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CN101146449A - Pesticide composition - Google Patents

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CN101146449A
CN101146449A CNA2006800097091A CN200680009709A CN101146449A CN 101146449 A CN101146449 A CN 101146449A CN A2006800097091 A CNA2006800097091 A CN A2006800097091A CN 200680009709 A CN200680009709 A CN 200680009709A CN 101146449 A CN101146449 A CN 101146449A
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pesticide
liquid component
powdered
weight
parts
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田上学
植田展仁
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Sumitomo Chemical Co Ltd
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Abstract

The coated pesticidal granule obtained by aggregating a powdery pesticide with a thermosetting resin enables the controlled release of the pesticidal active ingredient. Furthermore, controlled release pesticide granules can be produced by the following steps: mixing a powdery pesticide with a first liquid component as a raw material for a thermosetting resin; adding a second liquid component as a raw material for a thermosetting resin; the first liquid component is then reacted with the second liquid component to produce the thermoset resin.

Description

农药组合物 Pesticide composition

技术领域 technical field

本发明涉及一种农药组合物,所述农药组合物含有处于可控释放形式的活性成分。The present invention relates to a pesticidal composition containing an active ingredient in a controlled release form.

背景技术 Background technique

常规上提出了各种农药配方,所述农药配方能够使农药活性成分得到持久的释放以保持功效,降低植物毒性等。作为这种可控释放的农药配方,已知有微胶囊配方、包覆有热固性树脂的农药粒剂(JP 11-5704A)、通过将农药活性成分与聚氨酯树脂混合获得的配方(JP 52-28942A)等。Various pesticide formulations have been conventionally proposed, which enable sustained release of pesticide active ingredients to maintain efficacy, reduce phytotoxicity, and the like. As such controlled-release pesticide formulations, there are known microcapsule formulations, pesticide granules coated with thermosetting resins (JP 11-5704A), formulations obtained by mixing the pesticide active ingredient with polyurethane resin (JP 52-28942A )wait.

发明内容 Contents of the invention

本发明提供一种农药组合物,所述农药组合物含有处于可控释放形式的农药活性成分。The present invention provides a pesticidal composition containing a pesticidal active ingredient in a controlled release form.

而且,本发明提供一种用于生产农药组合物的方法,所述农药组合物含有处于可控释放形式的农药活性成分。Furthermore, the present invention provides a method for producing a pesticidal composition containing a pesticidal active ingredient in a controlled release form.

本发明涉及一种包覆的农药粒剂,所述农药粒剂通过用热固性树脂使粉末状农药聚集而得到。例如如下所述生产这种农药粒剂。即,生产方法包括将粉末状农药与作为用于热固性树脂的原料的第一液体组分混合的步骤;随后将作为用于热固性树脂的原料的第二液体组分加入其中的步骤;通过使第一液体组分与第二液体组分反应以生成热固性树脂获得农药粒剂的步骤;以及还将第一液体组分和第二液体组分同时或依次加入到得到的农药粒剂中,并且使它们反应以用热固性树脂包覆农药粒剂的步骤。The present invention relates to a coated pesticide granule obtained by aggregating a powdered pesticide with a thermosetting resin. Such pesticide granules are produced, for example, as described below. That is, the production method includes the steps of mixing a powdery pesticide with a first liquid component as a raw material for a thermosetting resin; subsequently adding thereto a second liquid component as a raw material for a thermosetting resin; by making the first A step of reacting a liquid component with a second liquid component to generate a thermosetting resin to obtain a pesticide granule; and also simultaneously or sequentially adding the first liquid component and the second liquid component to the obtained pesticide granule, and making They react to the step of coating the pesticide granules with a thermosetting resin.

在本发明中,粉末状农药可以是单独的处于粉末形式的农药活性成分,并且通常是含有农药活性成分和稀释剂的粉末状组合物,平均粒径(体积中值直径)通常等于或小于100μm,特别是1至100μm,优选为1至30μm。In the present invention, the powdered pesticide may be a separate pesticide active ingredient in powder form, and is usually a powder composition containing the pesticide active ingredient and a diluent, and the average particle diameter (volume median diameter) is usually equal to or less than 100 μm , especially 1 to 100 μm, preferably 1 to 30 μm.

可以通过激光衍射粒径分析器如由MALVERN生产的MASTERSIZER2000等测量平均粒径。The average particle size can be measured by a laser diffraction particle size analyzer such as MASTERSIZER 2000 produced by MALVERN or the like.

作为农药活性成分通常提到的有:固体杀虫化合物、昆虫生长调节化合物、杀菌化合物、除草化合物、植物生长调节化合物、驱虫剂等,并且其具体实例包括下面显示的化合物。这些化合物在常温(20℃)下是固体,然而,优选的是熔点更高的化合物,其在例如50℃为固体。As the pesticidal active ingredients are generally mentioned: solid insecticidal compounds, insect growth regulating compounds, fungicidal compounds, herbicidal compounds, plant growth regulating compounds, insect repellents and the like, and specific examples thereof include the compounds shown below. These compounds are solid at ordinary temperature (20°C), however, compounds with a higher melting point which are solid at, for example, 50°C are preferred.

杀虫化合物和昆虫生长调节化合物包括拟除虫菊酯化合物,如溴氰菊酯、四溴菊酯、氟丙菊酯和胺菊酯;氨基甲酸酯化合物,如残杀威、异丙威、灭杀威、速灭威、XMC、甲萘威、嘧螨威(pyrimicarb)、克百威、灭多威和双氧威(phenoxycarb);有机磷化合物,如乙酰甲胺磷、三氯磷酸酯、杀虫威、二甲基亚硝胺、哒嗪硫磷、益棉磷和保棉磷;脲化合物,如除虫脲、氯蜱啶脲(chlorofluazuron)、虱螨脲、氟铃脲、氟虫脲、氟环脲、灭蝇胺、丁醚脲、噻螨酮、氟酰脲、氟苯脲、杀铃脲、4-氯-2-(2-氯-2-甲基丙基)-5-(6-碘-3-吡啶基甲氧基)哒嗪-3(2H)-酮、1-(2,6-二氟苯甲酰基)-3-[2-氟-4-(三氟甲基)苯基)脲、1-(2,6-二氟苯甲酰基)-3-[2-氟-4-(1,1,2,3,3,3-六氟丙氧基)苯基]脲、2-叔丁基亚氨基-3-异丙基-5-苯基-3,4,5,6-四氢-2H-1,3,5-噻二嗪(thiadiazon)-4-酮和1-(2,6-二氟苯甲酰基)-3-[2-氟-4-(1,1,2,2-四氟乙氧基)苯基]脲;拟新烟酸酯(neonicotinoid)化合物,如吡虫啉、啶虫脒、噻虫胺、烯啶虫胺和diacloden;杀螟丹、噻嗪酮、杀虫环、杀虫磺、双氧威、喹螨醚(fenezaquin)、唑螨酯、哒螨灵、伏蚁腙、硫双威、虫螨腈、唑螨酯、吡蚜酮、嘧螨醚、虫酰肼、吡螨胺、唑蚜威、茚虫威、氟虫胺、弥拜菌素、伊维菌素(ivermectin)、硼酸、对二氯苯等。Insecticidal compounds and insect growth-regulating compounds include pyrethroid compounds such as deltamethrin, perfenthrin, bifenthrin, and tetramethrin; carbamate compounds such as propoxur, isoprocarb, Carbaryl, amecarb, XMC, carbaryl, pyrimicarb, carbofuran, methomyl, and phenoxycarb; organophosphorus compounds such as acephate, triclosate, Chormocarb, dimethylnitrosamine, pyridazuron, acetphos, and acetphos; urea compounds such as diflubenzuron, chlorofluazuron, lufenuron, hexaflumuron, flubenzuron , Flucyclouron, cyromazine, diafenthiuron, hexythiazox, fluorourea, hexafenuron, triflumuron, 4-chloro-2-(2-chloro-2-methylpropyl)-5- (6-iodo-3-pyridylmethoxy)pyridazin-3(2H)-one, 1-(2,6-difluorobenzoyl)-3-[2-fluoro-4-(trifluoromethyl base) phenyl) urea, 1-(2,6-difluorobenzoyl)-3-[2-fluoro-4-(1,1,2,3,3,3-hexafluoropropoxy)benzene base] urea, 2-tert-butylimino-3-isopropyl-5-phenyl-3,4,5,6-tetrahydro-2H-1,3,5-thiadiazine (thiadiazon)-4 -one and 1-(2,6-difluorobenzoyl)-3-[2-fluoro-4-(1,1,2,2-tetrafluoroethoxy)phenyl]urea; pseudoneonicotinic acid Esters (neonicotinoid) compounds such as imidacloprid, acetamiprid, clothianidin, nitenpyram, and diacloden; cartap, buprofezin, bisultap, sulfon, fenoxycarb, fenezaquin , Fenpyramid, Pyridaben, Hydramethylnon, Thiodicarb, Chlorfenapyr, Fenpyroxan, Pymetrozine, Pyrimizafen, Tebufenozide, Tetrapyramid, Fenpyramid, Indoxacarb, Fluoride Insectamine, mibamectin, ivermectin, boric acid, p-dichlorobenzene, etc.

杀菌化合物包括苯并咪唑化合物,如苯菌灵、多菌灵、噻菌灵和甲基硫菌灵以及它们的前体;氨基甲酸苯酯化合物,如乙霉威;二羧基亚胺(dicarboxyimide)化合物,如腐霉利、异菌脲和乙烯菌核利;唑化合物,如烯唑醇、烯丙苯噻唑、环氧唑醇(epoxyconazole)、戊唑醇、苯醚甲环唑、环丙唑醇、氟硅唑和三唑酮;酰基丙氨酸化合物,如甲霜灵;甲酰胺化合物,如氟吡菌胺(furametpyr)、灭锈胺、氟酰胺和trifluzamide;有机磷化合物,如甲基三氯乙磷酸(triclofos-methyl)、三乙膦酸铝和定菌磷;苯胺基嘧啶化合物,如嘧霉胺、嘧菌胺和嘧菌环胺;氰基吡咯化合物,如咯菌腈和拌种咯;抗生素,如杀稻瘟菌素S(blastocidin S)、春雷霉素、多氧菌素和有效霉素;甲氧基丙烯酸酯和甲氧基丙烯酰胺化合物,如嘧菌酯、醚菌酯和苯氧菌胺;白菌清、代森锰锌、克菌丹、灭菌丹、三环唑、咯喹酮、烯丙苯噻唑、四氯苯酞(fthalide)、霜脲氰、烯酰吗啉、活化酯-S-甲基、噁唑菌酮、噁喹酸、氟啶胺、嘧菌腙、双氯氰菌胺、4-氯-3-甲基-2(3H)-苯并噻唑酮(chlobenthiazone)、异戊二酮(isovaledione)、四氯间苯二氰、硫代邻苯二甲酰亚胺氧基联苯氧胂(thiophthalimideoxybisphenoxyarsine)、氨基甲酸3-碘-2-丙基丁酯、对羟基苯甲酸酯、脱氢乙酸钠、山梨酸钾等。Fungicidal compounds include benzimidazole compounds such as benomyl, carbendazim, thiabendazole, and thiophanate-methyl and their precursors; phenylcarbamate compounds such as diethofencarb; dicarboxyimides Compounds such as procymidone, iprodione, and vinclozolin; azole compounds such as diniconazole, allylbenzothiazole, epoxyconazole, tebuconazole, difenoconazole, cyproconazole Alcohols, flusilazoles, and triazolones; acylalanine compounds, such as metalaxyl; formamide compounds, such as furametpyr, methazolamine, fluoroamide, and trifluzamide; organophosphorus compounds, such as methyl Triclofos-methyl, triclofos-methyl, triclofos-methyl, and triclofos; anilinopyrimidine compounds such as pyrimethanil, pyrimethanil, and cyprodinil; cyanopyrrole compounds such as fludioxonil and cyprodinil Antibiotics such as blasticidin S, kasugamycin, polyoxin, and validamycin; methoxyacrylate and methoxyacrylamide compounds such as azoxystrobin, krexabactin esters and phenoxystrobin; blephazil, mancozeb, captan, folpet, tricyclazole, pyroquinone, allylbenzothiazole, tetrachlorophthalide (fthalide), cymoxanil, alkenyl Acylmorpholine, activated ester-S-methyl, oxaflucone, oxquinic acid, fluazinam, pyrizone, diclofenac, 4-chloro-3-methyl-2(3H)-benzene Chlobenthiazone, isovaledione, tetrachloroisophthalocyanine, thiophthalimideoxybisphenoxyarsine, 3-iodo-2-propane carbamate Butyl butyl ester, paraben, sodium dehydroacetate, potassium sorbate, etc.

除草化合物包括三嗪化合物,如莠去津和嗪草酮;脲化合物,如伏草龙和异丙隆;羟基苄腈化合物,如溴苯腈和碘苯腈;2,6-二硝基苯胺化合物,如二甲戊灵和氟乐灵;芳氧基链烷酸化合物,如2,4-滴、麦草畏、氯氟吡氧乙酸和2-甲基-4-氯丙酸;磺酰脲化合物,如苄嘧磺隆、甲磺隆、烟嘧磺隆、氟嘧磺隆和环丙嘧磺隆;咪唑啉酮化合物,如咪唑烟酸、咪唑喹啉酸和咪唑乙烟酸;双草醚、bisthiobac-sodium、三氟羧草醚、甲磺草胺、白草枯、唑嘧磺草胺(flumeturam)、氟胺磺隆、精噁唑禾草灵、吡氟酰草胺、氟草敏、异噁唑草酮、草丁磷铵(ammonium glufosinate)、草甘膦、灭草松、苯噻酰草胺、敌稗、氟噻草胺、氟烯草酸、丙炔氟草胺等。Herbicidal compounds include triazine compounds, such as atrazine and metrizone; urea compounds, such as fenflurone and isoproturon; hydroxybenzonitrile compounds, such as bromoxynil and ioxynil; 2,6-dinitroaniline Compounds such as pendimethalin and trifluralin; aryloxyalkanoic acid compounds such as 2,4-D, dicamba, fluroxypyr, and 2-methyl-4-chloropropionic acid; sulfonylureas Compounds such as bensulfuron-methyl, metsulfuron-methyl, nicosulfuron, flurisulfuron-methyl, and cyprosulfuron-methyl; imidazolinone compounds such as imazethapyr, imazaquin, and imazethapyr; bisfluben, bisthiobac -sodium, acifluorfen, sulfentram, diquat, flumeturam, flusulfuron-methyl, fenoxaprop-p-ethyl, diflufenamide, flumetram, isoprop Oxaflumelezone, ammonium glufosinate, glyphosate, bentazone, mefenacet, propanil, flufenacet, flufenoxalic acid, propargyl flufenamide, etc.

植物生长调节化合物包括马来酰肼、矮壮素(chlormequat)、乙烯磷、赤霉素、甲哌鎓、噻苯隆、抗倒胺、亚异砜磷、烯效唑等。驱虫剂包括1S,3R,4R,6R-蒈-3,4-二醇、2,5-吡啶二甲酸二丙酯等。Plant growth regulating compounds include maleic hydrazide, chlormequat, ethenylphos, gibberellin, mepiperium, thiadizuron, triadamide, sulfophos, uniconazole, and the like. Insect repellents include 1S, 3R, 4R, 6R-carene-3,4-diol, 2,5-dipropyl pyridinedicarboxylate and the like.

在本发明中,即使在液体农药活性成分的情况下,也可以将它用作粉末状农药,即处于固定在稀释剂上的粉末的形式的组合物。In the present invention, even in the case of a liquid pesticide active ingredient, it can be used as a powder pesticide, that is, a composition in the form of a powder fixed on a diluent.

稀释剂是用于粉末状农药的固体载体,并且包括矿物载体,例如高岭土矿物,如高岭石、地开石、珍珠陶土和多水高岭石(halocite);蛇纹石,如贵橄榄石、利蛇纹石(lizartite)、叶蛇纹石和镁绿泥石;蒙脱土矿物,如钠型蒙脱土、钙型蒙脱土和镁型蒙脱土;蒙脱石,如皂石、锂蒙脱石(hectrite)、锌蒙脱石和hyderite;云母类,如叶蜡石、滑石、寿山石、白云母、多硅白云母、绢云母和伊利石;二氧化硅,如方晶石、无定形二氧化硅和石英;硅酸镁水合物,如绿坡缕石和海泡石;硫酸盐矿物,如石膏;白云石、碳酸钙、沸石、沸腾石、凝灰石、蛭石、合成锂皂石(laponite)、浮石、硅藻土、酸性粘土、白土等。这些可以单独或以两种或更多种组合使用。Diluents are solid carriers for powdered pesticides and include mineral carriers such as kaolin minerals such as kaolinite, dickite, nacrite and halocite; serpentines such as chrysanthemum , lizartite (lizartite), antigorite and magnesium chloride; montmorillonite minerals, such as sodium montmorillonite, calcium montmorillonite and magnesium montmorillonite; montmorillonite, such as saponite, Hectorite (hectrite), sauconite and hyderite; micas, such as pyrophyllite, talc, shoushanite, muscovite, polysilicic muscovite, sericite and illite; silicon dioxide, such as cristobalite, Shaped silica and quartz; magnesium silicate hydrates such as attapulgite and sepiolite; sulfate minerals such as gypsum; dolomite, calcium carbonate, zeolite, zeolite, tuff, vermiculite, lithium soap Laponite, pumice, diatomaceous earth, acid clay, clay, etc. These can be used alone or in combination of two or more.

除农药活性成分以外,粉末状农药还可以含有用于农药的助剂,如稀释剂、表面活性剂、稳定剂、着色剂、香料等。In addition to the active ingredients of pesticides, powdered pesticides may also contain adjuvants for pesticides, such as diluents, surfactants, stabilizers, colorants, fragrances, etc.

表面活性剂包括非离子表面活性剂,如聚氧乙烯烷基醚、聚氧乙烯烷基芳基醚、聚氧乙烯羊毛脂醇、聚氧乙烯烷基酚福尔马林缩合物、聚氧乙烯山梨聚糖脂肪酸酯、聚氧乙烯甘油基单脂肪酸酯、聚氧化丙二醇单脂肪酸酯、聚氧乙烯山梨醇脂肪酸酯、聚氧乙烯蓖麻油衍生物、聚氧乙烯脂肪酸酯、高级脂肪酸甘油酯、山梨聚糖脂肪酸酯、蔗糖脂肪酸酯、聚氧乙烯聚氧丙烯嵌段聚合物、聚氧乙烯脂肪酰胺、烷基醇酰胺和聚氧乙烯烷基胺;阳离子表面活性剂,如烷基胺盐酸盐(例如,十二烷基胺盐酸盐)、烷基季铵盐(例如,十二烷基三甲基铵盐、烷基二甲基苄基铵盐、烷基毗啶鎓盐、烷基异喹啉鎓盐、二烷基吗啉鎓盐)、苯索氯铵和聚烷基乙烯基吡啶鎓盐;阴离子表面活性剂,如脂肪酸钠盐(例如,棕榈酸钠)、醚羧酸的钠盐(例如,聚氧乙烯月桂基醚羧酸钠)、高级脂肪酸的氨基酸缩合物(例如,月桂酰基肌氨酸钠、N-月桂酰基谷氨酸钠)、高级脂肪酸酯磺酸盐(例如,高级烷基磺酸盐、月桂酯磺酸盐)、二烷基磺基琥珀酸盐(例如,二辛基磺基琥珀酸盐)、高级脂肪酰胺磺酸盐(例如,油酰胺磺酸盐)、烷基芳基磺酸盐(例如,十二烷基苯磺酸钠、二异丙基萘磺酸盐)、烷基芳基磺酸盐的福尔马林缩合物、高级醇硫酸酯盐(例如,十五烷-2-硫酸盐)、聚氧乙烯烷基磷酸盐(例如,二聚氧乙烯十二烷基醚磷酸盐)、苯乙烯-马来酸盐共聚物等;两性表面活性剂,如N-月桂基丙氨酸、N,N,N-三甲基氨基丙酸、N,N,N-三羟基乙基氨基丙酸、N-己基-N,N-二甲基氨基乙酸、1-(2-羧乙基)吡啶鎓甜菜碱和卵磷脂。Surfactants include nonionic surfactants, such as polyoxyethylene alkyl ether, polyoxyethylene alkyl aryl ether, polyoxyethylene lanolin alcohol, polyoxyethylene alkylphenol formalin condensate, polyoxyethylene Sorbitan fatty acid ester, polyoxyethylene glyceryl mono fatty acid ester, polyoxypropylene glycol mono fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene castor oil derivative, polyoxyethylene fatty acid ester, advanced Fatty acid glycerides, sorbitan fatty acid esters, sucrose fatty acid esters, polyoxyethylene polyoxypropylene block polymers, polyoxyethylene fatty amides, alkylolamides and polyoxyethylene alkylamines; cationic surfactants, Such as alkylamine hydrochloride (for example, dodecylamine hydrochloride), alkyl quaternary ammonium salt (for example, dodecyltrimethylammonium salt, alkyldimethylbenzylammonium salt, alkyl pyridinium salts, alkylisoquinolinium salts, dialkylmorpholinium salts), benzethonium chloride and polyalkylvinylpyridinium salts; anionic surfactants such as sodium salts of fatty acids (for example, palmitic acid sodium), sodium salts of ether carboxylic acids (for example, sodium polyoxyethylene lauryl ether carboxylate), amino acid condensates of higher fatty acids (for example, sodium lauroyl sarcosinate, sodium N-lauroyl glutamate), higher Fatty acid ester sulfonates (e.g., higher alkyl sulfonates, lauryl sulfonates), dialkyl sulfosuccinates (e.g., dioctyl sulfosuccinate), higher fatty acid amide sulfonates (e.g., oleamide sulfonate), alkylarylsulfonate (e.g., sodium dodecylbenzenesulfonate, diisopropylnaphthalenesulfonate), formalin of alkylarylsulfonate Lin condensates, higher alcohol sulfates (for example, pentadecane-2-sulfate), polyoxyethylene alkyl phosphates (for example, dipolyoxyethylene lauryl ether phosphate), styrene-malay salt copolymer, etc.; amphoteric surfactants, such as N-lauryl alanine, N,N,N-trimethylalanine, N,N,N-trihydroxyethylalanine, N-hexyl -N,N-Dimethylglycine, 1-(2-carboxyethyl)pyridinium betaine and lecithin.

稳定剂包括例如酚抗氧化剂、胺抗氧化剂、磷类抗氧化剂、硫类抗氧化剂、紫外吸收剂、环氧化植物油,如环氧化大豆油、环氧化亚麻油和环氧化菜籽油;酸式磷酸异丙酯、液体石蜡、1,2-亚乙基二醇等。Stabilizers include, for example, phenolic antioxidants, amine antioxidants, phosphorus antioxidants, sulfur antioxidants, UV absorbers, epoxidized vegetable oils such as epoxidized soybean oil, epoxidized linseed oil, and epoxidized rapeseed oil ; Isopropyl acid phosphate, liquid paraffin, 1,2-ethylene glycol, etc.

着色剂包括例如若丹明,如若丹明B和黄若丹明(solar rhodamine)和色料,如Yellow No.4、Blue No.1和Red No.2,并且香料包括例如酯香料,如乙酰乙酸乙酯、庚酸乙酯(ethyl enantate)、肉桂酸乙酯和乙酸异戊酯;有机酸香料,如己酸和肉桂酸;醇香料,如肉桂醇、香叶醇、柠檬醛和癸醇;醛,如香草醛、胡椒醛和紫苏醛(perilaldehyde);酮香料,如麦芽酚和甲基β-萘基酮、薄荷醇等。Colorants include, for example, rhodamines, such as Rhodamine B and solar rhodamine, and colorants, such as Yellow No. 4, Blue No. 1, and Red No. 2, and fragrances include, for example, ester fragrances such as ethyl acetoacetate Esters, ethyl enantate, ethyl cinnamate, and isoamyl acetate; organic acid fragrances, such as caproic acid and cinnamic acid; alcohol fragrances, such as cinnamyl alcohol, geraniol, citral, and decanol; aldehydes , such as vanillin, piperonal and perilaldehyde; ketone flavors, such as maltol and methyl β-naphthyl ketone, menthol, etc.

当粉末状农药包含稀释剂时,在粉末状农药中的农药活性成分的量通常为1至95重量%,优选为10至90重量%,稀释剂的量通常为5至99重量%,优选为10至90重量%。当粉末状农药包含用于农药的助剂时,用于农药的助剂的总量通常为1至30重量%,优选为2至20重量%。When the powdery pesticide contains a diluent, the amount of the pesticide active ingredient in the powdery pesticide is usually 1 to 95% by weight, preferably 10 to 90% by weight, and the amount of the diluent is usually 5 to 99% by weight, preferably 10 to 90% by weight. When the powdery pesticide contains an adjuvant for pesticides, the total amount of adjuvants for pesticides is usually 1 to 30% by weight, preferably 2 to 20% by weight.

通过混合并且粉碎农药活性成分、在必要时的稀释剂,此外在必要时的用于农药的助剂,如表面活性剂、稳定剂、着色剂、香料等,获得粉末状农药。此外,还可以通过混合预先被粉碎成粉末状的组分获得粉末状农药。Powdered pesticides are obtained by mixing and pulverizing pesticide active ingredients, diluents if necessary, and auxiliaries for pesticides such as surfactants, stabilizers, colorants, fragrances, etc. if necessary. In addition, powdered pesticides can also be obtained by mixing components that have been pulverized into powders in advance.

作为用于固定粉末状农药的热固性树脂,提及的有:尿素树脂、氨基甲酸酯-尿素树脂、环氧树脂等,并且在本发明中,特别优选氨基甲酸酯树脂。As the thermosetting resin for fixing the powdery pesticide, there are mentioned: urea resin, urethane-urea resin, epoxy resin and the like, and in the present invention, urethane resin is particularly preferable.

本发明的农药粒剂的平均粒径(体积中值直径)通常为1至200μm,优选为10至200μm,更优选为20至150μm。可以通过激光衍射粒度分析器,如由MALVERN生产的MASTERSIZER 2000等测量平均粒径。The average particle diameter (volume median diameter) of the pesticide granules of the present invention is usually 1 to 200 μm, preferably 10 to 200 μm, more preferably 20 to 150 μm. The average particle diameter can be measured by a laser diffraction particle size analyzer such as MASTERSIZER 2000 produced by MALVERN or the like.

通常通过使两种不同的液体组分反应获得热固性树脂,并且通过例如下列方法生产本发明的农药粒剂:将粉末状农药与作为用于热固性树脂的原料的第一液体组分混合,然后将作为用于热固性树脂的原料的第二液体组分加入其中,使第一液体组分与第二液体组分反应以生成热固性树脂,此外在必要时,同时或依次加入第一液体组分和第二液体组分,并且使它们反应以生成热固性树脂。通过调节第一液体组分和第二液体组分的量,可以调节由热固性树脂制成的包覆层的厚度以将可控释放的程度改变至需要的程度。第一液体组分和第二液体组分各自不必限于只由一种组分组成,并且可以是混合物。A thermosetting resin is usually obtained by reacting two different liquid components, and the pesticide granules of the present invention are produced by, for example, mixing a powdered pesticide with the first liquid component as a raw material for the thermosetting resin, and then A second liquid component as a raw material for a thermosetting resin is added thereto, the first liquid component is reacted with the second liquid component to produce a thermosetting resin, and furthermore, when necessary, the first liquid component and the second liquid component are added simultaneously or sequentially. two liquid components and react them to form a thermosetting resin. By adjusting the amounts of the first liquid component and the second liquid component, the thickness of the coating layer made of thermosetting resin can be adjusted to vary the degree of controlled release to a desired degree. Each of the first liquid component and the second liquid component is not necessarily limited to consist of only one component, and may be a mixture.

当热固性树脂是氨基甲酸酯树脂时,第一液体组分和第二液体组分中的一种是多元醇,并且另一种是聚异氰酸酯。When the thermosetting resin is a urethane resin, one of the first liquid component and the second liquid component is a polyol, and the other is a polyisocyanate.

多元醇包括缩合的聚酯多元醇、聚醚多元醇、聚丙烯酸多元醇、聚甲基丙烯酸多元醇、内酯类聚酯多元醇、聚碳酸酯多元醇、天然多元醇和它们的变性产物等。所述缩合的聚酯多元醇通常是通过多元醇与二元酸的缩合反应得到的。聚醚多元醇通常是通过环氧丙烷或环氧乙烷与多元醇的加成聚合等得到的。聚丙烯酸多元醇和聚甲基丙烯酸多元醇通常是通过下列反应得到的:聚丙烯酸与多元醇的缩合反应、聚甲基丙烯酸与多元醇的缩合反应、丙烯酸与多元醇的缩合反应、甲基丙烯酸与多元醇的缩合反应、丙烯酸酯单体的聚合反应或甲基丙烯酸酯单体的聚合反应。内酯类聚酯多元醇是使用多元醇作为引发剂通过ε-己内酯的开环聚合得到的。聚碳酸酯多元醇通常是通过二醇与碳酸酯的反应得到的,并且多元醇包括亚甲基二醇、1,2-亚乙基二醇、1,2-丙二醇、1,4-丁二醇、1,6-己二醇、三羟甲基丙烷、聚丁二醇、甘油和它们的低聚物等。Polyols include condensed polyester polyols, polyether polyols, polyacrylic polyols, polymethacrylic polyols, lactone polyester polyols, polycarbonate polyols, natural polyols and their denatured products, and the like. The condensed polyester polyols are generally obtained by condensation reaction of polyols with dibasic acids. Polyether polyols are generally obtained by addition polymerization of propylene oxide or ethylene oxide and polyols, or the like. Polyacrylic acid polyol and polymethacrylic acid polyol are usually obtained through the following reactions: condensation reaction of polyacrylic acid and polyol, condensation reaction of polymethacrylic acid and polyol, condensation reaction of acrylic acid and polyol, methacrylic acid and Condensation of polyols, polymerization of acrylate monomers or polymerization of methacrylate monomers. Lactone-based polyester polyols are obtained by ring-opening polymerization of ε-caprolactone using polyols as initiators. Polycarbonate polyols are usually obtained by the reaction of diols with carbonates, and polyols include methylene glycol, 1,2-ethylene glycol, 1,2-propylene glycol, 1,4-butanediol Alcohol, 1,6-hexanediol, trimethylolpropane, polytetramethylene glycol, glycerin and their oligomers, etc.

作为在本发明中使用的多元醇,优选支链多元醇,以及支链多元醇和直链多元醇的混合物,并且在所述混合物之中,优选的是这样的混合物,其中,基于存在于多元醇中的羟基,源自直链多元醇的羟基的数量等于或小于60%。支链多元醇是在分子中含有三个或更多个羟基的多元醇,并且优选在分子中含有三个羟基的多元醇。直链多元醇是在分子中含有两个羟基的多元醇,并且通常在分子的两端中的每一个含有羟基。As the polyol used in the present invention, preferred are branched chain polyols, and mixtures of branched chain polyols and linear polyols, and among the mixtures, preferred are mixtures in which, based on the presence in the polyol In the hydroxyl group, the number of hydroxyl groups derived from linear polyols is equal to or less than 60%. The branched polyol is a polyol containing three or more hydroxyl groups in a molecule, and preferably a polyol containing three hydroxyl groups in a molecule. A linear polyol is a polyol containing two hydroxyl groups in a molecule, and usually contains a hydroxyl group at each of both ends of the molecule.

优选上述直链多元醇是OH当量等于或小于100的直链多元醇,以及OH当量等于或小于100的直链多元醇与OH当量等于或大于100的直链多元醇的混合物,并且在混合物之中,优选的是这样的混合物,其中,基于存在于多元醇中的羟基,源自OH当量等于或大于100的直链多元醇的羟基的数量等于或小于60%。OH当量等于或小于100的直链多元醇包括1,2-亚乙基二醇、1,2-丙二醇、1,3-丙二醇等。Preferably, the aforementioned linear polyol is a linear polyol having an OH equivalent of 100 or less, and a mixture of a linear polyol having an OH equivalent of 100 or less and a linear polyol having an OH equivalent of 100 or greater, and between the mixture Among them, preferred is a mixture in which the number of hydroxyl groups derived from a linear polyol having an OH equivalent of 100 or more is 60% or less based on the hydroxyl groups present in the polyol. The linear polyhydric alcohol having an OH equivalent of 100 or less includes ethylene glycol, 1,2-propanediol, 1,3-propanediol, and the like.

聚异氰酸酯包括甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)、萘二异氰酸酯、甲苯二异氰酸酯、六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、苯二亚甲基二异氰酸酯、4,4-亚甲基双(异氰酸环己酯)、三甲基六亚甲基二异氰酸酯、1,3-(异氰酸甲酯基)环己烷、三苯基甲烷三异氰酸酯、三(异氰酸苯酯基)硫代磷酸酯等。还可以使用变性的异氰酸酯及其低聚物代替上述聚异氰酸酯单体,条件是它们具有流动性。变性的异氰酸酯包括加合物变性的异氰酸酯、缩二脲变性的异氰酸酯、异氰脲酸酯变性的异氰酸酯、嵌段变性的异氰酸酯、预聚物变性的异氰酸酯、二聚化变性的异氰酸酯等。出于容易控制反应和低蒸气压以及优异的可加工性的观点,优选聚亚甲基聚苯基异氰酸酯(聚合的MDI),其通过使苯胺和福尔马林缩合并且使得到的多胺光气化而获得。Polyisocyanates include toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), naphthalene diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, xylylene diisocyanate, 4,4-methylenebis(cyclohexylisocyanate), trimethylhexamethylene diisocyanate, 1,3-(isocyanatomethyl)cyclohexane, triphenylmethane triisocyanate, Tris(isocyanatophenyl)phosphorothioate and the like. Denatured isocyanates and oligomers thereof may also be used instead of the above-mentioned polyisocyanate monomers, provided they have fluidity. The denatured isocyanate includes adduct denatured isocyanate, biuret denatured isocyanate, isocyanurate denatured isocyanate, block denatured isocyanate, prepolymer denatured isocyanate, dimerization denatured isocyanate and the like. From the viewpoint of easy reaction control and low vapor pressure and excellent processability, polymethylene polyphenylisocyanate (polymerized MDI), which is obtained by condensing aniline and formalin and making the resulting polyamine photosensitive, is preferable. obtained by gasification.

通过使多元醇与聚异氰酸酯在加热下,例如在40至100℃反应生成氨基甲酸酯树脂。在这种操作中,在必要时加入硬化催化剂,如有机金属化合物、胺等。The urethane resin is produced by reacting a polyol with a polyisocyanate under heating, for example, at 40 to 100°C. In this operation, a hardening catalyst such as an organometallic compound, an amine, etc. is added as necessary.

硬化催化剂包括有机金属化合物,如二醋酸二丁锡、二丁锡化二氯、二月桂酸二丁锡、二丁基硫代锡酸、辛酸亚锡、二月桂酸二正辛锡等,三亚乙基二胺、N-甲基吗啉、N,N-二甲基二(十二烷基)胺、N-十二烷基吗啉、N,N-二甲基环己胺、N-乙基吗啉、二甲基乙醇胺、N,N-二甲基苄基胺、1,8-二氮杂双环[5.4.0]十一碳烯-7、钛酸异丙酯、钛酸四丁酯、钒酸氧异丙酯、锆酸正丙酯、1,4-二氮杂双环[2.2.2]辛烷等。Hardening catalysts include organometallic compounds such as dibutyltin diacetate, dibutyltin dichloride, dibutyltin dilaurate, dibutylthiostannoic acid, stannous octoate, dioctyltin dilaurate, etc., triethylene Diamine, N-methylmorpholine, N,N-dimethylbis(dodecyl)amine, N-dodecylmorpholine, N,N-dimethylcyclohexylamine, N-ethyl Morpholine, Dimethylethanolamine, N,N-Dimethylbenzylamine, 1,8-diazabicyclo[5.4.0]undecene-7, isopropyl titanate, tetrabutyl titanate , Oxyisopropyl vanadate, n-propyl zirconate, 1,4-diazabicyclo[2.2.2]octane, etc.

当热固性树脂是氨基甲酸酯树脂时,可以使用多元醇或聚异氰酸酯中的任何一种作为第一液体组分,并且优选地,使用多元醇作为第一液体组分并且使用聚异氰酸酯作为第二液体组分。当使用硬化催化剂时,可以将硬化催化剂加入到第一液体组分和第二液体组分中的任何一种中,并且优选加入到第一液体组分中。When the thermosetting resin is a urethane resin, either polyol or polyisocyanate may be used as the first liquid component, and preferably, polyol is used as the first liquid component and polyisocyanate is used as the second liquid component. liquid component. When a hardening catalyst is used, the hardening catalyst may be added to any one of the first liquid component and the second liquid component, and is preferably added to the first liquid component.

当热固性树脂是尿素树脂时,第一液体组分和第二液体组分中的任何一种是多胺或水,并且另一种是聚异氰酸酯。When the thermosetting resin is a urea resin, any one of the first liquid component and the second liquid component is polyamine or water, and the other is polyisocyanate.

聚异氰酸酯包括上述聚异氰酸酯,并且多胺包括二亚乙基三胺、三亚乙基四胺等。The polyisocyanates include the above-mentioned polyisocyanates, and the polyamines include diethylenetriamine, triethylenetetramine, and the like.

当热固性树脂是尿素树脂时,可以使用多胺、水或聚异氰酸酯中的任何一种作为第一液体组分,并且优选使用多胺作为第一液体组分并且使用聚异氰酸酯作为第二液体组分。当使用水作为液体组分时,通常使用聚异氰酸酯作为第一液体组分并且使用水作为第二液体组分。When the thermosetting resin is a urea resin, any one of polyamine, water or polyisocyanate may be used as the first liquid component, and it is preferable to use polyamine as the first liquid component and polyisocyanate as the second liquid component . When water is used as the liquid component, generally polyisocyanate is used as the first liquid component and water is used as the second liquid component.

当热固性树脂是氨基甲酸酯-尿素树脂时,第一液体组分和第二液体组分中的一种是多元醇和多胺的混合物,并且另一种是聚异氰酸酯。优选使用多元醇和多胺的混合物作为第一液体组分,并且使用聚异氰酸酯作为第二液体组分。When the thermosetting resin is a urethane-urea resin, one of the first liquid component and the second liquid component is a mixture of polyol and polyamine, and the other is polyisocyanate. Preference is given to using mixtures of polyols and polyamines as the first liquid component and polyisocyanates as the second liquid component.

当热固性树脂是环氧树脂时,第一液体组分和第二液体组分中的任何一种是硬化剂,并且另一种是含有缩水甘油基的化合物。When the thermosetting resin is an epoxy resin, either one of the first liquid component and the second liquid component is a hardener, and the other is a glycidyl group-containing compound.

硬化剂通常是多胺,并且含有缩合甘油基的化合物通常包括聚缩水甘油醚、聚缩水甘油胺等。The hardener is generally a polyamine, and the compound containing a condensed glyceryl group generally includes polyglycidyl ether, polyglycidylamine, and the like.

多胺包括二亚乙基三胺、三亚乙基四胺、间-苯二甲胺、异佛二酮二胺、甲基亚氨基双丙胺、萜烷二胺、间苯二胺、二氨基苯基甲烷、二氨基二苯基砜、二氨基二乙基二苯基甲烷、聚酰胺变性的多胺、酮变性的多胺、环氧变性的多胺、硫脲变性的多胺、曼尼希变性的多胺、迈克尔加成变性的多胺等,并且含有缩水甘油基的化合物包括聚缩水甘油醚,如双酚A类聚缩水甘油醚、双酚F类聚缩水甘油醚、氢化双酚A类聚缩水甘油醚、萘类聚缩水甘油醚、溴化双酚A类聚缩水甘油醚、双酚S类聚缩水甘油醚、双酚AF类聚缩水甘油醚、联苯类聚缩水甘油醚、Fluolein类聚缩水甘油醚、苯酚酚醛清漆类聚缩水甘油醚、邻甲酚酚醛清漆类聚缩水甘油醚、DPP酚醛清漆类聚缩水甘油醚、三羟基苯基甲烷类聚缩水甘油醚和四苯氧基乙烷(tetraphenylolethane)类聚缩水甘油醚;和聚缩水甘油胺,如四缩水甘油基二氨基二苯基甲烷类聚缩水甘油胺、乙内酰脲类聚缩水甘油胺、1,3-双(N,N-二缩水甘油基氨基甲基)环己烷、苯胺类聚缩水甘油胺、甲苯胺类聚缩水甘油胺、三缩水甘油基异氰酸酯类聚缩水甘油胺和氨基苯酚类聚缩水甘油胺。Polyamines include diethylenetriamine, triethylenetetramine, m-xylylenediamine, isophordionediamine, methyliminodipropylamine, terpanediamine, m-phenylenediamine, diaminobenzene Diaminodiphenylsulfone, diaminodiethyldiphenylmethane, polyamide-denatured polyamine, ketone-denatured polyamine, epoxy-denatured polyamine, thiourea-denatured polyamine, Mannich Denatured polyamines, Michael addition denatured polyamines, etc., and compounds containing glycidyl groups include polyglycidyl ethers, such as bisphenol A polyglycidyl ethers, bisphenol F polyglycidyl ethers, hydrogenated bisphenol A Polyglycidyl ether-like, polyglycidyl ether of naphthalene, polyglycidyl ether of brominated bisphenol A, polyglycidyl ether of bisphenol S, polyglycidyl ether of bisphenol AF, polyglycidyl ether of biphenyl, Fluolein polyglycidyl ether, phenol novolac polyglycidyl ether, o-cresol novolac polyglycidyl ether, DPP novolac polyglycidyl ether, trihydroxyphenylmethane polyglycidyl ether and tetraphenoxy Tetraphenylolethane polyglycidyl ethers; and polyglycidylamines, such as tetraglycidyldiaminodiphenylmethane polyglycidylamines, hydantoin polyglycidylamines, 1,3-bis (N,N-diglycidylaminomethyl)cyclohexane, aniline polyglycidylamines, toluidine polyglycidylamines, triglycidylisocyanate polyglycidylamines, and aminophenol polyglycidylamines .

优选使用多胺作为第一液体组分并且使用聚缩水甘油醚或聚缩水甘油胺作为第二液体组分。Preference is given to using polyamines as the first liquid component and polyglycidyl ethers or polyglycidylamines as the second liquid component.

本发明还提供一种用于生产农药组合物的方法,所述方法包括将粉末状农药与作为用于热固性树脂的原料的第一液体组分混合的步骤;随后将作为用于热固性树脂的原料的第二液体组分加入其中的步骤;以及使第一液体组分与第二液体组分反应以生成热固性树脂的步骤。The present invention also provides a method for producing an agrochemical composition, the method comprising the step of mixing a powdered agrochemical with a first liquid component as a raw material for a thermosetting resin; subsequently used as a raw material for a thermosetting resin the step of adding the second liquid component therein; and the step of reacting the first liquid component with the second liquid component to form a thermosetting resin.

在本发明的生产方法中,第一液体组分和第二液体组分的粘度通常等于或小于2000mPa·s。In the production method of the present invention, the viscosities of the first liquid component and the second liquid component are generally equal to or less than 2000 mPa·s.

当热固性树脂是氨基甲酸酯树脂时,多元醇的粘度等于或小于1000mPa·s,更优选等于或小于800mPa·s(B型粘度计,25℃,12rpm),并且聚异氰酸酯的粘度等于或小于300mPa·s,更优选等于或小于200mPa·s(B型粘度计,25℃,12rpm)。When the thermosetting resin is a urethane resin, the viscosity of the polyol is equal to or less than 1000 mPa·s, more preferably equal to or less than 800 mPa·s (B-type viscometer, 25°C, 12 rpm), and the viscosity of the polyisocyanate is equal to or less than 300 mPa·s, more preferably equal to or less than 200 mPa·s (B-type viscometer, 25° C., 12 rpm).

通常通过将第一液体组分加入到容器中,同时在干燥条件下在容器中碾压粉末状农药,进行将粉末状农药与作为用于热固性树脂的原料的第一液体组分混合的步骤,其中不将粉末状农药分散于液体介质中。这个步骤通常在0至100℃,优选在10至80℃进行。出于安全性的观点,该步骤优选在氮气气氛下进行。作为在容器中碾压粉末状农药的方法,提及的有:例如a)其中使容纳有粉末状农药的盘型或滚筒型容器绕倾斜或水平轴旋转的方法;b)其中在容纳有粉末状农药的容器中,安置尺寸与容器的底部的直径大致相同的搅拌叶片并且使其旋转的方法;和c)其中在容纳有粉末状农药的容器中,通过空气流碾压粉末状农药的方法。The step of mixing the powdered pesticide with the first liquid component as a raw material for the thermosetting resin is usually performed by adding the first liquid component to the container while rolling the powdered pesticide in the container under dry conditions, Wherein the powdered pesticide is not dispersed in the liquid medium. This step is usually carried out at 0 to 100°C, preferably at 10 to 80°C. From the viewpoint of safety, this step is preferably performed under a nitrogen atmosphere. As a method of rolling powdered pesticides in a container, there are mentioned, for example: a) a method in which a pan-type or a drum-shaped container containing powdered pesticides is rotated about an inclined or horizontal axis; b) a method in which powdery pesticides are housed In a container containing powdery pesticides, a method of arranging and rotating a stirring blade whose size is approximately the same as the diameter of the bottom of the container; and c) a method wherein, in a container containing powdery pesticides, the powdery pesticides are crushed by air flow .

将作为用于热固性树脂的原料的第二液体组分加入其中的随后步骤也在0至100℃,优选在10至80℃进行。出于安全性的观点,该步骤优选在氮气气氛下进行。基于1当量第一液体组分,以通常为0.9至1.05当量,优选0.95至1.00当量的比例使用第二液体组分。The subsequent step of adding thereto the second liquid component as a raw material for the thermosetting resin is also performed at 0 to 100°C, preferably at 10 to 80°C. From the viewpoint of safety, this step is preferably performed under a nitrogen atmosphere. The second liquid component is used in a proportion of usually 0.9 to 1.05 equivalent, preferably 0.95 to 1.00 equivalent, based on 1 equivalent of the first liquid component.

如果热固性树脂是聚氨酯树脂并且第一液体组分是多元醇,那么第二液体组分是聚异氰酸酯,并且有利的是适当地调节聚异氰酸酯的量,使得聚异氰酸酯基于异氰酸酯基(NCO)的量相对于1当量基于羟基(OH)的多元醇为0.8至1.1当量,优选为0.9至1.1当量,更优选为0.95至1.05当量。If the thermosetting resin is polyurethane resin and the first liquid component is polyol, the second liquid component is polyisocyanate, and it is advantageous to adjust the amount of polyisocyanate appropriately so that the amount of polyisocyanate based on isocyanate groups (NCO) is relatively The polyol based on hydroxyl group (OH) is 0.8 to 1.1 equivalents, preferably 0.9 to 1.1 equivalents, more preferably 0.95 to 1.05 equivalents to 1 equivalent.

使第一液体组分和第二液体组分反应以加工热固性树脂的步骤也通常在0至100℃,优选在40至80℃进行。出于安全性的观点,该步骤优选在氮气气氛下进行。在该步骤中,优选进行混合,同时通过旋转叶片对粉末状农药给予剪切力。更特别提到的有:通过以50至3000m/分钟,优选100至2000m/分钟,更优选200至1000m/分钟的速度(根据叶片前缘的速度)旋转的叶片,搅拌粉末状农药的方法。通常进行搅拌直至未硬化的热固性树脂完全硬化,并且得到的农药粒剂不表现出粘性。可以根据热固性树脂的种类和过程的温度改变搅拌时间。The step of reacting the first liquid component and the second liquid component to process the thermosetting resin is also generally carried out at 0 to 100°C, preferably at 40 to 80°C. From the viewpoint of safety, this step is preferably performed under a nitrogen atmosphere. In this step, mixing is preferably performed while imparting shear force to the powdered pesticide by rotating blades. More particularly mentioned is the method of agitating the powdered pesticide by means of blades rotating at a speed of 50 to 3000 m/min, preferably 100 to 2000 m/min, more preferably 200 to 1000 m/min (according to the speed of the leading edge of the blade). Stirring is usually carried out until the unhardened thermosetting resin is completely hardened and the resulting pesticide granules do not exhibit stickiness. The stirring time can be changed according to the kind of thermosetting resin and the temperature of the process.

向如上所述获得的农药粒剂中,另外在必要时,将第一液体组分和第二液体组分同时或依次加入,并且使这些组分反应以生成热固性树脂,并且将该步骤进行一次或重复几次以增加由热固性树脂制成的包覆层的厚度,并且促进颗粒的相互凝聚,从而可以延迟活性成分的放出。即,可以根据目的调节活性成分的放出速度。To the pesticide granules obtained as described above, if necessary, the first liquid component and the second liquid component are added simultaneously or sequentially, and these components are reacted to generate a thermosetting resin, and this step is performed once Or repeat several times to increase the thickness of the coating layer made of thermosetting resin, and promote the mutual aggregation of the particles, so that the release of the active ingredient can be delayed. That is, the release rate of the active ingredient can be adjusted according to the purpose.

基于100重量份粉末状农药,未固化的热固性树脂的加入量,即第一液体组分和第二液体组分的总量通常为5至150重量份,优选为10至100重量份,更优选为25至80重量份。Based on 100 parts by weight of powdered pesticide, the added amount of uncured thermosetting resin, that is, the total amount of the first liquid component and the second liquid component is usually 5 to 150 parts by weight, preferably 10 to 100 parts by weight, more preferably 25 to 80 parts by weight.

作为在本发明的生产方法中使用的具体容器,提及的有:由SeishinKigyo K.K.生产的NEWGRAMACHINE,作为其中颗粒在容器中表现出沿其外围的圆周运动的装置;以及由Fukae Powtec K.K.生产的HIGH SPEEDMIXER和HIGH FLEX GRAR,作为配备有在混合器中的低转速搅拌器和在侧面上的高转速切碎机的装置,其中通过两个叶片的作用将装入的原料在短时间内混合、分散并且剪切。此外,提及的有:由Freund Sangyo K.K.生产的HIGH SPEED MIXER、由Powrex K.K.生产的VERTICALGRANULATOR、由Okada Seiko K.K.生产的NEW SPEED MILL,作为表现出相同功能的装置。As specific containers used in the production method of the present invention, mentioned are: NEWGRAMACHINE produced by SeishinKigyo K.K. as a device in which particles exhibit circular motion along its periphery in the container; and HIGH produced by Fukae Powtec K.K. SPEEDMIXER and HIGH FLEX GRAR, as a device equipped with a low-speed stirrer in the mixer and a high-speed chopper on the side, where the charged raw materials are mixed, dispersed in a short time by the action of two blades And cut. In addition, HIGH SPEED MIXER produced by Freund Sangyo K.K., VERTICALGRANULATOR produced by Powrex K.K., NEW SPEED MILL produced by Okada Seiko K.K. are mentioned as devices exhibiting the same function.

此外,还可以使用在JP 9-75703A中描述的装置。In addition, the device described in JP 9-75703A can also be used.

在本发明的生产方法中,无需使用溶剂如水等,因此干燥操作等不是必需的,所以可以容易地生产含有处于可控释放方式的农药活性成分的农药粒剂。In the production method of the present invention, there is no need to use a solvent such as water, etc., and therefore drying operations, etc. are not necessary, so that the agricultural chemical granule containing the active ingredient of the agricultural chemical in a controlled release manner can be easily produced.

可以将本发明的农药粒剂直接喷射到将要被控制的害虫上或将要被保护的植物或土壤中,或用水稀释,并且在必要时加入助剂如表面活性剂等以得到悬浮液,并且喷射悬浮液。The pesticide granules of the present invention can be sprayed directly onto the pests to be controlled or to the plants or soil to be protected, or diluted with water, and if necessary, add adjuvants such as surfactants etc. to obtain a suspension, and spray suspension.

实施例Example

将通过下列实施例进一步详细说明本发明,但是本发明不限于这些实施例。The present invention will be further explained in detail by the following examples, but the present invention is not limited to these examples.

在下列生产实施例中,使用HIGH SPEED MIXER装置(LFS-GS-1J型,由Fukae Powtec K.K.生产)。In the following production examples, a HIGH SPEED MIXER device (LFS-GS-1J type, produced by Fukae Powtec K.K.) was used.

HIGH SPEED MIXER装置是搅拌装置,其具有:在上部具有开口的水平圆盘型容器部分;搅拌桨,所述搅拌叶片围绕作为通过水平圆盘型容器部分的底部中心的轴的垂直线旋转;和切碎叶片,所述切碎叶片围绕作为穿过所述容器部分的侧面的轴的水平线旋转,其中所述容器部分具有约2L的容积和约18cm的内径,并且搅拌叶片由三个叶片组成,所述三个叶片具有约为9cm的半径并且连接到底面上,使得三个叶片可以沿着容器部分的底面和内壁旋转。切碎叶片具有两对孪生叶片,所述孪生叶片具有2cm的半径并且旋转式连接到容器部分的侧壁面上,以不与该容器部分的底面和搅拌叶片接触。The HIGH SPEED MIXER device is a stirring device having: a horizontal disc-shaped container part having an opening at an upper part; a stirring blade rotating around a vertical line as an axis passing through the bottom center of the horizontal disc-shaped container part; and A chopping blade that rotates around a horizontal line that is an axis passing through the side of the container portion having a volume of about 2 L and an inner diameter of about 18 cm, and the stirring blade is composed of three blades, so The three blades have a radius of about 9 cm and are connected to the bottom surface so that the three blades can rotate along the bottom surface and the inner wall of the container part. The chopping blades had two pairs of twin blades having a radius of 2 cm and were rotatably attached to the side wall surface of the container part so as not to be in contact with the bottom surface of the container part and the stirring blades.

参考实施例1(粉末状农药1的制备)Reference example 1 (preparation of powdery pesticide 1)

将45.5重量份作为农药活性成分的5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺(常用名:呋吡菌胺(furametpyr))和9重量份TOKUSEAL GU-N(由Tokuyama Soda Co.,Ltd.生产的无定形二氧化硅水合物)以及45.5重量份作为稀释剂的膨润土FUJI(由Hojun K.K.生产)均匀地混合,并且通过离心粉碎机将混合物全部粉碎,以得到平均粒径为5.0μm(通过由MALVERN生产的MASTERSIZER 2000测量)的粉末状农药1。45.5 parts by weight of 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4-isobenzofuryl)-1,3-dimethylpyridine as a pesticide active ingredient Azole-4-carboxamide (common name: furametpyr) and 9 parts by weight of TOKUSEAL GU-N (amorphous silica hydrate produced by Tokuyama Soda Co., Ltd.) and 45.5 parts by weight as Bentonite FUJI (manufactured by Hojun K.K.) of the diluent was uniformly mixed, and the whole mixture was pulverized by a centrifugal pulverizer to obtain powdered pesticide 1 with an average particle diameter of 5.0 μm (measured by MASTERSIZER 2000 produced by MALVERN).

参考实施例2(粉末状农药2的制备)Reference example 2 (preparation of powdery pesticide 2)

将65重量份作为农药活性成分的(E)-N-(6-氯-3-吡啶基甲基)-N-乙基-N’-甲基-2-硝基亚乙烯基二胺(常用名:烯啶虫胺)和35重量份作为稀释剂的SHOKOZAN Clay S(高岭粘土:由Shokozan Kogyosho K.K.生产)均匀地混合,并且通过离心粉碎机将混合物全部粉碎,以得到平均粒径为1 6.0μm(通过由MALVERN生产的MASTERSIZER 2000测量)的粉末状农药2。With 65 parts by weight of (E)-N-(6-chloro-3-pyridylmethyl)-N-ethyl-N'-methyl-2-nitroethylenediamine (commonly used Name: Nitenpyram) and 35 parts by weight of SHOKOZAN Clay S (kaolin clay: produced by Shokozan Kogyosho K.K.) as a diluent were uniformly mixed, and the whole mixture was pulverized by a centrifugal mill to obtain an average particle diameter of 1 6.0 μm (measured by MASTERSIZER 2000 manufactured by MALVERN) of powdered pesticide 2.

参考实施例3(多元醇预混合物1的制备)Reference example 3 (preparation of polyol premix 1)

将54.1重量份SUMIFEN TM(由Sumika Bayer Urethane K.K.生产的支链聚醚多元醇)和45.9重量份SUMIFEN 1600U(由Sumika Bayer UrethaneK.K.生产的直链聚醚多元醇)均匀地混合以得到多元醇预混合物1。多元醇预混合物1的粘度为393 m·Pa(B型粘度计,25℃,12rpm,Rotor No.1)。54.1 parts by weight of SUMIFEN™ (branched polyether polyol produced by Sumika Bayer Urethane K.K.) and 45.9 parts by weight of SUMIFEN 1600U (linear polyether polyol produced by Sumika Bayer Urethane K.K.) were uniformly mixed to obtain a polyol Alcohol Premix 1. The viscosity of polyol premix 1 is 393 m Pa (B-type viscometer, 25°C, 12rpm, Rotor No.1).

参考实施例4(多元醇预混合物2的制备)Reference Example 4 (preparation of polyol premix 2)

将41.3重量份SUMIFEN TM(由Sumika Bayer Urethane K.K.生产的支链聚醚多元醇)和58.7重量份SUMIFEN 1600U(由Sumika Bayer UrethaneK.K.生产的直链聚醚多元醇)均匀地混合以得到多元醇预混合物2。多元醇预混合物2的粘度为282m·Pa(B型粘度计,25℃,12rpm,Rotor No.1)。参考实施例5(多元醇预混合物3的制备)41.3 parts by weight of SUMIFEN™ (branched polyether polyol produced by Sumika Bayer Urethane K.K.) and 58.7 parts by weight of SUMIFEN 1600U (linear polyether polyol produced by Sumika Bayer Urethane K.K.) were uniformly mixed to obtain a polyol Alcohol Premix 2. The viscosity of the polyol premixture 2 is 282 m·Pa (B-type viscometer, 25° C., 12 rpm, Rotor No.1). Reference Example 5 (preparation of polyol premix 3)

将31.2重量份SUMIFEN TM(由Sumika Bayer Urethane K.K.生产的支链聚醚多元醇)和68.8重量份SUMIFEN 1600U(由Sumika Bayer UrethaneK.K.生产的直链聚醚多元醇)均匀地混合以得到多元醇预混合物3。多元醇预混合物3的粘度为277m·Pa(B型粘度计,25℃,12rpm,Rotor No.1)。参考实施例6(多元醇预混合物4的制备)31.2 parts by weight of SUMIFEN™ (a branched polyether polyol produced by Sumika Bayer Urethane K.K.) and 68.8 parts by weight of SUMIFEN 1600U (a linear polyether polyol produced by Sumika Bayer Urethane K.K.) were uniformly mixed to obtain a polyol Alcohol Premix 3. The viscosity of the polyol premixture 3 is 277mPa (B-type viscometer, 25°C, 12rpm, Rotor No.1). Reference Example 6 (preparation of polyol premix 4)

将19.9重量份1,2-亚乙基二醇(由Nippon Shokubai Co.,Ltd.生产)和80.1重量份SUMIFEN 1600U(由Sumika Bayer Urethane K.K.生产的直链聚醚多元醇)均匀地混合以得到多元醇预混合物4。多元醇预混合物4的粘度为176m·Pa(B型粘度计,25℃,12rpm,Rotor No.1)。19.9 parts by weight of 1,2-ethylene glycol (produced by Nippon Shokubai Co., Ltd.) and 80.1 parts by weight of SUMIFEN 1600U (a linear polyether polyol produced by Sumika Bayer Urethane K.K.) were uniformly mixed to obtain Polyol Premix 4. The viscosity of the polyol premixture 4 is 176 m·Pa (B-type viscometer, 25° C., 12 rpm, Rotor No.1).

生产实施例1Production Example 1

将100重量份粉末状农药1装入到上述HIGH SPEED MIXER装置的容器中,并且使搅拌叶片(转速:1800rpm)和切碎叶片(转速:2000rpm)旋转。在该装置中,通过全部在碾压状态下的搅拌器搅拌粉末状农药,并且主要通过切碎叶片将强剪切力施加到粉末状农药上。接着,将容器加热,并且加入1.55重量份多元醇预混合物1,同时将粉末状农药的温度保持在75±5℃。观察到多元醇预混合物1渗透到粉末状农药中的情景。三分钟后,加入0.95重量份聚异氰酸酯{SUMIDUL 44V10(由Sumika Bayer UrethaneK.K.生产的聚亚甲基聚苯基聚异氰酸酯),粘度:130m·Pa(25℃)},同时将粉末状农药的温度保持在75±5℃。在刚加入之后,增稠现象得到证实,之后粘度降低,并且观察到聚氨酯树脂的硬化(相对于100重量份粉末状农药,对应于2.5重量份聚氨酯树脂)。100 parts by weight of the powdered pesticide 1 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 1800rpm) and the chopping blade (rotational speed: 2000rpm) were rotated. In this device, powdered pesticides are stirred by agitators all in a rolling state, and strong shearing force is applied to the powdered pesticides mainly by chopping blades. Next, the container was heated, and 1.55 parts by weight of polyol premix 1 was added while maintaining the temperature of the powdered pesticide at 75±5°C. The penetration of the polyol premix 1 into the powdered pesticide was observed. Three minutes later, add 0.95 parts by weight of polyisocyanate {SUMIDUL 44V10 (polymethylene polyphenyl polyisocyanate produced by Sumika Bayer Urethane K.K.), viscosity: 130m Pa (25°C)}, and simultaneously powdered pesticide The temperature is maintained at 75±5°C. Immediately after the addition, a thickening phenomenon was confirmed, after which the viscosity decreased, and hardening of the polyurethane resin was observed (corresponding to 2.5 parts by weight of the polyurethane resin with respect to 100 parts by weight of the powdered pesticide).

此外,5分钟后,将1)加入1.55重量份多元醇预混合物1、2)继续搅拌并且混合3分钟、3)加入0.95重量份聚异氰酸酯和4)继续搅拌并且混合5分钟的操作重复3次,同时继续搅拌,将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 1.55 parts by weight of polyol premix 1, 2) continuing to stir and mix for 3 minutes, 3) adding 0.95 parts by weight of polyisocyanate and 4) continuing to stir and mixing for 5 minutes was repeated 3 times , while continuing to stir, the temperature in the HIGH SPEED MIXER device was kept at 75±5°C, after that, the mixture was allowed to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药为10重量份的聚氨酯树脂原料(氨基甲酸酯树脂原料的添加频率:4次;每次添加的氨基甲酸酯树脂原料的添加量:2.5重量份;氨基甲酸酯树脂原料的总添加量:10重量份),获得本发明的农药粒剂。Therefore, the total amount of polyurethane resin raw materials used is 10 parts by weight relative to 100 parts by weight of powdered pesticide (addition frequency of urethane resin raw materials: 4 times; addition amount of urethane resin raw materials added each time: 2.5 parts by weight; the total amount of urethane resin raw material added: 10 parts by weight), to obtain the pesticide granule of the present invention.

生产实施例2至6Production Examples 2 to 6

根据与生产实施例1中相同的过程,通过以每次添加为2.5重量份的量、表1中所述的添加频率添加氨基甲酸酯树脂原料,获得本发明的农药粒剂。According to the same procedure as in Production Example 1, the pesticide granules of the present invention were obtained by adding the urethane resin raw material in an amount of 2.5 parts by weight per addition at the addition frequency described in Table 1.

表1Table 1

粉末状农药1(重量份)Powdered pesticide 1 (parts by weight) 每次添加的树脂原料(*)添加量(重量份)Resin raw material added each time ( * ) added amount (parts by weight) 树脂原料的添加频率(*)Addition frequency of resin raw materials ( * ) 树脂原料的总添加量(重量份)The total addition amount of resin raw material (weight part) 生产实施例1Production Example 1 100100 2.52.5 4次4 times 1010 生产实施例2Production Example 2 100100 2.52.5 8次8 times 2020 生产实施例3Production Example 3 100100 2.52.5 12次12 times 3030 生产实施例4Production Example 4 100100 2.52.5 16次16 times 4040 生产实施例5Production Example 5 100100 2.52.5 20次20 times 5050 生产实施例6Production Example 6 100100 2.52.5 22次22 times 5555

(*)树脂原料指氨基甲酸酯树脂原料,并且其量为多元醇预混合物和聚异氰酸酯之和。( * ) Resin raw material refers to urethane resin raw material, and its amount is the sum of polyol premix and polyisocyanate.

试验实施例1Test Example 1

1)平均粒径的测量1) Measurement of average particle size

通过由MALVERN生产的MASTERSIZER 2000测量在生产实施例1至6中获得的本发明的农药粒剂的体积中值直径。结果示于表2中。The volume median diameters of the pesticide granules of the present invention obtained in Production Examples 1 to 6 were measured by MASTERSIZER 2000 produced by MALVERN. The results are shown in Table 2.

2)洗脱试验2) Elution test

将粉末状农药1和在生产实施例1至6中获得的本发明的农药粒剂以根据5-氯-N=(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺为5mg的量装入100mL螺旋管中,并且将200g离子交换水加入其中,并且使混合物在25℃的恒温室中保持24小时。之后,通过过滤器过滤出固体组分,并且测量洗脱到水中的5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺的量,并且计算洗脱到水中的比例(洗脱率)。结果示于表2中。The powdery pesticide 1 and the pesticide granules of the present invention obtained in Production Examples 1 to 6 were prepared according to 5-chloro-N=(1,3-dihydro-1,1,3-trimethyl-4- An amount of 5 mg of isobenzofuryl)-1,3-dimethylpyrazole-4-carboxamide was charged into a 100 mL spiral tube, and 200 g of ion-exchanged water was added thereto, and the mixture was placed in a constant temperature room at 25° C. Keep for 24 hours. After that, the solid component was filtered through a filter, and 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4-isobenzofuranyl) eluted into water was measured - the amount of 1,3-dimethylpyrazole-4-carboxamide, and the ratio eluted into water (elution rate) was calculated. The results are shown in Table 2.

表2Table 2

体积中值直径(μm)Volume median diameter (μm) 洗脱率(%)Elution rate (%) 在1天后in 1 day 在3天后in 3 days 粉末状农药1powdered pesticide 1 5.05.0 8585 100100 生产实施例1Production Example 1 34.734.7 8080 9090 生产实施例2Production Example 2 36.936.9 7474 8888 生产实施例3Production Example 3 40.940.9 4545 8080 生产实施例4Production Example 4 43.143.1 4141 7373 生产实施例5Production Example 5 44.844.8 3939 6969 生产实施例6Production Example 6 45.045.0 3636 5656

生产实施例7Production Example 7

将100重量份粉末状农药2装入上述HIGH SPEED MIXER装置的容器中,并且使该装置的搅拌叶片(转速:1800rpm)和切碎叶片(转速:2000rpm)旋转。在该装置中,通过全部处于碾压状态下的搅拌器搅拌粉末状农药,并且主要通过切碎叶片将强剪切力施加到粉末状农药上。接着,将容器加热,并且加入1.55重量份多元醇预混合物1,同时将粉末状农药的温度保持在75±5℃。观察到多元醇预混合物1渗透到粉末状农药中的情景。三分钟后,加入0.95重量份聚异氰酸酯{SUMIDUL 44V10(由Sumika BayerUrethane K.K.生产的聚亚甲基聚苯基聚异氰酸酯)},同时将粉末状农药的温度保持在75±5℃。在刚加入之后,增稠现象得到证实,之后粘度降低,并且观察到聚氨酯树脂的硬化(相对于100重量份粉末状农药,对应于2.5重量份聚氨酯树脂)。100 parts by weight of the powdered pesticide 2 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 1800rpm) and the chopping blade (rotational speed: 2000rpm) of the device were rotated. In this device, powdered pesticides are stirred by agitators all in a rolling state, and strong shearing force is applied to the powdered pesticides mainly by chopping blades. Next, the container was heated, and 1.55 parts by weight of polyol premix 1 was added while maintaining the temperature of the powdered pesticide at 75±5°C. The penetration of the polyol premix 1 into the powdered pesticide was observed. Three minutes later, 0.95 parts by weight of polyisocyanate {SUMIDUL 44V10 (polymethylene polyphenyl polyisocyanate produced by Sumika BayerUrethane K.K.)} was added while maintaining the temperature of the powdered pesticide at 75±5°C. Immediately after the addition, a thickening phenomenon was confirmed, after which the viscosity decreased, and hardening of the polyurethane resin was observed (corresponding to 2.5 parts by weight of the polyurethane resin relative to 100 parts by weight of the powdered pesticide).

此外,5分钟后,将1)加入1.55重量份多元醇预混合物1、2)继续搅拌并且混合3分钟、3)加入0.95重量份聚异氰酸酯和4)继续搅拌并且混合5分钟的操作重复19次,同时继续搅拌,将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 1.55 parts by weight of polyol premix 1, 2) continuing to stir and mix for 3 minutes, 3) adding 0.95 parts by weight of polyisocyanate and 4) continuing to stir and mixing for 5 minutes was repeated 19 times , while continuing to stir, the temperature in the HIGH SPEED MIXER device was kept at 75±5°C, after that, the mixture was allowed to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药2为50重量份的聚氨酯树脂原料(氨基甲酸酯树脂原料的添加频率:20次;每次添加的氨基甲酸酯树脂原料的添加量:2.5重量份;氨基甲酸酯树脂原料的总添加量:50重量份),获得本发明的农药粒剂。Therefore, the total amount used is 50 parts by weight of the polyurethane resin raw material relative to 100 parts by weight of the powdered pesticide 2 (addition frequency of the urethane resin raw material: 20 times; the addition amount of the urethane resin raw material added each time: 2.5 parts by weight; the total addition amount of the urethane resin raw material: 50 parts by weight), to obtain the pesticide granule of the present invention.

生产实施例8至11Production Examples 8 to 11

根据与在生产实施例7中相同的步骤,通过以每次添加为2.5重量份的量、表3中所述的添加频率添加氨基甲酸酯树脂原料获得本发明的农药粒剂。According to the same procedure as in Production Example 7, the pesticide granules of the present invention were obtained by adding the urethane resin raw material in an amount of 2.5 parts by weight per addition at the addition frequency described in Table 3.

表3table 3

粉末状粒剂2(重量份)Powdered granules 2 (parts by weight) 每次添加的树脂原料(*)的添加量(重量份)Addition amount (parts by weight) of resin raw material ( * ) added each time 树脂原料(*)的添加频率Addition frequency of resin raw material ( * ) 树脂原料(*)的总添加量(重量份)Total amount of resin raw materials ( * ) added (parts by weight) 生产实施例7Production Example 7 100100 2.52.5 20次20 times 5050 生产实施例8Production Example 8 100100 2.52.5 24次24 times 6060 生产实施例9Production Example 9 100100 2.52.5 28次28 times 7070 生产实施例10Production Example 10 100100 2.52.5 32次32 times 8080 生产实施例11Production Example 11 100100 2.52.5 40次40 times 100100

(*)树脂原料指氨基甲酸酯树脂原料,并且其量为多元醇预混合物和聚异氰酸酯之和。( * ) Resin raw material refers to urethane resin raw material, and its amount is the sum of polyol premix and polyisocyanate.

试验实施例2Test Example 2

1)平均粒径的测量1) Measurement of average particle size

通过由MALVERN生产的MASTERSIZER 2000测量在生产实施例7至11中获得的本发明的农药粒剂的体积中值直径。结果示于表4中。The volume median diameters of the pesticide granules of the present invention obtained in Production Examples 7 to 11 were measured by MASTERSIZER 2000 produced by MALVERN. The results are shown in Table 4.

2)洗脱试验2) Elution test

将粉末状农药和在生产实施例7至11中获得的本发明的农药粒剂以根据(E)-N-(6-氯-3-吡啶基甲基)-N-乙基-N’-甲基-2-硝基亚乙烯基二胺为5mg的量装入100mL螺旋管中,并且将100g离子交换水加入其中,并且使混合物在25℃的恒温室中保持24小时。之后,通过过滤器过滤固体组分,并且测量洗脱到水中的(E)-N-(6-氯-3-吡啶基甲基)-N-乙基-N’-甲基-2-硝基亚乙烯基二胺的量,并且计算洗脱到水中的比例(洗脱率)。结果示于表4中。Powdered pesticides and pesticide granules of the present invention obtained in Production Examples 7 to 11 were prepared according to (E)-N-(6-chloro-3-pyridylmethyl)-N-ethyl-N'- An amount of 5 mg of methyl-2-nitroethylenediamine was charged into a 100 mL spiral tube, and 100 g of ion-exchanged water was added thereto, and the mixture was kept in a constant temperature room at 25° C. for 24 hours. After that, the solid component was filtered through a filter, and (E)-N-(6-chloro-3-pyridylmethyl)-N-ethyl-N'-methyl-2-nitrate eluted into water was measured The amount of vinylidene diamine was calculated, and the ratio eluted into water (elution rate) was calculated. The results are shown in Table 4.

表4Table 4

体积中值直径(μm)Volume median diameter (μm) 洗脱率(%)Elution rate (%) 在1天后in 1 day 在3天后in 3 days 粉末农药2Powder Pesticide 2 16.016.0 100100 100100 生产实施例7Production Example 7 53.353.3 8686 9090 生产实施例8Production Example 8 52.352.3 7777 8484 生产实施例9Production Example 9 57.457.4 23twenty three 5151 生产实施例10Production Example 10 57.957.9 1212 23twenty three 生产实施例11Production Example 11 61.561.5 33 55

生产实施例12Production Example 12

将100重量份粉末状农药1装入上述HIGH SPEED MIXER装置的容器中,并且使该装置的搅拌叶片(转速:850rpm)和切碎叶片(转速:2000rpm)旋转。接着,将容器加热,并且加入1.55重量份多元醇预混合物1,同时将粉末状农药的温度保持在75±5℃。三分钟后,加入0.95重量份聚异氰酸酯{SUMIDUL 44V10(由Sumika Bayer Urethane K.K.生产的聚亚甲基聚苯基聚异氰酸酯)},同时将粉末状农药的温度保持在75±5℃。(相对于100重量份粉末状农药,对应于2.5重量份聚氨酯树脂)。100 parts by weight of the powdered pesticide 1 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 850rpm) and the chopping blade (rotational speed: 2000rpm) of the device were rotated. Next, the container was heated, and 1.55 parts by weight of polyol premix 1 was added while maintaining the temperature of the powdered pesticide at 75±5°C. Three minutes later, 0.95 parts by weight of polyisocyanate {SUMIDUL 44V10 (polymethylene polyphenyl polyisocyanate produced by Sumika Bayer Urethane K.K.)} was added while maintaining the temperature of the powdered pesticide at 75±5°C. (corresponding to 2.5 parts by weight of polyurethane resin relative to 100 parts by weight of powdered pesticide).

此外,5分钟后,将1)加入1.55重量份多元醇预混合物1、2)继续搅拌并且混合3分钟、3)加入0.95重量份聚异氰酸酯和4)继续搅拌并且混合5分钟的操作重复19次,同时继续搅拌,将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 1.55 parts by weight of polyol premix 1, 2) continuing to stir and mix for 3 minutes, 3) adding 0.95 parts by weight of polyisocyanate and 4) continuing to stir and mixing for 5 minutes was repeated 19 times , while continuing to stir, the temperature in the HIGH SPEED MIXER device was kept at 75±5°C, after that, the mixture was allowed to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药为50重量份的聚氨酯树脂原料(氨基甲酸酯树脂原料的添加频率:20次;每次添加的氨基甲酸酯树脂原料的添加量:2.5重量份;氨基甲酸酯树脂原料的总添加量:50重量份),获得本发明的农药粒剂。Therefore, the total amount of polyurethane resin raw materials used is 50 parts by weight relative to 100 parts by weight of powdered pesticide (addition frequency of urethane resin raw materials: 20 times; addition amount of urethane resin raw materials added each time: 2.5 parts by weight; the total amount of urethane resin raw materials added: 50 parts by weight), to obtain the pesticide granules of the present invention.

得到的农药粒剂具有比在生产实施例5中获得的本发明的农药粒剂更大的平均粒径。The obtained pesticide granules had a larger average particle diameter than the pesticide granules of the present invention obtained in Production Example 5.

生产实施例13Production Example 13

将100重量份粉末状农药1装入上述HIGH SPEED MIXER装置的容器中,并且使该装置的搅拌叶片(转速:1800rpm)和切碎叶片(转速:2000 rpm)旋转。接着,将混合容器加热,并且加入1.65重量份多元醇预混合物2,同时将粉末状农药的温度保持在75±5℃。三分钟后,加入0.85重量份聚异氰酸酯{SUMIDUL 44V10(由Sumika Bayer Urethane K.K.生产的聚亚甲基聚苯基聚异氰酸酯)},同时将粉末状农药的温度保持在75±5℃。(相对于100重量份粉末状农药,对应于2.5重量份聚氨酯树脂)。100 parts by weight of the powdered pesticide 1 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 1800rpm) and the chopping blade (rotational speed: 2000rpm) of the device were rotated. Next, the mixing vessel was heated, and 1.65 parts by weight of polyol premix 2 was added while maintaining the temperature of the powdered pesticide at 75±5°C. Three minutes later, 0.85 parts by weight of polyisocyanate {SUMIDUL 44V10 (polymethylene polyphenyl polyisocyanate produced by Sumika Bayer Urethane K.K.)} was added while maintaining the temperature of the powdered pesticide at 75±5°C. (corresponding to 2.5 parts by weight of polyurethane resin relative to 100 parts by weight of powdered pesticide).

此外,5分钟后,将1)加入1.65重量份多元醇预混合物2、2)继续搅拌并且混合3分钟、3)加入0.85重量份聚异氰酸酯和4)继续搅拌并且混合5分钟的操作重复19次,同时继续搅拌,将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 1.65 parts by weight of polyol premix 2, 2) continuing to stir and mix for 3 minutes, 3) adding 0.85 parts by weight of polyisocyanate and 4) continuing to stir and mixing for 5 minutes was repeated 19 times , while continuing to stir, the temperature in the HIGH SPEED MIXER device was kept at 75±5°C, after that, the mixture was allowed to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药为50重量份的聚氨酯树脂原料(氨基甲酸酯树脂原料的添加频率:20次;每次添加的氨基甲酸酯树脂原料的添加量:2.5重量份;氨基甲酸酯树脂原料的总添加量:50重量份),获得本发明的农药粒剂。Therefore, the total amount of polyurethane resin raw materials used is 50 parts by weight relative to 100 parts by weight of powdered pesticide (addition frequency of urethane resin raw materials: 20 times; addition amount of urethane resin raw materials added each time: 2.5 parts by weight; the total amount of urethane resin raw materials added: 50 parts by weight), to obtain the pesticide granules of the present invention.

与在生产实施例5中获得的本发明的农药粒剂相比,得到的农药粒剂提供5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺的更快的洗脱。Compared with the pesticide granules of the present invention obtained in Production Example 5, the obtained pesticide granules provided 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4- faster elution of isobenzofuryl)-1,3-dimethylpyrazole-4-carboxamide.

生产实施例14Production Example 14

将100重量份粉末状农药1装入上述HIGH SPEED MIXER装置的容器中,并且使该装置的搅拌叶片(转速:1800rpm)和切碎叶片(转速:2000rpm)旋转。接着,将混合容器加热,并且加入1.71重量份多元醇预混合物3,同时将粉末状农药的温度保持在75±5℃。三分钟后,加入0.79重量份聚异氰酸酯{SUMIDUL 44V10(由Sumika Bayer Urethane K.K.生产的聚亚甲基聚苯基聚异氰酸酯)},同时将粉末状农药的温度保持在75±5℃。(相对于100重量份粉末状农药,对应于2.5重量份聚氨酯树脂)。100 parts by weight of the powdered pesticide 1 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 1800rpm) and the chopping blade (rotational speed: 2000rpm) of the device were rotated. Next, the mixing vessel was heated, and 1.71 parts by weight of polyol premix 3 was added while maintaining the temperature of the powdered pesticide at 75±5°C. Three minutes later, 0.79 parts by weight of polyisocyanate {SUMIDUL 44V10 (polymethylene polyphenyl polyisocyanate produced by Sumika Bayer Urethane K.K.)} was added while maintaining the temperature of the powdered pesticide at 75±5°C. (corresponding to 2.5 parts by weight of polyurethane resin relative to 100 parts by weight of powdered pesticide).

此外,5分钟后,将1)加入1.71重量份多元醇预混合物3、2)继续搅拌并且混合3分钟、3)加入0.79重量份聚异氰酸酯和4)继续搅拌并且混合5分钟的操作重复19次,同时继续搅拌,将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 1.71 parts by weight of polyol premix 3, 2) continuing to stir and mix for 3 minutes, 3) adding 0.79 parts by weight of polyisocyanate and 4) continuing to stir and mixing for 5 minutes was repeated 19 times , while continuing to stir, the temperature in the HIGH SPEED MIXER device was kept at 75±5°C, after that, the mixture was allowed to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药为50重量份的聚氨酯树脂原料(氨基甲酸酯树脂原料的添加频率:20次;每次添加的氨基甲酸酯树脂原料的添加量:2.5重量份;氨基甲酸酯树脂原料的总添加量:50重量份),获得本发明的农药粒剂。Therefore, the total amount of polyurethane resin raw materials used is 50 parts by weight relative to 100 parts by weight of powdered pesticide (addition frequency of urethane resin raw materials: 20 times; addition amount of urethane resin raw materials added each time: 2.5 parts by weight; the total amount of urethane resin raw materials added: 50 parts by weight), to obtain the pesticide granules of the present invention.

与在生产实施例5中获得的本发明的农药粒剂相比,得到的农药粒剂提供5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺的更快的洗脱。Compared with the pesticide granules of the present invention obtained in Production Example 5, the obtained pesticide granules provided 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4- faster elution of isobenzofuryl)-1,3-dimethylpyrazole-4-carboxamide.

生产实施例15Production Example 15

将100重量份粉末状农药1装入上述HIGH SPEED MIXER装置的容器中,并且使该装置的搅拌叶片(转速:1800rpm)和切碎叶片(转速:2000rpm)旋转。接着,将混合容器加热,并且加入3.10重量份多元醇预混合物1,同时将粉末状农药的温度保持在75±5℃。三分钟后,加入1.90重量份聚异氰酸酯{SUMIDUL 44V10(由Sumika Bayer Urethane K.K.生产的聚亚甲基聚苯基聚异氰酸酯)},同时将粉末状农药的温度保持在75±5℃。(相对于100重量份粉末状农药,对应于5.0重量份聚氨酯树脂)。100 parts by weight of the powdered pesticide 1 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 1800rpm) and the chopping blade (rotational speed: 2000rpm) of the device were rotated. Next, the mixing vessel was heated, and 3.10 parts by weight of polyol premix 1 was added while maintaining the temperature of the powdered pesticide at 75±5°C. Three minutes later, 1.90 parts by weight of polyisocyanate {SUMIDUL 44V10 (polymethylene polyphenyl polyisocyanate produced by Sumika Bayer Urethane K.K.)} was added while maintaining the temperature of the powdered pesticide at 75±5°C. (corresponding to 5.0 parts by weight of polyurethane resin relative to 100 parts by weight of powdered pesticide).

此外,5分钟后,将1)加入3.10重量份多元醇预混合物1、2)继续搅拌并且混合3分钟、3)加入1.90重量份聚异氰酸酯和4)继续搅拌并且混合5分钟的操作重复19次,同时继续搅拌,从而将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 3.10 parts by weight of polyol premix 1, 2) continuing to stir and mix for 3 minutes, 3) adding 1.90 parts by weight of polyisocyanate and 4) continuing to stir and mixing for 5 minutes was repeated 19 times , while continuing to stir, thereby keeping the temperature in the HIGH SPEED MIXER device at 75±5°C, after that, allowing the mixture to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药为50重量份的聚氨酯树脂原料(氨基甲酸酯树脂原料的添加频率:10次;每次添加的氨基甲酸酯树脂原料的添加量:5.0重量份;氨基甲酸酯树脂原料的总添加量:50重量份),获得本发明的农药粒剂。Therefore, the total amount used is 50 parts by weight of the polyurethane resin raw material relative to 100 parts by weight of the powdered pesticide (addition frequency of the urethane resin raw material: 10 times; addition amount of the urethane resin raw material added each time: 5.0 parts by weight; the total amount of carbamate resin raw materials added: 50 parts by weight), to obtain the pesticide granules of the present invention.

与在生产实施例5中获得的本发明的农药粒剂相比,得到的农药粒剂提供5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺的更慢的洗脱。Compared with the pesticide granules of the present invention obtained in Production Example 5, the obtained pesticide granules provided 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4- (isobenzofuryl)-1,3-dimethylpyrazole-4-carboxamide with slower elution.

生产实施例16Production Example 16

将100重量份粉末状农药1装入上述HIGH SPEED MIXER装置的容器中,并且使该装置的搅拌叶片(转速:1800rpm)和切碎叶片(转速:2000rpm)旋转。接着,将混合容器加热,并且加入1.20重量份多元醇预混合物4,同时将粉末状农药的温度保持在75±5℃。三分钟后,加入1.30重量份聚异氰酸酯{SUMIDUL 44V10(由Sumika Bayer Urethane K.K.生产的聚亚甲基聚苯基聚异氰酸酯)},同时将粉末状农药的温度保持在75±5℃。(相对于100重量份粉末状农药,对应于2.5重量份聚氨酯树脂)。100 parts by weight of the powdered pesticide 1 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 1800rpm) and the chopping blade (rotational speed: 2000rpm) of the device were rotated. Next, the mixing vessel was heated, and 1.20 parts by weight of polyol premix 4 was added while maintaining the temperature of the powdered pesticide at 75±5°C. Three minutes later, 1.30 parts by weight of polyisocyanate {SUMIDUL 44V10 (polymethylene polyphenyl polyisocyanate produced by Sumika Bayer Urethane K.K.)} was added while maintaining the temperature of the powdered pesticide at 75±5°C. (corresponding to 2.5 parts by weight of polyurethane resin relative to 100 parts by weight of powdered pesticide).

此外,5分钟后,将1)加入1.20重量份多元醇预混合物4、2)继续搅拌并且混合3分钟、3)加入1.30重量份聚异氰酸酯和4)继续搅拌并且混合5分钟的操作重复19次,同时继续搅拌,将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 1.20 parts by weight of polyol premix 4, 2) continuing to stir and mix for 3 minutes, 3) adding 1.30 parts by weight of polyisocyanate and 4) continuing to stir and mixing for 5 minutes was repeated 19 times , while continuing to stir, the temperature in the HIGH SPEED MIXER device was kept at 75±5°C, after that, the mixture was allowed to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药为50重量份的聚氨酯树脂原料(氨基甲酸酯树脂原料的添加频率:20次;每次添加的氨基甲酸酯树脂原料的添加量:2.5重量份;氨基甲酸酯树脂原料的总添加量:50重量份),获得本发明的农药粒剂。Therefore, the total amount of polyurethane resin raw materials used is 50 parts by weight relative to 100 parts by weight of powdered pesticide (addition frequency of urethane resin raw materials: 20 times; addition amount of urethane resin raw materials added each time: 2.5 parts by weight; the total amount of urethane resin raw materials added: 50 parts by weight), to obtain the pesticide granules of the present invention.

生产实施例17Production Example 17

将100重量份粉末状农药1装入上述HIGH SPEED MIXER装置的容器中,并且使该装置的搅拌叶片(转速:1800rpm)和切碎叶片(转速:2000rpm)旋转。接着,将混合容器加热,并且加入0.83重量份多胺混合物(E206W硬化剂,由Konishi K.K.生产,粘度:400m·Pa(25℃)),同时将粉末状农药的温度保持在75±5℃。三分钟后,加入1.67重量份聚缩水甘油醚(E206W主试剂,由Konishi K.K.生产,双酚F类环氧主试剂,粘度:500m·Pa(25℃)),同时将粉末状农药的温度保持在75±5℃。(相对于100重量份粉末状农药,对应于2.5重量份环氧树脂)。100 parts by weight of the powdered pesticide 1 was charged into the container of the above-mentioned HIGH SPEED MIXER device, and the stirring blade (rotational speed: 1800rpm) and the chopping blade (rotational speed: 2000rpm) of the device were rotated. Next, the mixing vessel was heated, and 0.83 parts by weight of a polyamine mixture (E206W hardener, produced by Konishi K.K., viscosity: 400 mPa (25°C)) was added while maintaining the temperature of the powdered pesticide at 75±5°C. After three minutes, add 1.67 parts by weight polyglycidyl ether (E206W main reagent, produced by Konishi K.K., bisphenol F epoxy main reagent, viscosity: 500m Pa (25 ℃)), keep the temperature of powdered pesticide simultaneously At 75±5°C. (corresponding to 2.5 parts by weight of epoxy resin relative to 100 parts by weight of powdered pesticide).

此外,5分钟后,将1)加入0.83重量份E206W硬化剂、2)继续搅拌并且混合3分钟、3)加入1.67重量份E206W主试剂和4)继续搅拌并且混合5分钟的操作重复19次,同时继续搅拌,将HIGH SPEED MIXER装置中的温度保持在75±5℃,之后,让混合物冷却以得到本发明的农药粒剂。In addition, after 5 minutes, the operation of 1) adding 0.83 parts by weight of E206W hardener, 2) continuing to stir and mix for 3 minutes, 3) adding 1.67 parts by weight of E206W main agent, and 4) continuing to stir and mix for 5 minutes was repeated 19 times, While continuing to stir, the temperature in the HIGH SPEED MIXER device was maintained at 75±5°C, after which the mixture was allowed to cool to obtain the pesticide granules of the present invention.

因此,使用总量相对于100重量份粉末状农药为50重量份的环氧树脂原料(环氧树脂原料的添加频率:20次;每次添加的环氧树脂原料的添加量:2.5重量份;环氧树脂原料的总添加量:50重量份),获得本发明的农药粒剂。Therefore, use total amount to be the epoxy resin raw material of 50 weight parts (the addition frequency of epoxy resin raw material: 20 times; the addition amount of the epoxy resin raw material that adds every time: 2.5 weight parts; The total addition amount of epoxy resin raw material: 50 weight parts), obtains the pesticide granule of the present invention.

工业适用性Industrial applicability

本发明的农药粒剂能够使农药活性成分得到可控释放。本发明的生产方法能够容易提供含有处于可控释放形式的农药活性成分的农药组合物。The pesticide granule of the invention can control the release of pesticide active ingredients. The production method of the present invention can easily provide an agrochemical composition containing an agrochemical active ingredient in a controlled release form.

Claims (17)

1.一种包覆的农药粒剂,所述农药粒剂通过用热固性树脂使粉末状农药聚集而得到。CLAIMS 1. A coated pesticide granule obtained by aggregating a powdered pesticide with a thermosetting resin. 2.根据权利要求1所述的农药粒剂,其中所述热固性树脂是氨基甲酸酯树脂、尿素树脂或环氧树脂。2. The pesticide granule according to claim 1, wherein the thermosetting resin is a urethane resin, a urea resin or an epoxy resin. 3.根据权利要求1所述的农药粒剂,其中所述热固性树脂是氨基甲酸酯树脂。3. The pesticide granule according to claim 1, wherein the thermosetting resin is a urethane resin. 4.根据权利要求1、2或3所述的农药粒剂,其中所述粉末状农药是包含农药活性成分和稀释剂的组合物。4. The pesticide granule according to claim 1, 2 or 3, wherein the powdered pesticide is a composition comprising a pesticide active ingredient and a diluent. 5.根据权利要求1、2或3所述的农药粒剂,其中所述粉末状农药是包含5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺作为农药活性成分的粉末状农药。5. The pesticide granule according to claim 1, 2 or 3, wherein the powdered pesticide contains 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4 -isobenzofuryl)-1,3-dimethylpyrazole-4-carboxamide as a powdered pesticide as a pesticide active ingredient. 6.根据权利要求5所述的农药粒剂,其中所述粉末状农药是包含5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺作为农药活性成分和稀释剂的粉末状农药。6. The pesticide granule according to claim 5, wherein the powdered pesticide contains 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4-isobenzone Furyl)-1,3-dimethylpyrazole-4-carboxamide as a powdered pesticide as a pesticide active ingredient and diluent. 7.根据权利要求1、2或3所述的农药粒剂,其中所述粉末状农药是包含(E)-N-(6-氯-3-吡啶基甲基)-N-乙基-N’-甲基-2-硝基亚乙烯基二胺作为农药活性成分的粉末状农药。7. The pesticide granule according to claim 1, 2 or 3, wherein the powdered pesticide comprises (E)-N-(6-chloro-3-pyridylmethyl)-N-ethyl-N '-Methyl-2-nitrovinylidenediamine as a powdered pesticide as a pesticide active ingredient. 8.根据权利要求7所述的农药粒剂,其中所述粉末状农药是包含(E)-N-(6-氯-3-吡啶基甲基)-N-乙基-N’-甲基-2-硝基亚乙烯基二胺作为农药活性成分和稀释剂的粉末状农药。8. The pesticide granule according to claim 7, wherein the powdered pesticide comprises (E)-N-(6-chloro-3-pyridylmethyl)-N-ethyl-N'-methyl - 2-Nitroethylenediamine as a pesticide active ingredient and diluent in powdered pesticides. 9.一种用于生产农药组合物的方法,所述方法包括将粉末状农药与作为用于热固性树脂的原料的第一液体组分混合的步骤;加入作为用于热固性树脂的原料的第二液体组分的步骤;然后使第一液体组分与第二液体组分反应以生成热固性树脂。9. A method for producing a pesticide composition, said method comprising the steps of mixing a powdered pesticide with a first liquid component as a raw material for a thermosetting resin; adding a second liquid component as a raw material for a thermosetting resin The step of liquid components; then reacting the first liquid component with the second liquid component to form a thermosetting resin. 10.根据权利要求9所述的用于生产农药组合物的方法,所述方法包括将粉末状农药与作为用于热固性树脂的原料的第一液体组分混合的步骤,加入作为用于热固性树脂的原料的第二液体组分,从而通过使第一液体组分与第二液体组分反应以生成热固性树脂获得农药粒剂的步骤,将第一液体组分和第二液体组分同时或依次加入得到的农药粒剂中,然后使它们反应以用所述热固性树脂包覆所述农药粒剂的步骤。10. The method for producing an agrochemical composition according to claim 9, said method comprising the step of mixing a powdered agrochemical with a first liquid component as a raw material for a thermosetting resin, adding The second liquid component of the raw material, thereby by making the first liquid component react with the second liquid component to generate the step of obtaining the pesticide granule of the thermosetting resin, the first liquid component and the second liquid component are simultaneously or sequentially A step of adding to the obtained pesticide granules and then allowing them to react to coat the pesticide granules with the thermosetting resin. 11.根据权利要求9或10所述的用于生产农药组合物的方法,其中所述粉末状农药是包含5-氯-N-(1,3-二氢-1,1,3-三甲基-4-异苯并呋喃基)-1,3-二甲基吡唑-4-甲酰胺作为农药活性成分的粉末状农药。11. The method for producing a pesticide composition according to claim 9 or 10, wherein the powdered pesticide comprises 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl Base-4-isobenzofuryl)-1,3-dimethylpyrazole-4-carboxamide as a powdered pesticide as the active ingredient of the pesticide. 12.根据权利要求9或10所述的用于生产农药组合物的方法,其中所述粉末状农药是包含(E)-N-(6-氯-3-吡啶基甲基)-N-乙基-N’-甲基-2-硝基亚乙烯基二胺作为农药活性成分的粉末状农药。12. The method for producing a pesticide composition according to claim 9 or 10, wherein the powdered pesticide comprises (E)-N-(6-chloro-3-pyridylmethyl)-N-ethane A powdered pesticide with N'-methyl-2-nitroethylenediamine as the active ingredient of the pesticide. 13.根据权利要求9或10所述的用于生产农药组合物的方法,其中所述热固性树脂是氨基甲酸酯树脂、尿素树脂或环氧树脂。13. The method for producing an agrochemical composition according to claim 9 or 10, wherein the thermosetting resin is a urethane resin, a urea resin or an epoxy resin. 14.根据权利要求9或10所述的用于生产农药组合物的方法,其中所述热固性树脂是氨基甲酸酯树脂。14. The method for producing an agrochemical composition according to claim 9 or 10, wherein the thermosetting resin is a urethane resin. 15.根据权利要求14所述的用于生产农药组合物的方法,其中第一液体组分是多元醇,并且第二液体组分是聚异氰酸酯。15. The method for producing an agrochemical composition according to claim 14, wherein the first liquid component is a polyol, and the second liquid component is a polyisocyanate. 16.根据权利要求9或10所述的用于生产农药组合物的方法,其中所述热固性树脂是环氧树脂。16. The method for producing an agrochemical composition according to claim 9 or 10, wherein the thermosetting resin is an epoxy resin. 17.根据权利要求16所述的用于生产农药组合物的方法,其中第一液体组分是多胺,并且第二液体组分是聚缩水甘油醚或聚缩水甘油胺。17. The method for producing an agrochemical composition according to claim 16, wherein the first liquid component is a polyamine, and the second liquid component is polyglycidyl ether or polyglycidylamine.
CNA2006800097091A 2005-03-28 2006-01-27 Pesticide composition Pending CN101146449A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9750257B2 (en) 2009-01-30 2017-09-05 Sumitomo Chemical Company, Limited Coated seed
CN111848421A (en) * 2020-08-19 2020-10-30 贵州省烟草科学研究院 Polyether-based pesticide adjuvant and preparation method and application thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9750257B2 (en) 2009-01-30 2017-09-05 Sumitomo Chemical Company, Limited Coated seed
CN111848421A (en) * 2020-08-19 2020-10-30 贵州省烟草科学研究院 Polyether-based pesticide adjuvant and preparation method and application thereof
CN111848421B (en) * 2020-08-19 2023-04-28 贵州省烟草科学研究院 Polyether-based pesticide auxiliary agent and preparation method and application thereof

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