醇                  1.1重量% 紅色色素                  0.2重量% 將上述之矽砂及聚丙二醇以外的成分均一混合粉碎,而得到粉碎物。於矽砂加入聚丙二醇並使其均一濕潤後,加入前述粉碎物,進行均一混合,並於前述核粒子被覆前述粉碎物,而得到粒劑。Preparation Example 7 [Coated Granules] Fluoropyrazine                  2 wt% Silica sand (granular: particle size 0.3~1.4 mm)  95.85 wt% Sodium lauryl sulfate                  0.1 wt% Silicon dioxide                   0.75 wt% Polypropylene glycol                   1.1 wt% Red pigment                        0.2 wt% The above-mentioned silica sand and components other than polypropylene glycol are uniformly mixed and pulverized to obtain a pulverized product. After adding polypropylene glycol to the silica sand and making it uniformly wet, the above-mentioned pulverized product is added and uniformly mixed, and the above-mentioned pulverized product is coated on the above-mentioned core particles to obtain granules.

製劑例8 [被覆型粒劑] 氟吡嘧                    2重量% 烷基苯磺酸鈉              0.1重量% 高嶺土                    1重量% 紅色色素                 0.2重量% 聚乙二醇                 1.15重量% 粒狀碳酸鈣 (粒徑0.42~0.85mm)         95.55重量% 將上述之粒狀碳酸鈣及聚乙二醇以外的成分均一混合粉碎,而得到粉碎物。於粒狀碳酸鈣加入聚乙二醇並使其均一濕潤後,加入粉碎物,進行均一混合,並於前述核粒子被覆前述粉碎物,而得到粒劑。Preparation Example 8 [Coated Granules] Fluoropyrazine                            2 wt% Sodium alkylbenzenesulfonate                     0.1 wt% Kaolin                           1 wt% Red pigment                       0.2 wt% Polyethylene glycol                         1.15 wt% Granular calcium carbonate (particle size 0.42~0.85 mm)         95.55 wt% The granular calcium carbonate and the components other than polyethylene glycol are uniformly mixed and pulverized to obtain a pulverized product. After polyethylene glycol is added to the granular calcium carbonate to uniformly wet it, the pulverized product is added and uniformly mixed, and the pulverized product is coated on the core particles to obtain granules.

製劑例9 [被覆型粒劑] 氟吡嘧                     2重量% 烷基苯磺酸鈉               0.1重量% 二氧化矽                   0.5重量% 高嶺土                    0.5重量% 藍色色素                  0.2重量% 聚丙二醇                  1.15重量% 矽砂(粒狀:粒徑0.25~1.0mm)  95.55重量% 將上述矽砂及聚丙二醇以外的成分均一混合粉碎,而得到粉碎物。於矽砂加入聚丙二醇並使其均一濕潤後,加入粉碎物,進行均一混合,並於前述核粒子被覆前述粉碎物,而得到粒劑。Preparation Example 9 [Coated Granules] Fluoropyrazine                     2 wt% Sodium alkylbenzenesulfonate               0.1 wt% Silicon dioxide                   0.5 wt% Kaolin                   0.5 wt% Blue pigment                  0.2 wt% Polypropylene glycol                    1.15 wt% Silica sand (granular: particle size 0.25~1.0 mm)  95.55 wt% The above-mentioned silica sand and components other than polypropylene glycol are uniformly mixed and pulverized to obtain a pulverized product. After adding polypropylene glycol to the silica sand and uniformly moistening it, the pulverized product is added and uniformly mixed, and the pulverized product is coated on the above-mentioned core particles to obtain granules.

製劑例10 [被覆型粒劑] 氟吡嘧                     2重量% 高嶺土                    1.5重量% 藍色色素                  0.2重量% 二烷基磺基琥珀酸鈉          0.1重量% 聚氧化烯山梨糖醇脂肪酸酯     0.2重量% 大豆油                     1重量% 矽砂(粒狀:粒徑0.25~1.0mm)    95重量% 將氟吡嘧、高嶺土、藍色色素均一混合粉碎,而得到粉碎物。於矽砂加入預先混合之二烷基磺基琥珀酸鈉、聚氧化烯山梨糖醇脂肪酸酯及大豆油的混合物並使其均一濕潤後,加入粉碎物,進行均一混合,並於前述核粒子被覆前述粉碎物,而得到粒劑。Preparation Example 10 [Coated Granules] Fluopyrazine                          2 wt% Kaolin                    1.5 wt% Blue Pigment                  0.2 wt% Sodium Dialkyl Sulfosuccinate          0.1 wt% Polyoxyalkylene Sorbitol Fatty Acid Ester     0.2 wt% Soybean Oil                     1 wt% Silica Sand (granular: particle size 0.25~1.0 mm)    95 wt% Fluopyrazine, kaolin, and blue pigment are uniformly mixed and pulverized to obtain a pulverized product. After adding a pre-mixed mixture of sodium dialkyl sulfosuccinate, polyoxyalkylene sorbitol fatty acid ester, and soybean oil to silica sand and uniformly moistening it, the pulverized product is added and uniformly mixed, and the pulverized product is coated on the core particles to obtain granules.

比較製劑例1 [流動劑] 氟吡嘧                        10重量% 木質素磺酸鈉                   2.5重量% 二烷基磺基琥珀酸鈉               0.2重量% 丙二醇                        10重量% 黃原膠                         0.3重量% 聚矽氧系消泡劑                   0.5重量% 防黴劑 (有機氮硫系複合物、有機溴系化合物)  0.03重量% 水                           76.47重量% 於水加入氟吡嘧、木質素磺酸鈉、二烷基磺基琥珀酸鈉、丙二醇及聚矽氧系消泡劑並混合後,進行藉由珠磨機之濕式粉碎,而得到漿料(A液)。其次,混合黃原膠、防黴劑及水並溶解,而得到水溶液(B液)。混合經調製之A液780重量份與B液230重量份,而得到流動劑。Comparative Preparation Example 1 [Flowing Agent] Fluoropyrazine                      10 wt% Sodium lignin sulfonate                   2.5 wt% Sodium dialkyl sulfosuccinate               0.2 wt% Propylene glycol                        10 wt% Xanthan gum                        0.3 wt% Polysilicone defoaming agent                   0.5 wt% Anti-mold agent (Organic nitrogen-sulfur complex, organic bromine compound)  0.03 wt% Water                    76.47% by weight After adding fluopyridine, sodium lignin sulfonate, sodium dialkyl sulfosuccinate, propylene glycol and polysilicone defoamer to water and mixing, wet grinding is performed by a bead mill to obtain a slurry (liquid A). Next, xanthan gum, anti-mold agent and water are mixed and dissolved to obtain an aqueous solution (liquid B). 780 parts by weight of the prepared liquid A and 230 parts by weight of liquid B are mixed to obtain a fluidizing agent.

比較製劑例2 [顆粒水合劑] 氟吡嘧                    20重量% 二烷基磺基琥珀酸鈉           1重量% 木質素磺酸鈉                7重量% 二氧化矽                   1重量% 黏土                      71重量% 將上述成分均一混合粉碎,加入水充分捏合後,將此捏合物通過擠出型造粒機,進行造粒乾燥而得到顆粒水合劑。Comparative Preparation Example 2 [Granular Hydration Agent] Fluoropyrazine                    20 wt% Sodium dialkyl sulfosuccinate               1 wt% Sodium lignin sulfonate                    7 wt% Silicon dioxide                                   1 wt% Clay       ...

(試驗例1 對於二化螟類及飛蝨類之田間試驗) 對田間種植25日後之水稻田間,以原體量(有效成分量、在氟吡嘧劑,為氟吡嘧量,以下相同)成為指定量的方式,將製劑例1之粒劑(擠出型粒劑)藉由水面施用進行處理(田面水處理)。針對對照製劑,同樣於田間種植25日後,將二化螟類防除用製劑之培丹4%粒劑以原體量(培丹量)成為指定量的方式,藉由水面施用進行處理,進而從該處理3週(21日)後,將飛蝨類防除用製劑之布酚淨25%流動劑以原體量(布酚淨量)成為指定量的方式,藉由莖葉散布進行處理。針對無處理區,任何製劑皆未施用。(Test Example 1 Field test on rice stem borers and flies) Twenty-five days after field planting, the granules (extrudable granules) of Preparation Example 1 were applied to the rice field by surface water application (field surface water treatment) in a manner that the original amount (active ingredient amount, in fluopyridine, fluopyridine amount, the same below) became a specified amount. For the control preparation, 25 days after planting in the field, the preparation for controlling striped stem borers, Pedan 4% granules, were applied to the water surface in the amount of the original body (Pedan amount) to the specified amount. Three weeks after the treatment (21 days), the preparation for controlling flying flies, Bufenjing 25% liquid, was applied to the leaves in the amount of the original body (bufenjing amount) to the specified amount. For the untreated area, no preparation was applied.

於經製劑處理之日(田間種植25日後)的14、21、28、35日後,集計在各區隨機選出之20株的分蘗數,及因二化螟類(主要為三化螟)導致之損害莖數。依照以下之式,算出損害莖率。 損害莖率(%)=(各處理日之損害莖數/20株之總分蘗數)×100 將結果示於下述之表1。又,同於14、21、28、35、42日後,集計寄生在各區隨機選出之20株的各株之飛蝨類(褐飛蝨及白背飛蝨的合計)的固體數(成蟲及幼蟲數的合計),作為飛蝨類之寄生蟲數。將結果示於下述之表2。14, 21, 28, and 35 days after the treatment (25 days after field planting), the number of tillers of 20 plants randomly selected in each area and the number of stems damaged by Chilo suppressalis (mainly Striped Stem Borer) were counted. The stem damage rate was calculated according to the following formula. Stem damage rate (%) = (number of damaged stems on each treatment day/total number of tillers of 20 plants) × 100 The results are shown in Table 1 below. In addition, after 14, 21, 28, 35, and 42 days, the solid counts (total number of adults and larvae) of flies (the total number of brown flies and white-backed flies) parasitizing each of 20 randomly selected plants in each area were counted as the number of fly parasites. The results are shown in Table 2 below.

試驗的結果,如表1~2所示,於本發明之固形製劑即氟吡嘧粒劑,在100g/ha的處理量,確認不僅顯示相較對於二化螟類之對照製劑更高之損害抑制效果,亦顯著抑制飛蝨類之寄生蟲數。另一方面,在對照製劑之培丹粒劑及布酚淨流動劑之處理區(體系防除處理區),因二化螟類導致之損害莖率雖較無處理區抑制在更低,但為飛蝨類之寄生蟲數的減少率較少,對於飛蝨類之密度抑制效果較低的結果。如此,確認本發明之氟吡嘧粒劑僅以1次的處理即具有長期之持續性,相較對照製劑之二化螟類防除用製劑及飛蝨類防除用製劑之體系處理,對於二化螟類及飛蝨類顯示更高之防除活性。The results of the test, as shown in Tables 1 and 2, show that the solid preparation of the present invention, i.e., fluopyramide granules, at a treatment amount of 100 g/ha, not only showed a higher damage inhibition effect on the striped stem borer than the control preparation, but also significantly inhibited the number of parasites of flying flies. On the other hand, in the treatment area (systemic control treatment area) of the control preparation of petan granules and fenfen clean flowable agent, the rate of stem damage caused by striped stem borer was lower than that of the untreated area, but the reduction rate of the number of parasites of flying flies was lower, resulting in a lower density inhibition effect on flying flies. Thus, it was confirmed that the fluopyramide granules of the present invention had long-term persistence after only one treatment, and showed higher control activity against striped stem borers and flies compared to systemic treatment of control formulations of the striped stem borers and flies.

又,藉由比較從各處理區所收穫之稻米的重量,評估對各製劑之稻米的收量的影響。將結果示於下述之表3。In addition, the effect of each preparation on the rice yield was evaluated by comparing the weight of rice harvested from each treatment area. The results are shown in Table 3 below.

如表3所示,於氟吡嘧粒劑之處理區,確認相較對照製劑之體系防除處理區更高,對於無處理區提昇12%之收量的效果。藉由以上之結果,根據本發明之固形製劑(擠出型粒劑),確認藉由1次的處理,不僅減低化水稻害蟲防除作業的勞力,相較對照製劑亦顯示更為優異之增收效果。As shown in Table 3, in the treatment area of fluopyramide granules, it was confirmed that the systemic control treatment area of the control preparation was higher, and the yield of the untreated area was increased by 12%. Through the above results, according to the solid preparation (extruded granules) of the present invention, it was confirmed that through one treatment, not only the labor of rice pest control operation was reduced, but also a more excellent yield-increasing effect was shown compared with the control preparation.

(試驗例2 對於褐飛蝨之室內試驗) 將播種3週後之水稻移植至瓦氏盆(1/5000a),於移植3日後,以原體量成為指定量的方式,將製造例1之粒劑(擠出型粒劑)或是製造例6之粒劑(被覆型粒劑),或氟吡嘧原體藉由水面施用進行處理(田面水處理)。針對無處理區,任何製劑及藥劑皆未施用。於經製劑或藥劑處理之日(移植3日後)之3、29、42日後,對各盆放飼褐飛蝨之二齡幼蟲,於該放飼6日後或是7日後觀察幼蟲生死,依照以下之式算出修正死蟲率。 修正死蟲率(%)=[{(無處理區之生存蟲數/放飼蟲數)-(處理區之生存蟲數/放飼蟲數)}/(無處理區之生存蟲數/放飼蟲數)]×100 試驗係以2連制進行。將結果示於下述之表4。(Test Example 2 Indoor test on brown fly) Rice 3 weeks after sowing was transplanted into a Warburg pot (1/5000a). 3 days after transplantation, the granules of Preparation Example 1 (extrusion type granules) or the granules of Preparation Example 6 (coated type granules) or Fluopyridine were applied to the water surface to treat the original body amount (field surface water treatment). For the untreated area, no preparations or drugs were applied. 3, 29, and 42 days after the day of preparation or drug treatment (3 days after transplantation), the second-instar larvae of brown fly were released into each pot, and the life and death of the larvae were observed 6 or 7 days after the release, and the corrected mortality rate was calculated according to the following formula. Corrected mortality rate (%) = [{(Number of surviving insects in the untreated area/Number of released insects)-(Number of surviving insects in the treated area/Number of released insects)}/(Number of surviving insects in the untreated area/Number of released insects)] × 100 The test was conducted in two consecutive runs. The results are shown in Table 4 below.

試驗的結果,如表4所示,於本發明之固形製劑即氟吡嘧之被覆型粒劑及擠出型粒劑,於各處理之29、42日後,即使放飼水稻害蟲,亦顯示較氟吡嘧原體更高之修正死蟲率。因此,確認藉由成為此等之粒劑,相較原體,長期的持續性更為優異。The test results are shown in Table 4. The solid preparation of the present invention, i.e., the coated granules and extruded granules of fluopyrazole, showed a higher corrected mortality rate than fluopyrazole even when rice pests were released 29 and 42 days after each treatment. Therefore, it was confirmed that by becoming such granules, the long-term sustainability was superior to that of fluopyrazole.

(試驗例3 對於二化螟類之田間試驗) 將製劑例1之粒劑(擠出型粒劑)與適當量之砂混和後,對移植25日後之水稻田間,以原體量成為指定量的方式,藉由均一水面施用,進行處理(田面水處理)。又,於同日,將比較製劑例1之流動劑以成為40L/10a的處理水量的方式以水進行稀釋,並以原體量成為指定量的方式,藉由噴霧器對莖葉部進行噴霧處理。針對無處理區,任何製劑皆未施用。於製劑處理時,雖未觀察到因二化螟類(優勢種三化螟)導致之對莖部的損害,但於處理之28日後及42日後,藉由目視計數各株之莖數及因二化螟類(優勢種三化螟)導致之芯枯莖數。進行25m2 之區每30株的調査,依然以下之式,算出損害莖率。 損害莖率(%)={(每30株之芯枯莖數)/(每30株之總莖數)}×100 將結果示於下述之表5。(Test Example 3 Field test on rice stem borer) The granules of Preparation Example 1 (extrusion type granules) were mixed with an appropriate amount of sand, and then treated by uniformly applying the original volume to the rice field 25 days after transplantation (field surface water treatment). On the same day, the flowable agent of Comparative Preparation Example 1 was diluted with water to a treatment water volume of 40L/10a, and then sprayed on the stems and leaves with a sprayer in such a way that the original volume became the specified amount. No preparation was applied to the untreated area. Although no stem damage caused by Chilo suppressalis (dominant species Yellow stem borer) was observed during the preparation treatment, the number of stems of each plant and the number of stem core blight caused by Chilo suppressalis (dominant species Yellow stem borer) were visually counted 28 days and 42 days after the treatment. A survey was conducted for every 30 plants in a 25m2 area, and the stem damage rate was calculated using the following formula. Stem damage rate (%) = {(number of stem core blight per 30 plants)/(total number of stems per 30 plants)}×100 The results are shown in Table 5 below.

試驗的結果,如表5所示,本發明之擠出型粒劑對於二化螟類(優勢種三化螟),相較流動劑經過長期間,亦顯示高防除活性。The test results are shown in Table 5. The extruded granules of the present invention showed high control activity against Chilo suppressalis (dominant species) over a long period of time compared to the mobile formulation.

(試驗例4 對於褐飛蝨之田間試驗) 將製劑例1之粒劑(擠出型粒劑)與適當量之砂混和後,對移植25日後之水稻田間,以原體量成為指定量的方式,藉由均一水面施用,進行處理(田面水處理)。又,於同日,將比較製劑例1之流動劑以成為40L/10a的處理水量的方式以水進行稀釋,並以原體量成為指定量的方式,藉由噴霧器對莖葉部進行噴霧處理。針對無處理區,任何製劑皆未施用。於製劑處理時,雖未觀察到因飛蝨類對稻的寄生,但於處理之31、49、56日後,藉由目視計數寄生在各株頭之褐飛蝨成蟲及幼蟲數。將進行25m2 之區每30株的調査的結果,以每株之寄生蟲數(成蟲及幼蟲的合計)示於下述之表6。(Test Example 4 Field test against brown fly) The granules of Preparation Example 1 (extrusion type granules) were mixed with an appropriate amount of sand, and then applied uniformly to the rice field 25 days after transplantation in such a manner that the original volume became a specified volume (field surface water treatment). On the same day, the flowable agent of Comparative Preparation Example 1 was diluted with water in such a manner that the treatment water volume became 40L/10a, and then sprayed on the stems and leaves in such a manner that the original volume became a specified volume by a sprayer. No preparation was applied to the untreated area. Although no parasitism of rice by flies was observed during the preparation treatment, the number of adults and larvae of brown flies parasitizing on each plant head was visually counted 31, 49, and 56 days after treatment. The results of the survey of 30 plants in a 25 m2 plot are shown in Table 6 below as the number of parasites per plant (total of adults and larvae).

試驗的結果,如表6所示,本發明之擠出型粒劑對於褐飛蝨,相較流動劑經過長期間,亦顯示高防除活性。The test results are shown in Table 6. The extruded granules of the present invention showed high control activity against brown plant flies even after a long period of time compared to the liquid formulation.

(參考試驗例 顆粒水合劑與流動劑之對比試驗) 將比較製劑例1之流動劑或比較製劑例2之顆粒水合劑以成為150L/10a的處理水量的方式以水進行稀釋,並以原體量成為指定量的方式,藉由噴霧器對移植48日後之水稻莖葉部進行噴霧處理。針對無處理區,任何製劑皆未施用。於各處理前及處理之4、7、19、33日後,對A4尺寸之黏著板擦落寄生在各株頭之飛蝨類,藉由目視計數灰飛蝨成蟲及幼蟲數。將進行24m2 之區每30株的調査的結果以每株之寄生蟲數(成蟲及幼蟲的合計)示於下述之表7。(Reference Test Example Comparative Test of Granular Hydrator and Flowing Agent) The flowing agent of Comparative Preparation Example 1 or the granular hydrate of Comparative Preparation Example 2 was diluted with water in a treatment water volume of 150L/10a, and the original volume was made into a specified amount, and then sprayed on the rice stems and leaves 48 days after transplantation by a sprayer. For the untreated area, no preparation was applied. Before each treatment and 4, 7, 19, and 33 days after the treatment, the fly species parasitizing on each plant head were wiped off on an A4-sized sticky board, and the number of gray fly adults and larvae was counted visually. The results of the survey of 30 plants in a 24 m2 plot are shown in Table 7 below as the number of parasites per plant (total of adults and larvae).

試驗的結果,如表7所示,於流動劑與顆粒水合劑,對於灰飛蝨,顯示同程度之防除活性。因此,藉由上述之結果,本發明之擠出型粒劑與顆粒水合劑相比較,可說經過長期間,亦顯示高防除活性。 [產業上之可利用性]The test results, as shown in Table 7, show that the flowable agent and the granular hydrate agent show the same degree of control activity against gray fly flies. Therefore, based on the above results, it can be said that the extruded granules of the present invention show high control activity over a long period of time compared with the granular hydrate. [Industrial Applicability]

如以上說明,根據本發明,變成可提供一種用以防除有害生物、尤其是水稻害蟲之防除活性的持續期間長之嶄新的固形製劑,及使用其之水稻害蟲防除方法、以及前述水稻害蟲防除用固形製劑之製造方法。例如,於本發明之水稻害蟲防除用固形製劑,於水稻之移植2~5週後藉由進行田面水處理,使得於以往一次之藥劑處理無法充分防除之飛蝨類及二化螟類的防除變成可一次防除,亦有效減低施加在米栽培農家之藥劑防除之勞力及提昇收穫率。As described above, according to the present invention, a novel solid formulation for controlling harmful organisms, especially rice pests, with a long duration of control activity, a rice pest control method using the same, and a method for producing the solid formulation for controlling rice pests can be provided. For example, the solid formulation for controlling rice pests of the present invention can be used to treat field water 2 to 5 weeks after rice transplantation, so that flies and rice stem borers that could not be fully controlled by a single treatment of pesticides can be controlled at one time, which can effectively reduce the labor of pesticide control applied to rice farmers and improve the yield rate.

Claims (17)

一種水稻害蟲防除用固形製劑,其係含有選自由下述式(1)表示之氟吡嘧(flupyrimin)及其鹽所成之群組中之至少1種的有效成分、固體載體、界面活性劑、以及結合劑,並為被覆型粒劑或擠出型粒劑
Figure 109120819-A0305-02-0050-1
A solid preparation for controlling rice pests, comprising at least one active ingredient selected from the group consisting of flupyrimin and its salts represented by the following formula (1), a solid carrier, a surfactant, and a binder, and is a coated granule or an extruded granule.
Figure 109120819-A0305-02-0050-1
如請求項1之水稻害蟲防除用固形製劑,其係被覆型粒劑,前述固體載體包含核粒子及增量劑。 For example, the solid preparation for controlling rice pests in claim 1 is a coated granule, and the solid carrier comprises core particles and an extender. 如請求項2之水稻害蟲防除用固形製劑,其中,前述核粒子的粒徑為63μm~6mm。 For example, in the solid preparation for controlling rice pests as in claim 2, the particle size of the core particles is 63μm~6mm. 如請求項2或3之水稻害蟲防除用固形製劑,其中,前述核粒子係選自由矽砂、粒狀碳酸鈣、矽藻土粒、粒狀黏土及浮石所成之群組中之至少1種。 For example, in the solid preparation for controlling rice pests as claimed in claim 2 or 3, the core particles are at least one selected from the group consisting of silica sand, granular calcium carbonate, diatomaceous earth particles, granular clay and pumice. 如請求項2或3之水稻害蟲防除用固形製劑,其中,前述增量劑係選自由黏土、碳酸鈣、高嶺土及二氧化矽所成之群組中之至少1種。 For example, the solid preparation for controlling rice pests as claimed in claim 2 or 3, wherein the aforementioned extender is at least one selected from the group consisting of clay, calcium carbonate, kaolin and silicon dioxide. 如請求項2或3之水稻害蟲防除用固形製劑,其中,前述結合劑係選自由流動石蠟、植物油脂、聚乙二醇及聚丙二醇所成之群組中之至少1種。 For example, the solid preparation for controlling rice pests as claimed in claim 2 or 3, wherein the aforementioned binder is at least one selected from the group consisting of liquid paraffin, vegetable oil, polyethylene glycol and polypropylene glycol. 如請求項1之水稻害蟲防除用固形製劑, 其係擠出型粒劑,前述固體載體包含增量劑,前述界面活性劑包含造粒性改良劑與崩壞及/或分散劑。 For example, the solid preparation for controlling rice pests in claim 1 is an extruded granule, the solid carrier includes an extender, and the surfactant includes a granulation improver and a disintegrating and/or dispersing agent. 如請求項7之水稻害蟲防除用固形製劑,其中,前述增量劑係選自由黏土、滑石、碳酸鈣、高嶺土、二氧化矽及膨潤土所成之群組中之至少1種。 For example, the solid preparation for controlling rice pests of claim 7, wherein the aforementioned extender is at least one selected from the group consisting of clay, talc, calcium carbonate, kaolin, silicon dioxide and bentonite. 如請求項7或8之水稻害蟲防除用固形製劑,其中,前述造粒性改良劑係選自由月桂基硫酸鈉、二烷基磺基琥珀酸鈉及烷基苯磺酸鈉所成之群組中之至少1種。 A solid preparation for controlling rice pests as claimed in claim 7 or 8, wherein the granulation improving agent is at least one selected from the group consisting of sodium lauryl sulfate, sodium dialkyl sulfosuccinate and sodium alkylbenzene sulfonate. 如請求項7或8之水稻害蟲防除用固形製劑,其中,前述崩壞及/或分散劑係選自由木質素磺酸鈉、木質素磺酸鈣、萘磺酸鈉福爾馬林縮合物、聚丙烯酸鈉、聚氧乙烯烷基醚硫酸鈉、聚氧化烯苯乙烯苯基醚硫酸鈉、聚氧化烯苯乙烯苯基醚磷酸鈉及聚氧乙烯聚氧丙烯聚合物硫酸鈉所成之群組中之至少1種。 For example, the solid preparation for controlling rice pests of claim 7 or 8, wherein the aforementioned disintegrating and/or dispersing agent is at least one selected from the group consisting of sodium lignin sulfonate, calcium lignin sulfonate, sodium naphthalene sulfonate formalin condensate, sodium polyacrylate, polyoxyethylene alkyl ether sodium sulfate, polyoxyalkylene styrene phenyl ether sodium sulfate, polyoxyalkylene styrene phenyl ether sodium phosphate and polyoxyethylene polyoxypropylene polymer sodium sulfate. 如請求項7或8之水稻害蟲防除用固形製劑,其中,前述結合劑係選自由聚乙烯醇、糊精、糖類、羧基甲基纖維素鈉、羥基丙基甲基纖維素及甲基纖維素所成之群組中之至少1種。 A solid preparation for controlling rice pests as claimed in claim 7 or 8, wherein the binder is at least one selected from the group consisting of polyvinyl alcohol, dextrin, sugars, sodium carboxymethylcellulose, hydroxypropylmethylcellulose and methylcellulose. 一種水稻害蟲防除方法,其係包含將如請求項1~11中任一項之水稻害蟲防除用固形製劑的有效量,施用在選自由水稻害蟲、水稻、土壤及田水面所成之群組中之至少1種之步驟。 A method for controlling rice pests, comprising the step of applying an effective amount of a solid preparation for controlling rice pests as described in any one of claims 1 to 11 to at least one selected from the group consisting of rice pests, rice, soil and field water surface. 如請求項12之水稻害蟲防除方法,其 中,前述水稻害蟲係選自由飛蝨類及二化螟類所成之群組中之至少1種。 The rice pest control method of claim 12, wherein the rice pest is at least one selected from the group consisting of flies and rice stem borers. 如請求項12或13之水稻害蟲防除方法,其中,前述水稻害蟲為藥劑抵抗性害蟲。 A rice pest control method as claimed in claim 12 or 13, wherein the rice pest is a pesticide-resistant pest. 如請求項12或13之水稻害蟲防除方法,其中,前述水稻害蟲防除用固形製劑的有效量以前述有效成分量計為耕地每10公畝1g~1kg。 For example, the rice pest control method of claim 12 or 13, wherein the effective amount of the solid preparation for rice pest control is 1g~1kg per 10 hectares of cultivated land, calculated as the amount of the active ingredient. 一種水稻害蟲防除用固形製劑之製造方法,其係如請求項2~6中任一項之水稻害蟲防除用固形製劑之製造方法,其特徵為包含:於前述核粒子加入前述結合劑,或前述結合劑及前述界面活性劑使其濕潤,而得到濕潤核粒子之濕潤步驟、與混合前述有效成分、前述界面活性劑及前述增量劑,或前述有效成分及前述增量劑並粉碎,而得到第1混合粉碎物之混合粉碎步驟、與混合前述濕潤核粒子與第1混合粉碎物,得到前述濕潤核粒子的表面以第1混合粉碎物被覆的被覆型粒劑之步驟。 A method for producing a solid preparation for controlling rice pests, which is a method for producing a solid preparation for controlling rice pests as claimed in any one of claims 2 to 6, characterized by comprising: a wetting step of adding the aforementioned binder, or the aforementioned binder and the aforementioned surfactant to the aforementioned core particles to make them wet, to obtain wet core particles, a mixing and grinding step of mixing the aforementioned active ingredient, the aforementioned surfactant and the aforementioned extender, or the aforementioned active ingredient and the aforementioned extender and grinding them to obtain a first mixed and ground product, and a step of mixing the aforementioned wet core particles with the first mixed and ground product to obtain a coated granule in which the surface of the aforementioned wet core particles is coated with the first mixed and ground product. 一種水稻害蟲防除用固形製劑之製造方法,其係如請求項7~11中任一項之水稻害蟲防除用固形製劑之製造方法,其特徵為包含:混合前述有效成分、前述增量劑及前述結合劑並粉碎,或混合前述有效成分、前述增量劑、前述結合劑、前述造粒性改良劑及前述崩壞及/或分散劑並粉碎,或混合 前述有效成分、前述增量劑及前述結合劑、與前述造粒性改良劑或前述崩壞及/或分散劑並粉碎,而得到第2混合粉碎物之混合粉碎步驟、與捏合第2混合粉碎物及水,或捏合第2混合粉碎物、水、前述造粒性改良劑及前述崩壞及/或分散劑,或捏合第2混合粉碎物及水、與前述造粒性改良劑或前述崩壞及/或分散劑,而得到捏合物之捏合步驟、與將前述捏合物以擠出型造粒機成型,而得到擠出型粒劑之步驟。A method for producing a solid preparation for controlling rice pests, which is a method for producing a solid preparation for controlling rice pests as claimed in any one of claims 7 to 11, characterized in that it comprises: mixing the aforementioned active ingredient, the aforementioned extender and the aforementioned binder and pulverizing, or mixing the aforementioned active ingredient, the aforementioned extender, the aforementioned binder, the aforementioned granulation improving agent and the aforementioned disintegration and/or dispersing agent and pulverizing, or mixing the aforementioned active ingredient, the aforementioned extender and the aforementioned binder, the aforementioned granulation improving agent and the aforementioned disintegration and/or dispersing agent and pulverizing. The invention further comprises a step of mixing and pulverizing the first mixed material and the second mixed material, and a step of kneading the second mixed material and water, or kneading the second mixed material, water, the granulation improver and the disintegration and/or dispersant, or kneading the second mixed material and water, and the granulation improver or the disintegration and/or dispersant to obtain a kneaded product, and a step of molding the kneaded product with an extrusion granulator to obtain extruded granules.
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