CN103347384B - 包含包封农药的农业化学配制剂 - Google Patents
包含包封农药的农业化学配制剂 Download PDFInfo
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- CN103347384B CN103347384B CN201280006365.4A CN201280006365A CN103347384B CN 103347384 B CN103347384 B CN 103347384B CN 201280006365 A CN201280006365 A CN 201280006365A CN 103347384 B CN103347384 B CN 103347384B
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 1
- YFNCATAIYKQPOO-UHFFFAOYSA-N thiophanate Chemical class CCOC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OCC YFNCATAIYKQPOO-UHFFFAOYSA-N 0.000 description 1
- DENPQNAWGQXKCU-UHFFFAOYSA-N thiophene-2-carboxamide Chemical class NC(=O)C1=CC=CS1 DENPQNAWGQXKCU-UHFFFAOYSA-N 0.000 description 1
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- YWBFPKPWMSWWEA-UHFFFAOYSA-O triazolopyrimidine Chemical class BrC1=CC=CC(C=2N=C3N=CN[N+]3=C(NCC=3C=CN=CC=3)C=2)=C1 YWBFPKPWMSWWEA-UHFFFAOYSA-O 0.000 description 1
- MCVUKOYZUCWLQQ-UHFFFAOYSA-N tridecylbenzene Chemical compound CCCCCCCCCCCCCC1=CC=CC=C1 MCVUKOYZUCWLQQ-UHFFFAOYSA-N 0.000 description 1
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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Abstract
本发明涉及一种含有悬浮农药A以及包含核和壳的微胶囊的含水组合物,其中该核含有农药B和非质子性极性溶剂B,并且该壳含有聚(甲基)丙烯酸酯,所述聚(甲基)丙烯酸酯以聚合形式包含丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸。本发明进一步涉及一种制备所述组合物的方法,包括混合农药A、水和微胶囊,涉及所述微胶囊,其中该核含有农药B和溶剂A,其中在该核中农药B与所有溶剂总和的重量比为1:1-1:10,并且其中该微胶囊基于该核中所有农药、该核中所有溶剂和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯。
Description
本发明涉及一种含有悬浮农药A以及包含核和壳的微胶囊的含水组合物,其中该核含有农药B和非质子性极性溶剂B,并且该壳含有聚(甲基)丙烯酸酯,所述聚(甲基)丙烯酸酯以聚合形式包含丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸。本发明进一步涉及一种制备所述组合物的方法,包括混合农药A、水和微胶囊,涉及所述微胶囊,其中该核含有农药B以及溶剂A和非质子性极性溶剂B,其中在该核中农药B与所有溶剂总和的重量比为1:1-1:10,并且其中该微胶囊基于该核中所有农药、该核中所有溶剂和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯;涉及一种制备所述微胶囊的方法,包括加热含有自由基引发剂、溶剂A和农药B以及选自丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸的单体的水包油乳液的步骤;最后涉及一种防治植物病原性真菌和/或不希望的植物生长和/或不希望的昆虫或螨虫侵袭和/或调节植物生长的方法,其中使所述微胶囊或所述含水组合物作用于特定有害物、其栖息地或待防止特定有害物的植物、土壤和/或不希望的植物和/或有用植物和/或其生长地。优选实施方案与其他优选实施方案的组合在本发明范围内。
包含聚(甲基)丙烯酸酯壳和含有农药的核的微胶囊是已知的。现有技术状态具有各种缺点:活性成分的高结晶倾向;配制剂在宽温度范围内的低稳定性;与其他农药的低相容性;高随风漂移性;活性成分被UV光分解;低耐雨水冲刷性。本发明的目的是克服该类问题。
该目的由一种含有悬浮农药A以及包含核和壳的微胶囊的含水组合物实现,其中该核含有农药B和非质子性极性溶剂B,并且该壳含有聚(甲基)丙烯酸酯,所述聚(甲基)丙烯酸酯以聚合形式包含丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸。
该含水组合物可以含有5-80重量%,优选10-70重量%,尤其是20-55重量%水。
该含水组合物通常含有5-80重量%,优选10-60重量%微胶囊。该含水组合物通常含有至少2重量%,优选至少5重量%,尤其是至少8重量%包封农药。
术语农药涉及至少一种选自杀真菌剂、杀虫剂、杀线虫剂、除草剂、安全剂和/或生长调节剂的活性物质。优选的农药是杀真菌剂、杀虫剂、除草剂和生长调节剂。尤其优选的农药是杀虫剂。还可以使用上述类别中两种或更多种农药的混合物。熟练技术人员熟知该类农药,它们例如可以在the Pesticide Manual,第15版(2009),The British Crop Protection Council,London中找到。合适的杀虫剂是选自如下类别的杀虫剂:氨基甲酸酯类、有机磷酸酯类、有机氯杀虫剂、苯基吡唑类、合成除虫菊酯类、新类烟碱类、斯皮诺素类(spinosins)、阿维菌素类(avermectins)、米尔霉素类(milbemycins)、保幼激素类似物、烷基卤、有机锡化合物、沙蚕毒素类似物、苯甲酰脲类、二酰基肼类、METI杀螨剂以及杀虫剂如氯化苦(chloropicrin)、拒嗪酮(pymetrozin)、氟啶虫酰胺(flonicamid)、四螨嗪(clofentezin)、噻螨酮(hexythiazox)、特苯唑(etoxazole)、杀螨硫隆(diafenthiuron)、克螨特(propargite)、三氯杀螨砜(tetradifon)、氟唑虫清(chlorfenapyr)、二硝酚(DNOC)、噻嗪酮(buprofezine)、灭蝇胺(cyromazine)、双甲脒(amitraz)、灭蚁腙(hydramethylnon)、灭螨醌(acequinocyl)、嘧螨酯(fluacrypyrim)、鱼藤酮(rotenone)或其衍生物。合适的杀真菌剂是选自如下类别的杀真菌剂:二硝基苯胺类、烯丙基胺类、苯胺基嘧啶类、抗生素类、芳族烃类、苯磺酰胺类、苯并咪唑类、苯并异噻唑类、二苯甲酮类、苯并噻二唑类、苯并三嗪类、苄基氨基甲酸酯类、氨基甲酸酯类、羧酰胺类、羧酸二酰胺类、氯代腈类、氰基乙酰胺肟类、氰基咪唑类、环丙烷羧酰胺类、二羧酰亚胺类、二氢二嗪类、二硝基苯基巴豆酸酯类、二硫代氨基甲酸酯类、二硫戊环类、乙基膦酸酯类、乙基氨基噻唑羧酰胺类、胍类、羟基-(2-氨基-)嘧啶类、羟基酰替苯胺类、咪唑类、咪唑啉酮类、无机物质、异苯并呋喃酮类、甲氧基丙烯酸酯类、甲氧基氨基甲酸酯类、吗啉类、N-苯基氨基甲酸酯类、唑烷二酮类、肟基乙酸酯类、肟基乙酰胺类、肽基嘧啶核苷、苯基乙酰胺类、苯基酰胺类、苯基吡咯类、苯基脲类、膦酸酯类、硫代磷酸酯类、邻氨甲酰苯甲酸类、苯邻二甲酰亚胺类、哌嗪类、哌啶类、丙酰胺类、哒嗪酮类、吡啶类、吡啶基甲基苯甲酰胺类、嘧啶胺类、嘧啶类、嘧啶酮腙类、吡咯并喹啉酮类、喹唑啉酮类、喹啉类、醌类、磺酰胺类、氨磺酰三唑类、噻唑羧酰胺类、硫代氨基甲酸酯类、托布津类(thiophanates)、噻吩羧酰胺类、甲苯甲酰胺类、三苯基锡化合物、三嗪类、三唑类。合适的除草剂是选自如下类别的除草剂:乙酰胺类、酰胺类、芳氧基苯氧基丙酸酯类、苯甲酰胺类、苯并呋喃、苯甲酸类、苯并噻二嗪酮类、联吡啶氨基甲酸酯类、氯代乙酰胺类、氯代羧酸、环己烷二酮类、二硝基苯胺类、二硝基苯酚类、二苯基醚类、甘氨酸类、咪唑啉酮类、异唑类、异唑烷酮类、腈类、N-苯基苯邻二甲酰亚胺类、二唑类、唑烷二酮类、羟乙酰胺类、苯氧基羧酸类、苯基氨基甲酸酯类、苯基吡唑类、苯基吡唑啉类、苯基哒嗪类、次膦酸类、氨基磷酸酯类、二硫代磷酸酯类、邻氨甲酰苯甲酸酯类、吡唑类、哒嗪酮类、吡啶类、吡啶羧酸类、吡啶羧酰胺类、嘧啶二酮类、嘧啶基(硫代)苯甲酸酯类、喹啉羧酸类、缩氨基脲类、磺酰氨基羰基三唑啉酮类、磺酰脲类、四唑啉酮类、噻二唑类、硫代氨基甲酸酯类、三嗪类、三嗪酮类、三唑类、三唑啉酮类、三唑并羧酰胺类、三唑并嘧啶类、三酮类、尿嘧啶类、脲类。
农药A为悬浮于含水组合物中的农药。悬浮农药的粒度通常例如为0.9-50μm,优选1-20μm。
农药A优选在20℃下在水中的溶解度小于10g/l。更优选它的溶解度小于1.0g/l,尤其小于0.2g/l。例如,在水中的溶解度为:唑菌胺酯(pyraclostrobin)1.9mg/l,丙氯灵(prochloraz)34mg/L,苯菌酮(metrafenon)0.5mg/l,甲体氯氰菊酯(alphacypermethrin)0.01mg/l。
农药A通常具有的熔点为至少30℃,优选至少40℃,尤其是至少45℃。例如熔点为:唑菌胺酯64℃,丙氯灵47℃,苯菌酮100℃,甲体氯氰菊酯79℃。
农药A优选包括杀虫剂,尤其是甲体氯氰菊酯。
农药B为含于微胶囊核中的农药。农药B可以以溶解形式、作为悬浮液、乳液或悬浮乳液存在于该核中。优选农药B以溶解形式存在。
在20℃下,农药B通常在沸程为235-290℃的芳烃(例如200ND)与2-庚酮的混合物(1:1重量%)中的溶解度为至少10重量%,优选至少20重量%,尤其是至少30重量%。
农药B优选在20℃下在水中的溶解度小于10g/l。更优选它的溶解度小于1.0g/l,尤其小于0.2g/l。
农药B通常具有的熔点为至少30℃,优选至少40℃,尤其是至少45℃。
农药A和农药B可以相同或不同,优选它们相同。优选农药A和B均为杀虫剂、除草剂或杀真菌剂(尤其是杀虫剂)。
该核可以含有水不溶混性溶剂A,水不溶混性溶剂A的合适实例是:
-烃类溶剂,如脂族、环状和芳族烃类(例如甲苯、二甲苯、石蜡、四氢萘、烷基化萘或其衍生物、中到高沸点的矿物油馏分(如煤油、柴油、煤焦油));
-植物油如玉米油、菜籽油;
-脂肪酸酯如C10-C22脂肪酸的C1-C10烷基酯;或
-植物油的甲基或乙基酯如菜籽油甲基酯或玉米油甲基酯。
上述溶剂的混合物也是可能的。优选的溶剂A是烃类,尤其是芳族烃。
优选溶剂A在20℃下在水中的溶解度为至多50g/l,更优选至多5g/l,尤其是至多0.5g/l。
溶剂A通常具有超过100℃,优选超过150℃,尤其是超过180℃的沸点。
该核可以含有非质子性极性溶剂B。非质子性极性溶剂B在20℃下在水中的溶解度为0.5-50g/l。溶剂B优选在水中的溶解度为0.5-20.0g/l,尤其是0.5-10.0g/l。不同种类溶剂B的混合物也是可能的。溶剂B通常不含碳-碳双键和/或叁键以避免副反应。
溶剂B优选为酮类,如脂族或芳族酮。合适实例是苯乙酮、2-庚酮或环己酮。更优选溶剂B为在20℃下在水中的溶解度为0.5-20g/l的酮类。溶剂B尤其为2-庚酮。
例如,列出一些溶解度值(所有数据为在20℃下的值):苯乙酮5.5g/l,2-庚酮4.3g/l,3-庚酮(2.6g/l),2-己酮(14g/l),5-甲基-2-己酮(5.4g/l),5-甲基-3-庚酮(3.0g/l),3-甲基-2-己酮(4.1g/l),4-甲基-2-己酮(4.3g/l),2-甲基-3-己酮(6.3g/l),4-甲基-3-己酮(5.2g/l),5-甲基-3-己酮(5.2g/l),3-乙基-2-戊酮(4.6g/l),3,3-二甲基-2-戊酮(7.3g/l),3,4-二甲基-2-戊酮(6.7g/l),4,4-二甲基-2-戊酮(10.4g/l),2,2-二甲基-3-戊酮(10.4g/l),2,4-二甲基-3-戊酮(5.7g/l),2-辛酮(0.9g/l),2,5-二甲基-3-己酮(2.6g/l),2,2-二甲基-3-己酮(2.8g/l),3,3-二甲基-2-己酮(2.7g/l),3,4-二甲基-2-己酮(1.4g/l),4,4-二甲基-3-己酮(2.5g/l),3-乙基-4-甲基-2-戊酮(1.7g/l),2-甲基-3-庚酮(1.4g/l),2-甲基-4-庚酮(1.7g/l),3-甲基-2-庚酮(0.9g/l),3-甲基-4-庚酮(1.9g/l),5-甲基-3-庚酮(1.1g/l),6-甲基-2-庚酮(0.8g/l),6-甲基-3-庚酮(0.9g/l),3-辛酮(0.8g/l),4-辛酮(1.0g/l),2,2,4-三甲基-3-戊酮(5.5g/l),3-乙基-3-甲基-2-戊酮(1.8g/l),5-甲基-2-庚酮(1.0g/l),异佛尔酮(15g/l)。
该核可以含有溶剂A或溶剂B,或者可以含有溶剂A和溶剂B二者。优选该核含有溶剂A且任选含有溶剂B。
该核尤其含有溶剂A和溶剂B。此时溶剂A与溶剂B的重量比通常为5:95-95:5,优选10:1-1:5,更优选5:1-1:2,尤其是3:1-1:1。
除了溶剂A和溶剂B外,该核可以含有其他溶剂。基于该核中所有溶剂的总重量,该核通常包含小于40重量%,优选小于20重量%,尤其小于5重量%其他溶剂。
该核中所有农药(例如农药B)的总和与该核中所有溶剂(例如溶剂A和溶剂B)的总和的重量比通常为5:1-1:20,优选1:1-1:10,更优选1:1.2-1:5,尤其是1:1.5-1:3。
基于核材料的总量,该核含有至少5重量%,优选至少15重量%,尤其是至少25重量%农药(例如农药B)。该核可以含有至多70重量%,优选至多50重量%农药。核材料的量通常由该核中所有农药和溶剂的总量计。
该核基于核材料的总量含有至少10重量%,优选至少20重量%,尤其是至少35重量%溶剂A。该核可以含有至多90重量%,优选至多70重量%溶剂A。
该核基于核材料的总量含有至少5重量%,优选至少10重量%,尤其是至少18重量%溶剂B。该核可以含有至多80重量%,优选至多65重量%溶剂B。
该核任选可以含有助剂,如下面所提到的那些。优选该核含有至少一种助剂(例如有机改性的聚硅氧烷,如Break Thru ;醇烷氧基化物,如,Atplus ,Plurafac 和Lutensol ;EO/PO嵌段聚合物,例如Pluronic 和Genapol ;醇乙氧基化物如Lutensol ;以及磺基琥珀酸二辛酯钠如Leophen )。
优选该微胶囊基于该核中所有农药(例如农药B)、该核中所有溶剂(例如溶剂A和B)和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯。尤其优选含有至多6.5重量%,尤其是6.0重量%,特别是5.5重量%的微胶囊。该微胶囊通常含有至少0.5重量%,优选至少1.5重量%,尤其是2.5重量%的聚(甲基)丙烯酸酯。
聚(甲基)丙烯酸酯的量通过将用于合成该壳的单体(如丙烯酸和甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和马来酸)的量加起来计算。
胶囊的平均粒度(借助光散射的z-平均;优选平均D4,3)为0.5-50μm,优选0.5-20μm,更优选1-10μm,尤其是1-8μm。
该壳含有以聚合形式包含丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸的聚(甲基)丙烯酸酯。
该聚(甲基)丙烯酸酯通常以聚合形式含有:
30-100重量%的一种或多种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸(单体I),
0-70重量%的一种或多种双官能和/或多官能单体(单体II),和
0-40重量%的一种或多种其他单体(单体III),
在每种情况下基于单体的总重量。
该聚(甲基)丙烯酸酯优选以聚合形式含有:
30-90重量%的一种或多种丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸(单体I),
10-70重量%的一种或多种双官能和/或多官能单体(单体II),和
0-40重量%的一种或多种其他单体(单体III),
在每种情况下基于单体的总重量。
所述单体的聚合通常得到聚(甲基)丙烯酸酯。聚(甲基)丙烯酸酯为已知的包封材料,例如由WO2008/071649,EP0457154或DE102007055813已知。
胶囊壁的聚(甲基)丙烯酸酯通常以共聚形式包含基于单体总重量为至少30重量%,在优选形式中为至少40重量%,在特别优选形式中为至少50重量%,更具体为至少55重量%,非常特别优选至少70重量%,以及至多100重量%,优选不超过90重量%,更具体不超过85重量%,非常特别优选不超过80重量%的至少一种选自丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和马来酸(单体I)的单体。
此外,胶囊壁的聚(甲基)丙烯酸酯优选以共聚形式包含基于单体总重量为至少10重量%,优选至少15重量%,优选至少20重量%,以及通常不超过70重量%,优选不超过60重量%,特别优选不超过50重量%的一种或多种双官能或多官能单体(单体II)。在另一优选实施方案中,胶囊壁的聚(甲基)丙烯酸酯优选以共聚形式包含基于单体总重量为至少10重量%,优选至少15重量%,以及通常不超过50重量%,优选不超过40重量%的一种或多种双官能或多官能单体(单体II)。
额外地,该聚(甲基)丙烯酸酯可以以共聚形式包含至多40重量%,优选至多30重量%,更具体为至多20重量%的其他单体III。胶囊壁优选仅由I和II组单体合成。
合适的单体I是丙烯酸和/或甲基丙烯酸的C1-C24烷基酯以及还有不饱和C3和C4羧酸如丙烯酸、甲基丙烯酸和马来酸。合适的单体I是丙烯酸的异丙基、异丁基、仲丁基和叔丁基酯以及对应的甲基丙烯酸酯,还特别优选丙烯酸的甲基、乙基、正丙基和正丁基酯以及对应的甲基丙烯酸酯。通常优选甲基丙烯酸酯和甲基丙烯酸。
根据一个优选实施方案,微胶囊壁基于单体I的总量以共聚形式包含10-60重量%马来酸、甲基丙烯酸和/或丙烯酸,更具体为甲基丙烯酸。
合适的单体II是双官能和/或多官能单体。双官能或多官能单体是指具有至少两个非共轭烯属双键的化合物。主要考虑的是二乙烯基单体和多乙烯基单体。它们导致胶囊壁在聚合过程中交联。在另一优选实施方案中,单体II包含一种或多种双官能和多官能单体。
合适的二乙烯基单体是二乙烯基苯和二乙烯基环己烷。优选的二乙烯基单体是二醇与丙烯酸或甲基丙烯酸的二酯,还有这些二醇的二烯丙基醚和二乙烯基醚。例如可以提到乙二醇二丙烯酸酯,乙二醇二甲基丙烯酸酯,1,3-丁二醇二甲基丙烯酸酯,甲代烯丙基甲基丙烯酰胺,丙烯酸烯丙酯和甲基丙烯酸烯丙酯。特别优选丙二醇、1,4-丁二醇、戊二醇和己二醇的二丙烯酸酯和对应的甲基丙烯酸酯。
优选的多乙烯基单体是多元醇与丙烯酸和/或甲基丙烯酸的多酯,还有这些多元醇的多烯丙基和多乙烯基醚,三乙烯基苯和三乙烯基环己烷。特别优选三羟甲基丙烷三丙烯酸酯和三甲基丙烯酸酯,季戊四醇三烯丙基醚,季戊四醇四烯丙基醚,季戊四醇三丙烯酸酯和季戊四醇四丙烯酸酯,还有它们的工业混合物。
所考虑的单体III是不同于单体I和II的其他单体,如乙酸乙烯酯、丙酸乙烯酯、乙烯基吡啶和苯乙烯或α-甲基苯乙烯。特别优选衣康酸,乙烯基膦酸,马来酸酐,丙烯酸2-羟基乙基酯和甲基丙烯酸2-羟基乙基酯,丙烯酰胺基-2-甲基丙烷磺酸,甲基丙烯腈,丙烯腈,甲基丙烯酰胺,N-乙烯基吡咯烷酮,N-羟甲基丙烯酰胺,N-羟甲基甲基丙烯酰胺,甲基丙烯酸二甲氨基乙酯和甲基丙烯酸二乙氨基乙酯。
通常将保护性胶体掺入胶囊壁中或胶囊壁上并且因此同样为胶囊壁的成分。通常而言,该聚合物的表面具有保护性胶体。因此,基于微胶囊总重量可以存在至多10重量%的保护性胶体。
本发明进一步涉及一种制备本发明组合物的方法,包括混合农药A、水和微胶囊。这例如可以在室温下进行。对于混合可以使用标准工业混合设备。优选混合农药A的含水悬浮液和含有农药B的微胶囊的含水悬浮液。农药A和农药B优选相同。
微胶囊通常可以由包括加热水包油乳液的步骤制备,该乳液含有自由基引发剂、农药B以及选自丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸的单体。微胶囊的制备方法是称为就地聚合的方法。形成微胶囊的原理基于由单体、自由基引发剂、保护性胶体和待包封的信息素制备稳定的水包油乳液。然后通过加热引发单体的聚合并且合适的话通过进一步提高温度而控制,所得聚合物形成包封信息素的胶囊壁。该通用原理例如描述于DE A10139171中。
本发明的含水组合物还可以包含常用于农业化学品配制剂的辅助剂。所用辅助剂分别取决于特定施用形式和活性物质。合适辅助剂的实例是分散剂或乳化剂(如其他加溶剂、保护性胶体、表面活性剂和粘附剂),有机和无机增稠剂,杀菌剂,防冻剂,消泡剂,合适的话还有着色剂和增粘剂或粘合剂(例如用于种子处理配制剂)。
合适的表面活性物质(辅助剂、润湿剂、增粘剂、分散剂或乳化剂)是芳族磺酸如木素磺酸(类型,挪威Borregaard)、苯酚磺酸、萘磺酸(类型,Akzo Nobel,USA)和二丁基萘磺酸(类型,德国BASF)及脂肪酸的碱金属、碱土金属和铵盐,烷基-和烷基芳基磺酸盐,烷基硫酸盐,月桂基醚硫酸盐和脂肪醇硫酸盐,以及硫酸化十六-、十七-和十八烷醇及脂肪醇乙二醇醚的盐,磺化萘及其衍生物与甲醛的缩合物,萘或萘磺酸与苯酚和甲醛的缩合物,聚氧乙烯辛基酚醚,乙氧基化异辛基酚、乙氧基化辛基酚或乙氧基化壬基酚,烷基苯基聚乙二醇醚,三丁基苯基聚乙二醇醚,烷基芳基聚醚醇,异十三烷醇,脂肪醇/氧化乙烯缩合物,乙氧基化蓖麻油,聚氧乙烯烷基醚或聚氧丙烯烷基醚,月桂醇聚乙二醇醚乙酸酯,山梨醇酯,木素亚硫酸盐废液,以及蛋白质,变性蛋白,多糖(例如甲基纤维素),疏水改性淀粉,聚乙烯醇(类型,瑞士Clariant),聚羧酸盐(类型,德国BASF),聚烷氧基化物,聚乙烯胺(类型,德国BASF),聚乙烯亚胺(类型,德国BASF),聚乙烯基吡咯烷酮及其共聚物。
特别合适的表面活性剂是阴离子性、阳离子性、非离子性和两性表面活性剂,嵌段聚合物和聚电解质。合适的阴离子性表面活性剂是磺酸、硫酸、磷酸或羧酸的碱金属、碱土金属或铵盐。磺酸盐的实例是烷基芳基磺酸盐、二苯基磺酸盐、α-烯烃磺酸盐、脂肪酸和油的磺酸盐、乙氧基化烷基酚的磺酸盐、缩合萘的磺酸盐、十二烷基-和十三烷基苯的磺酸盐、萘和烷基萘的磺酸盐、磺基琥珀酸盐或磺基琥珀酰胺酸盐。硫酸盐的实例是脂肪酸和油的硫酸盐、乙氧基化烷基酚的硫酸盐、醇的硫酸盐、乙氧基化醇的硫酸盐或脂肪酸酯的硫酸盐。磷酸盐的实例是磷酸盐酯。羧酸盐的实例是烷基羧酸盐和羧化醇或烷基酚乙氧基化物。
合适的非离子表面活性剂是烷氧基化物,N-烷基化脂肪酸酰胺,胺氧化物,酯或糖基表面活性剂。烷氧基化物的实例是诸如已经烷氧基化的醇、烷基酚、胺(例如牛油脂肪胺)、酰胺、芳基酚、脂肪酸或脂肪酸酯的化合物。氧化乙烯和/或氧化丙烯可以用于烷氧基化,优选氧化乙烯。N-烷基化脂肪酸酰胺的实例是脂肪酸葡糖酰胺或脂肪酸链烷醇酰胺。酯的实例是脂肪酸酯、甘油酯或甘油单酯。糖基表面活性剂的实例是脱水山梨醇、乙氧基化脱水山梨醇、蔗糖和葡萄糖酯或烷基聚葡糖苷。合适阳离子性表面活性剂的实例是季表面活性剂,例如具有一个或两个疏水性基团的季铵化合物,或长链伯胺的盐。合适的两性表面活性剂是烷基甜菜碱和咪唑啉类。合适的嵌段聚合物是包含聚氧乙烯和聚氧丙烯的嵌段的A-B或A-B-A类型嵌段聚合物或包含链烷醇、聚氧乙烯和聚氧丙烯的A-B-C类型嵌段聚合物。合适的聚电解质是聚酸或聚碱。聚酸的实例是聚丙烯酸的碱金属盐。聚碱的实例是聚乙烯基胺或聚乙烯胺。本发明组合物可以包含至少1重量%,优选至少5重量%的非离子表面活性剂(例如烷氧基化物)。
增稠剂(即赋予组合物以改性的流动性,即静止条件下的高粘度和搅动过程中的低粘度的化合物)的实例是多糖以及有机和无机粘土,如XanthanGum(,CP Kelco,USA),23(法国Rhodia),(R.T.Vanderbilt,USA)或(Engelhard Corp.,NJ,USA)。可以加入杀菌剂来保存和稳定该组合物。合适杀菌剂的实例是基于双氯酚和苄醇半缩甲醛的那些(ICI的或Thor Chemie的RS以及Rohm&Haas的MK)以及异噻唑啉酮衍生物如烷基异噻唑啉酮类和苯并异噻唑啉酮类(Thor Chemie的MBS)。合适防冻剂的实例是乙二醇、丙二醇、尿素和甘油。消泡剂的实例是聚硅氧烷乳液(例如SRE,德国Wacker或,法国Rhodia),长链醇,脂肪酸,脂肪酸盐,有机氟化合物及其混合物。增粘剂或粘合剂的实例是聚乙烯吡咯烷酮、聚乙酸乙烯酯、聚乙烯醇和纤维素醚(,日本Shin-Etsu)。
本发明进一步涉及如上所定义的微胶囊,其中该核含有农药B、溶剂A和非质子性极性溶剂B,并且所有农药B(在不止一种农药存在于该核中的情况下为该核中所有农药的总和)与该核中所有溶剂的总和的重量比为1:1-1:10,并且其中该微胶囊基于农药、溶剂和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯。
例如,该微胶囊包含壳和核,其中
-该核含有农药B、溶剂A和非质子性极性溶剂B,
-该壳含有以聚合形式包含丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸的聚(甲基)丙烯酸酯,
-该核中农药B与所有溶剂的总和的重量比为1:1-1:10,以及
-该微胶囊基于该核中所有农药、该核中所有溶剂和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯。
本发明微胶囊的其他优选实施方案如上所述。
本发明进一步涉及一种制备本发明微胶囊的方法,包括加热水包油乳液的步骤,该乳液含有自由基引发剂、溶剂A、非质子性极性溶剂B和农药B以及选自丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸的单体。该微胶囊制备方法是称为就地聚合的方法。形成微胶囊的原理基于由单体、自由基引发剂、保护性胶体、溶剂和待包封的农药制备稳定的水包油乳液。然后通过加热引发单体的聚合并且合适的话通过进一步提高温度而控制,所得聚合物形成包封信息素的胶囊壁。该通用原理例如描述于DE A10139171中。
本发明进一步涉及一种防治植物病原性真菌和/或不希望的植物生长和/或不希望的昆虫或螨虫侵袭和/或调节植物生长的方法,其中使本发明的微胶囊或含水组合物作用于特定有害物、其栖息地或待防止特定有害物的植物、土壤和/或不希望的植物和/或有用植物和/或其生长地。
可以处理各种植物,如禾谷类,例如小麦、黑麦、大麦、小黑麦、燕麦或稻;甜菜,例如糖用甜菜或饲料甜菜;水果,如仁果、核果或浆果,例如苹果、梨、李、桃、杏仁、樱桃、草莓、悬钩子、黑莓或鹅莓;豆科植物,例如扁豆、豌豆、苜蓿或大豆;油料植物,例如油菜、芥菜、橄榄、向日葵、椰子、可可豆、蓖麻油植物、油棕、花生或大豆;葫芦科植物,例如南瓜、黄瓜或甜瓜;纤维植物,例如棉花、亚麻、大麻或黄麻;柑桔类水果,例如橙子、柠檬、葡萄柚或橘;蔬菜,例如菠菜、莴苣、芦笋、卷心菜、胡萝卜、洋葱、西红柿、土豆、葫芦或柿子椒;月桂类植物,例如鳄梨、肉桂或樟脑;能量和原料植物,例如玉米、大豆、油菜、甘蔗或油棕;玉米;烟草;坚果;咖啡;茶;香蕉;葡萄藤(食用葡萄和酿酒用葡萄);啤酒花;草坪;甜菊叶(也称Stevia);天然橡胶植物或观赏和森林植物,例如花卉、灌木、阔叶树或常绿树,例如针叶树,以及植物繁殖材料如种子和这些植物的作物材料。优选的植物是大豆、棉花、玉米、苜蓿、小麦和蔬菜。
就本发明而言,“昆虫或螨虫”优选选自节肢动物和线虫,更优选有害昆虫、蜘蛛和线虫,甚至更优选昆虫、螨和线虫,其中最优选昆虫。优选的昆虫是蚜虫和鳞翅目昆虫。昆虫的实例是:
鳞翅目昆虫(鳞翅目(Lepidoptera)),例如小地老虎(Agrotis ypsilon)、黄地老虎(Agrotis segetum)、木棉虫(Alabama argillacea)、黎豆夜蛾(Anticarsia gemmatalis)、苹果银蛾(Argyresthia conjugella)、叉纹夜蛾(Autographa gamma)、树尺蠖(Bupalus piniarius)、枞卷叶蛾(Cacoeciamurinana)、Capua reticulana、厕蝇(Cheimatobia brumata)、云杉色卷蛾(Choristoneura fumiferana)、西部云杉色卷蛾(Choristoneura occidentalis)、二化螟(Cirphis unipuncta)、苹果小卷蛾(Cydia pomonella)、松毛虫(Dendrolimus pini)、黄瓜绢野螟(Diaphania nitidalis)、西南玉米杆草螟(Diatraea grandiosella)、埃及钻夜蛾(Earias insulana)、南美玉米苗斑螟(Elasmopalpus lignosellus)、女贞细卷蛾(Eupoecilia ambiguella)、Evetriabouliana、斑点夜蛾(Feltia subterranea)、蜡螟(Galleria mellonella)、李小食心虫(Grapholitha funebrana)、梨小食心虫(Grapholitha molesta)、棉铃虫(Heliothis armigera)、烟芽夜蛾(Heliothis virescens)、玉米穗虫(Heliothiszea)、菜螟(Hellula undalis)、尺蠖(Hibernia defoliaria)、美国白蛾(Hyphantria cunea)、苹果巢蛾(Hyponomeuta malinellus)、番茄虫蛾(Keiferia lycopersicella)、铁杉尺蠖(Lambdina fiscellaria)、甜菜夜蛾(Laphygma exigua)、咖啡潜叶蛾(Leucoptera coffeella)、旋纹潜蛾(Leucoptera scitella)、斑幕潜叶蛾(Lithocolletis blancardella)、葡萄浆果小卷蛾(Lobesia botrana)、甜菜网螟(Loxostege sticticalis)、舞毒蛾(Lymantriadispar)、模毒蛾(Lymantria monacha)、桃潜蛾(Lyonetia clerkella)、黄褐天幕毛虫(Malacosoma neustria)、甘蓝夜蛾(Mamestra brassicae)、黄杉毒蛾(Orgyia pseudotsugata)、玉米螟(Ostrinia nubilalis)、小眼夜蛾(Panolisflammea)、棉花红铃虫(Pectinophora gossypiella)、疆夜蛾(Peridromasaucia)、圆掌舟蛾(Phalera bucephala)、马铃薯麦蛾(Phthorimaeaoperculella)、柑桔潜叶蛾(Phyllocnistis citrella)、欧洲粉蝶(Pierisbrassicae)、苜蓿绿夜蛾(Plathypena scabra)、菜蛾(Plutella xylostella)、大豆夜蛾(Pseudoplusia includens)、美松梢小卷蛾(Rhyacionia frustrana)、马铃薯块茎蛾(Scrobipalpula absoluta)、麦蛾(Sitotroga cerealella)、葡萄卷叶蛾(Sparganothis pilleriana)、草地夜蛾(Spodoptera frugiperda)、海灰翅夜蛾(Spodoptera littoralis)、斜纹夜蛾(Spodoptera litura)、松异舟蛾(Thaumatopoea pityocampa)、绿色橡木飞蛾(Tortrix viridana)、粉纹夜蛾(Trichoplusia ni)和云杉线小卷蛾(Zeiraphera canadensis);
甲虫(鞘翅目(Coleoptera)),例如梨窄吉丁(Agrilus sinuatus)、直条叩头虫(Agriotes lineatus)、暗色叩头虫(Agriotes obscurus)、鞘翅目鳃金龟(Amphimallus solstitialis)、Anisandrus dispar、墨西哥棉铃象(Anthonomusgrandis)、苹花象(Anthonomus pomorum)、甜菜隐食甲(Atomaria linearis)、纵坑切梢小蠹(Blastophagus piniperda)、Blitophaga undata、蚕豆象(Bruchus rufimanus)、豌豆象(Bruchus pisorum)、欧洲兵豆象(Bruchuslentis)、苹卷象(Byctiscus betulae)、甜菜大龟甲(Cassida nebulosa)、Cerotoma trifurcata、白菜籽龟象(Ceuthorrhynchus assimilis)、芫菁龟象(Ceuthorrhynchus napi)、甜菜胫跳甲(Chaetocnema tibialis)、Conoderusvespertinus、石刁柏负泥虫(Crioceris asparagi)、长角叶甲(Diabroticalongicornis)、Diabrotica12-punctata、玉米根叶甲(Diabrotica virgifera)、墨西哥豆瓢虫(Epilachna varivestis)、烟草跳甲(Epitrix hirtipennis)、棉灰蒙象变种(Eutinobothrus brasiliensis)、欧洲松树皮象(Hylobius abietis)、埃及苜蓿叶象(Hypera brunneipennis)、紫苜蓿叶象(Hypera postica)、云杉八齿小蠹(Ips typographus)、烟草负泥虫(Lema bilineata)、黑角负泥虫(Lemamelanopus)、马铃薯叶甲(Leptinotarsa decemlineata)、甜菜叩甲(Limoniuscalifornicus)、稻水象甲(Lissorhoptrus oryzophilus)、Melanotus communis、油菜露尾甲(Meligethes aeneus)、大栗鳃金龟(Melolontha hippocastani)、五月鳃金龟(Melolontha melolontha)、水稻负泥虫(Oulema oryzae)、葡萄黑耳喙象(Ortiorrhynchus sulcatus)、草莓根象甲(Otiorrhynchus ovatus)、辣根猿叶甲(Phaedon cochleariae)、Phyllotreta chrysocephala、食叶鳃金龟属(Phyllophaga sp.)、庭园发丽金龟(Phyllopertha horticola)、大豆淡足跳甲(Phyllotreta nemorum)、黄曲条菜跳甲(Phyllotreta striolata)、日本金龟子(Popillia japonica)、豌豆叶象(Sitona lineatus)和谷象(Sitophilusgranaria);
双翅目昆虫(双翅目(Diptera)),例如埃及伊蚊(Aedes aegypti)、剌扰伊蚊(Aedes vexans)、墨西哥果蝇(Anastrepha ludens)、五斑按蚊(Anophelesmaculipennis)、地中海实蝇(Ceratitis capitata)、蛆症金蝇(Chrysomyabezziana)、Chrysomya hominivorax、Chrysomya macellaria、高粱瘿蚊(Contarinia sorghicola)、Cordylobia anthropophaga、尖音库蚊(Culexpipiens)、瓜蝇(Dacus cucurbitae)、油橄榄实蝇(Dacus oleae)、油菜叶瘿蚊(Dasineura brassicae)、小毛厕蝇(Fannia canicularis)、马蝇(Gasterophilusintestinalis)、刺舌蝇(Glossina morsitans)、Haematobia irritans、Haplodiplosis equestris、花生田灰地种蝇(Hylemyia platura)、纹皮蝇(Hypoderma lineata)、蔬菜斑潜蝇(Liriomyza sativae)、美国潜叶蝇(Liriomyza trifolii)、Lucilia caprina、铜绿蝇(Lucilia cuprina)、丝光绿蝇(Lucilia sericata)、Lycoria pectoralis、麦瘿蚊(Mayetiola destructor)、家蝇(Musca domestica)、厩腐蝇(Muscina stabulans)、羊狂蝇(Oestrus ovis)、欧洲麦秆蝇(Oscinella frit)、天仙子泉蝇(Pegomya hysocyami)、Phorbiaantiqua、萝卜蝇(Phorbia brassicae)、草种蝇(Phorbia coarctata)、樱桃实蝇(Rhagoletis cerasi)、苹果实蝇(Rhagoletis pomonella)、牛虻(Tabanusbovinus)、Tipula oleracea和欧洲大蚊(Tipula paludosa);
蓟马(缨翅目(Thysanoptera)),例如兰花蓟马(Dichromothrips corbetti)、烟褐蓟马(Frankliniella fusca)、苜蓿花蓟马(Frankliniella occidentalis)、东方花蓟马(Frankliniella tritici)、桔梗蓟马(Scirtothrips citri)、稻蓟马(Thripsoryzae)、棕榈蓟马(Thrips palmi)和烟蓟马(Thrips tabaci);
膜翅目昆虫(膜翅目(Hymenoptera)),例如新疆菜叶蜂(Athalia rosae)、切叶蚁(Atta cephalotes)、Atta sexdens、Atta texana、Hoplocampa minuta、Hoplocampa testudinea、小黄家蚁(Monomorium pharaonis)、热带火蚁(Solenopsis geminate)和红火蚁(Solenopsis invicta);
异翅目昆虫(异翅目(Heteroptera)),例如拟绿蝽(Acrosternum hilare)、玉米长蝽(Blissus leucopterus)、黑斑烟盲蝽(Cyrtopeltis notatus)、棉红蝽(Dysdercus cingulatus)、Dysdercus intermedius、麦扁盾蝽(Eurygasterintegriceps)、烟草蝽(Euschistus impictiventris)、棉红铃喙缘蝽(Leptoglossus phyllopus)、美洲牧草盲蝽(Lygus lineolaris)、牧草盲蝽(Lyguspratensis)、稻绿蝽(Nezara viridula)、甜菜拟网蝽(Piesma quadrata)、Solubea insularis和Thyanta perditor;
同翅目昆虫(同翅目(Homoptera)),例如Acyrthosiphon onobrychis、落叶松球蚜(Adelges laricis)、Aphidula nasturtii、甜菜蚜(Aphis fabae)、草莓根蚜(Aphis forbesi)、苹果蚜(Aphis pomi)、棉蚜(Aphis gossypii)、北美茶簏子蚜(Aphis grossulariae)、Aphis schneideri、卷叶蚜(Aphis spiraecola)、Aphis sambuci、豌豆蚜(Acyrthosiphon pisum)、马铃薯蚜(Aulacorthumsolani)、银叶粉虱(Bemisia argentifolii)、烟粉虱(Bemisia tabaci)、Brachycaudus cardui、杏圆尾蚜(Brachycaudus helichrysi)、Brachycauduspersicae、Brachycaudus prunicola、甘蓝蚜(Brevicoryne brassicae)、Capitophorus horni、Cerosipha gossypii、Chaetosiphon fragaefolii、Cryptomyzus ribis、高加索冷杉椎球蚜(Dreyfusia nordmannianae)、云杉椎球蚜(Dreyfusia piceae)、居根西圆尾蚜(Dysaphis radicola)、Dysaulacorthum pseudosolani、Dysaphis plantaginea、Dysaphis pyri、蚕豆微叶蝉(Empoasca fabae)、桃大尾蚜(Hyalopterus pruni)、Hyperomyzuslactucae、麦长管蚜(Macrosiphum avenae)、大戟长管蚜(Macrosiphumeuphorbiae)、蔷薇管蚜(Macrosiphon rosae)、Megoura viciae、巢莱修尾蚜(Melanaphis pyrarius)、麦无网蚜(Metopolophium dirhodum)、Myzodespersicae、冬葱瘤额蚜(Myzus ascalonicus)、Myzus cerasi、桃蚜(Myzuspersicae)、李瘤蚜(Myzus varians)、Nasonovia ribis-nigri、稻飞虱(Nilaparvata lugens)、囊柄瘿绵蚜(Pemphigus bursarius)、蔗飞虱(Perkinsiella saccharicida)、忽布疣蚜(Phorodon humuli)、苹木虱(Psyllamali)、梨木虱(Psylla piri)、冬葱瘤蛾蚜(Rhopalomyzus ascalonicus)、玉米蚜(Rhopalosiphum maidis)、禾谷溢管蚜(Rhopalosiphum padi)、Rhopalosiphum insertum、Sappaphis mala、Sappaphis mali、麦二叉蚜(Schizaphis graminum)、Schizoneura lanuginosa、麦长管蚜(Sitobionavenae)、白背飞虱(Sogatella furcifera)、白粉虱(Trialeurodesvaporariorum)、Toxoptera aurantiiand和葡萄根瘤蚜(Viteus vitifolii);
白蚁(等翅目(Isoptera)),例如Calotermes flavicollis、Leucotermesflavipes、黄肢散白蚁(Reticulitermes flavipes)、欧洲散白蚁(Reticulitermeslucifugus)和Termes natalensis;
直翅目昆虫(直翅目(Orthoptera)),例如居屋艾蟋(Acheta domestica)、东方蜚蠊(Blatta orientalis)、德国小蠊(Blattella germanica)、欧洲球螋(Forficula auricularia)、蝼蛄(Gryllotalpa gryllotalpa)、飞蝗(Locustamigratoria)、双纹黑蝗(Melanoplus bivittatus)、红足黑蝗(Melanoplusfemur-rubrum)、墨西哥黑蝗(Melanoplus mexicanus)、迁飞黑蝗(Melanoplus sanguinipes)、石栖黑蝗(Melanoplus spretus)、条纹红蝗(Nomadacris septemfasciata)、美洲蟑螂(Periplaneta americana)、美洲沙漠蝗(Schistocerca americana)、Schistocerca peregrina、Stauronotusmaroccanus和庭疾灶螽(Tachycines asynamorus),
蜘蛛纲(Arachnoidea),如蜘蛛(蜱螨目(Acarina)),例如软蜱科(Argasidae)、硬蜱科(Ixodidae)和疥螨科(Sarcoptidae),如长星形壁虱(Amblyomma americanum)、热带花蜱(Amblyomma variegatum)、波斯锐缘蜱(Argas persicus)、牛壁虱(Boophilus annulatus)、Boophilusdecoloratus、微小牛蜱(Boophilus microplus)、Dermacentor silvarum、Hyalomma truncatum、蓖子硬蜱(Ixodes ricinus)、Ixodes rubicundus、Ornithodorus moubata、Otobius megnini、鸡皮刺螨(Dermanyssusgallinae)、绵羊疥病(Psoroptes ovis)、Rhipicephalus appendiculatus、Rhipicephalus evertsi、人疥螨(Sarcoptes scabiei),瘿螨属(Eriophyidae),如苹果刺锈螨(Aculus schlechtendali)、Phyllocoptrata oleivora和Eriophyessheldoni;细螨属(Tarsonemidae),如Phytonemus pallidus和侧多食跗线螨(Polyphagotarsonemus latus);细须螨属(Tenuipalpidae),如紫红短须螨(Brevipalpus phoenicis);叶螨属(Tetranychidae),如朱砂叶螨(Tetranychuscinnabarinus)、神泽叶螨(Tetranychus kanzawai)、太平洋叶螨(Tetranychuspacificus)、棉叶螨(Tetranychus telarius)和二点叶螨(Tetranychus urticae),苹果叶螨(Panonychus ulmi)、柑椐叶螨(Panonychus citri)和oligonychuspratensis;
蚤目(Siphonatera),例如印鼠客蚤(Xenopsylla cheopsis)、角叶属(Ceratophyllus)。
施用可以在播种之前或之中进行。分别将农业化学化合物及其组合物施用或处理于植物繁殖材料,尤其是种子上的方法在本领域是已知的并且包括拌种、包衣、造粒、撒粉、浸泡和繁殖材料的犁沟内施用方法。在优选实施方案中,通过不诱发萌发的方法,例如通过拌种、造粒、包衣和撒粉分别将微胶囊或其组合物施用于植物繁殖材料上。在优选实施方案中,将悬浮类型(FS)组合物用于种子处理。FS组合物通常可以包含1-800g/l活性物质,1-200g/l表面活性剂,0-200g/l防冻剂,0-400g/l粘合剂,0-200g/l颜料和至多1升溶剂,优选水。
微胶囊或含水组合物可以直接使用或者以其农业化学配制剂形式,例如以可直接喷雾溶液、悬浮液、分散体、乳液、油分散体形式借助喷雾、雾化、撒粉、铺展、刷涂、浸渍或浇灌来使用。施用形式完全取决于意欲的目的;在任何情况下意欲确保农药的最佳可能分布。即用制剂中的活性物质浓度可在较宽范围内变化。它们通常为0.0001-10重量%,优选0.001-1重量%活性物质。活性物质还可以成功地以超低容量法(ULV)使用,其中可以施用包含超过95重量%活性物质的组合物或者甚至可以施用不含添加剂的活性物质。
当用于植物保护中时,活性物质(也称为农药)的施用量取决于所需效果的种类为0.001-2kg/ha,优选0.005-2kg/ha,更优选0.05-0.9kg/ha,尤其是0.1-0.75kg/ha。在例如通过撒粉、包衣或浸透种子而处理植物繁殖材料如种子中,每100kg植物繁殖材料(优选种子)通常要求的活性物质量为0.1-1000g,优选1-1000g,更优选1-100g,最优选5-100g。当用于材料或储存产品的保护中时,活性物质的施用量取决于施用区域的种类和所需效果。在材料保护中的常规施用量例如为0.001g-2kg活性物质/米3被处理材料,优选0.005g-1kg活性物质/米3被处理材料。
各种类型的油、润湿剂、辅助剂、除草剂、杀菌剂、其他杀真菌剂和/或农药可加入含水组合物中,合适的话恰在紧临使用前加入(桶混合)。这些试剂通常可以与本发明组合物以1:100-100:1,优选1:10-10:1的重量比混合。可以使用的辅助剂尤其是有机改性的聚硅氧烷如Break Thru S ;醇烷氧基化物如Atplus ,Atplus MBA ,Plurafac LF 和LutensolON ;EO/PO嵌段聚合物,例如Pluronic RPE 和Genapol ;醇乙氧基化物如Lutensol XP ;以及磺基琥珀酸二辛酯钠如Leophen。
本发明具有多种优点:本发明降低了活性成分的结晶;它提高了该配制剂在宽温度范围内的稳定性;存在击倒和残留效力;它改善了与其他农药的相容性;它降低了随风漂移;包封的活性成分有效地防UV光;胶囊可以负载油溶性和水溶性活性成分二者以及辅助剂;胶囊具有增加的耐雨水冲刷性;对工人和用户具有降低的毒理学效果。
下列实施例对本发明给出进一步说明,但本发明并不限于这些实施例。
实施例
200 ND:芳族烃溶剂,沸程235-290℃,凝固点-16℃,萘含量小于0.9重量%(可由Exxon市购)。
150ND:芳族烃溶剂,沸程183-194℃,萘含量小于1.0重量%(可由Exxon市购)。
PVA:部分水解的聚乙烯醇,粘度17-19mPas(DIN 53015)。
PETIA:季戊四醇的三-和四丙烯酸酯的工业混合物。
实施例1—胶囊的制备
水相:
176g 水
116g 10重量%聚乙烯醇PVA水溶液
2g 2.5重量%亚硝酸钠水溶液
油相:
进料1: 2g 75重量%过新戊酸叔丁酯在烃中的溶液
进料2: 3g 10重量%叔丁基过氧化氢的水溶液
进料3:在18g水中的0.2g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为46.5%的胶囊悬浮液。平均粒度D[4,3]为2.1μm。
实施例2—胶囊的制备
水相:
133g 水
88g 10重量%聚乙烯醇PVA水溶液
1.5g 2.5重量%亚硝酸钠水溶液
油相:
进料1:1.5g 75重量%过新戊酸叔丁酯在烃中的溶液
进料2:2.4g 10重量%叔丁基过氧化氢的水溶液
进料3:在14g水中的0.2g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为48.2%的胶囊悬浮液。平均粒度D[4,3]为2.5μm。
实施例3—胶囊的制备
水相:
124g 水
82g 10重量%聚乙烯醇PVA水溶液
1.4g 2.5重量%亚硝酸钠水溶液
油相:
2.3g 甲基丙烯酸
16g 2-苯甲酰基-5-辛氧基苯酚
进料1:1.4g 75重量%过新戊酸叔丁酯在烃中的溶液
进料2:2.3g 10重量%叔丁基过氧化氢的水溶液
进料3:在13g水中的0.1g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为20%的胶囊悬浮液。平均粒度D[4,3]为4.9μm。
实施例4—胶囊的制备
水相:
137g 水
132g 10重量%聚乙烯醇PVA水溶液
2.3g 2.5重量%亚硝酸钠水溶液
油相:
进料1:2.2g 75重量%过新戊酸叔丁酯在烃中的溶液
进料2:3.6g 10重量%叔丁基过氧化氢的水溶液
进料3:在21g水中的0.2g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为52.8%的胶囊悬浮液。平均粒度D[4,3]为1.9μm。
实施例5—胶囊的制备
水相:
200g 水
132g 10重量%聚乙烯醇PVA水溶液
2.3g 2.5重量%亚硝酸钠水溶液
油相:
进料1:2.2g75重量%过新戊酸叔丁酯在烃中的溶液
进料2:3.6g10重量%叔丁基过氧化氢的水溶液
进料3:在21g水中的0.2g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为48.7%的胶囊悬浮液。平均粒度D[4,3]为2.3μm。
实施例6—胶囊的制备
水相:
133g 水
88g 10重量%聚乙烯醇PVA水溶液
1.5g 2.5重量%亚硝酸钠水溶液
油相:
进料1:1.5g75重量%过新戊酸叔丁酯在烃中的溶液
进料2:2.4g10重量%叔丁基过氧化氢的水溶液
进料3:在14g水中的0.1g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为46.3%的胶囊悬浮液。平均粒度D[4,3]为2.3μm。
实施例7—胶囊的制备
水相:
139g 水
92g 10重量%聚乙烯醇PVA水溶液
1.6g 2.5重量%亚硝酸钠水溶液
油相:
8g 2-苯甲酰基-5-辛氧基苯酚
进料1:1.5g 75重量%过新戊酸叔丁酯在烃中的溶液
进料2:2.5g 10重量%叔丁基过氧化氢的水溶液
进料3:在14g水中的0.1g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为49.4%的胶囊悬浮液。平均粒度D[4,3]为4.3μm。
实施例8—胶囊的制备
水相:
210g 水
120g 10重量%聚乙烯醇PVA水溶液
2.4g 2.5重量%亚硝酸钠水溶液
油相:
进料1:2g75重量%过新戊酸叔丁酯在烃中的溶液
进料2:3.3g10重量%叔丁基过氧化氢的水溶液
进料3:在19g水中的0.2g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为49.2%的胶囊悬浮液。平均粒度D[4,3]为2.5μm。
实施例9—胶囊的制备
水相:
182g 水
120g 10重量%聚乙烯醇PVA水溶液
2.1g 2.5重量%亚硝酸钠水溶液
油相:
进料1:2g75重量%过新戊酸叔丁酯在烃中的溶液
进料2:3.3g10重量%叔丁基过氧化氢的水溶液
进料3:在19g水中的0.2g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为48.5%的胶囊悬浮液。平均粒度D[4,3]为2.4μm。
实施例10—胶囊的制备
水相:
553g 水
391g 10重量%聚乙烯醇PVA水溶液
6.8g 2.5重量%亚硝酸钠水溶液
油相:
进料1:6.5g75重量%过新戊酸叔丁酯在烃中的溶液
进料2:11g 10重量%叔丁基过氧化氢的水溶液
进料3:在61g水中的0.6g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为49.1%的胶囊悬浮液。平均粒度D[4,3]为2.4μm。
实施例11—胶囊的制备
水相:
213g 水
59g 10重量%聚乙烯醇PVA水溶液
2g 2.5重量%亚硝酸钠水溶液
油相:
进料1:2g 75重量%过新戊酸叔丁酯在烃中的溶液
进料2:3.2g 10重量%叔丁基过氧化氢的水溶液
进料3:在18g水中的0.2g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在3500rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为49.2%的胶囊悬浮液。平均粒度D[4,3]为4.2μm。
实施例12—胶囊的制备
水相:
214g 水
220g 10重量%聚乙烯醇PVA水溶液
4.4g 2.5重量%亚硝酸钠水溶液
油相:
进料1:3.7g75重量%过新戊酸叔丁酯在烃中的溶液
进料2:6g10重量%叔丁基过氧化氢的水溶液
进料3:在30g水中的0.3g抗坏血酸
在40℃下将油相加入水相中,同时用溶解式搅拌器在4000rpm下分散15分钟。加入进料1并在搅拌的同时在60分钟内将该乳液加热至60℃,在额外2小时内加热至70℃。在30分钟内将它加热至85℃并在温度为85℃的同时在60分钟内加入进料2和3。在冷却至室温之后得到固体含量为54.5%的胶囊悬浮液。平均粒度D[4,3]为2.4μm。
实施例13-26—胶囊的制备
根据前述实施例如下表1中所示制备下列实施例。
表1:实施例13-26的详情
实施例27—农业化学品CS配制剂的制备
在室温下搅拌的同时将实施例1-26的胶囊粗悬浮液与水和添加剂混合。由此得到含有10重量%包封甲体氯氰菊酯、0.1重量%消泡剂、0.2重量%防腐剂、10.0重量%丙二醇防冻剂、16重量%非离子性烷基烷氧基化物表面活性剂、0.1重量%黄原胶和达到100%的水的含水CS农业化学品配制剂。
实施例28—农业化学品ZC配制剂的制备
制备含有10重量%悬浮甲体氯氰菊酯、0.1重量%消泡剂、0.2重量%防腐剂、15重量%丙二醇防冻剂、0.5重量%黄原胶、0.5重量%分散剂、0.1重量%酸性稳定剂和达到100%的水的悬浮浓缩物(SC)。在搅拌的同时将所得SC与实施例27的CS配制剂混合。由此得到含有5重量%包封甲体氯氰菊酯、5重量%悬浮甲体氯氰菊酯、0.1重量%消泡剂、0.2重量%防腐剂、12.5重量%丙二醇防冻剂、8重量%非离子性烷基烷氧基化物表面活性剂、0.3重量%黄原胶、0.2重量%分散剂、0.05重量%酸性稳定剂和达到100%的水的含水ZC农业化学品配制剂。
实施例29—储存稳定性
将实施例27的胶囊配制剂样品(基于实施例1、7和19)用于储存测试。将所有配制剂样品在-10℃或+54℃下储存2周。在2周后肉眼检测没有观察到沉降。
实施例30—分散性
将实施例27的胶囊配制剂样品用于分散性测试。将这些配制剂与标准水(19.2°dH)一起混入圆柱形刻度玻璃瓶中,得到0.1重量%甲体氯氰菊酯的浓度(典型施用浓度)。定性评价自发分散体并在2小时后将沉降物定量。所有样品是自分散性的且在2小时后没有显示沉降。
实施例31—UV稳定性
在室温下将两份样品用光(300-800nm,650W/m2)辐照46小时。在UV暴露之前和之后通过HPLC分析甲体氯氰菊酯在该样品中的浓度,以计算辐照后的回收率(recovery)(表2)。EC为甲体氯氰菊酯的乳液浓缩物(100g/l,在溶剂石脑油中)且可以由BASF SE市购。
表2:光稳定性测试结果
a)对比,非本发明
Claims (13)
1.一种含水组合物,其含有:
悬浮农药A,以及
包含核和壳的微胶囊,其中所述核含有农药B和非质子性极性溶剂B,并且所述壳含有聚(甲基)丙烯酸酯,所述聚(甲基)丙烯酸酯以聚合形式包含丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸,
其中溶剂B为2-庚酮,
其中核含有水不溶混性溶剂A,并且
其中溶剂A与溶剂B的重量比为5:95-95:5,
其中农药B以溶解形式存在,
其中溶剂A为烃类溶剂、植物油、脂肪酸酯、植物油的甲基或乙基酯或上述溶剂的混合物,
其中溶剂A在20℃下在水中的溶解度为至多50g/l。
2.根据权利要求1的组合物,其中所述农药A在20℃下在水中的溶解度小于10g/l。
3.根据权利要求1的组合物,其中溶剂A为烃。
4.根据权利要求2的组合物,其中溶剂A为烃。
5.根据权利要求1-4中任一项的组合物,其中溶剂A与溶剂B的重量比为10:1-1:5。
6.根据权利要求1-4中任一项的组合物,其中所述核中所有农药的总和与所述核中所有溶剂的总和的重量比为1:1-1:10。
7.根据权利要求5的组合物,其中所述核中所有农药的总和与所述核中所有溶剂的总和的重量比为1:1-1:10。
8.根据权利要求1-4中任一项的组合物,其中所述微胶囊基于所述核中所有农药、所述核中所有溶剂和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯。
9.根据权利要求7的组合物,其中所述微胶囊基于所述核中所有农药、所述核中所有溶剂和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯。
10.一种制备如权利要求1-9中任一项所定义的组合物的方法,包括混合所述农药A、水和所述微胶囊。
11.如权利要求10所定义的微胶囊,其中所述核含有所述农药B、溶剂A和所述非质子性极性溶剂B,其中在所述核中所述农药B与所有溶剂的总和的重量比为1:1-1:10,以及其中所述微胶囊基于所述核中所有农药、所述核中所有溶剂和聚(甲基)丙烯酸酯的总量含有至多7重量%聚(甲基)丙烯酸酯,
其中溶剂B为2-庚酮,
其中核含有水不溶混性溶剂A,并且
其中溶剂A与溶剂B的重量比为5:95-95:5。
12.一种制备如权利要求10所定义或根据权利要求11的微胶囊的方法,包括加热水包油乳液的步骤,所述乳液含有自由基引发剂、溶剂A和农药B以及选自丙烯酸和/或甲基丙烯酸的C1-C24烷基酯、丙烯酸、甲基丙烯酸和/或马来酸的单体。
13.一种防治植物病原性真菌和/或不希望的植物生长和/或不希望的昆虫或螨虫侵袭和/或调节植物生长的方法,其中使如权利要求10所定义或根据权利要求11的微胶囊或如权利要求1-9中任一项所定义的含水组合物作用于特定有害物、其栖息地或待防止特定有害物的植物、土壤和/或不希望的植物和/或有用植物和/或其生长地。
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US9681659B2 (en) | 2017-06-20 |
CA2823520A1 (en) | 2012-08-02 |
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