CN115135153A - 在土壤应用和叶面应用中活性提高的胶囊化拟除虫菊酯 - Google Patents
在土壤应用和叶面应用中活性提高的胶囊化拟除虫菊酯 Download PDFInfo
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- CN115135153A CN115135153A CN202180016104.XA CN202180016104A CN115135153A CN 115135153 A CN115135153 A CN 115135153A CN 202180016104 A CN202180016104 A CN 202180016104A CN 115135153 A CN115135153 A CN 115135153A
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- suspension concentrate
- isocyanate
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Fertilizers (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
- Investigation Of Foundation Soil And Reinforcement Of Foundation Soil By Compacting Or Drainage (AREA)
- Catching Or Destruction (AREA)
Abstract
本发明涉及基于各种拟除虫菊酯的水性胶囊悬浮液、其制备以及其以农业化学制剂形式的用途,特别是用于土壤施用。
Description
技术问题/目的
本发明涉及基于各种拟除虫菊酯的水性胶囊悬浮液、其制备方法以及其以农业化学制剂形式的用途,特别是用于土壤施用。
现有技术
拟除虫菊酯是一类既定的活性物质,有多种制剂类型可供选择,用途广泛,例如叶面应用、土壤应用、表面处理、浸渍材料等。
例如(GR制剂形式的L三氟氯氰菊酯)、(七氟菊酯GR)或(氯氰菊酯GR)专门针对土壤应途,特别是针对玉米根虫和类似物种。相较于这些已知的固体制剂,液体制剂在该领域并不常见。然而,固体制剂的一个缺点是通常需要相对高的施用率以及低负载量的制剂。
作物保护活性物质的成功微囊化已在文献中广泛描述,例如US77608085、EP0214936中。许多文献还明确提及拟除虫菊酯作为潜在的活性物质,例如US 5846554、WO1997/44125、WO 2016169683、EPl83999·
此外,例如在市场上有微囊化的久一三氟氯氰菊酯(Karate Zeon)和溴氰菊酯制剂(DelCaps CS 050),在每种情况下都用于叶面应用。
一些专利还提及了胶囊悬浮液用于土壤应用的潜在用途,例如W02016169683、W02016202659,其中拟除虫菊酯也被称为潜在的活性物质。也有关于土壤中微胶囊一般相互作用的科学文献。
W02011042495明确提及例如通过使用聚合物颗粒提高难溶性作物保护活性物质,特别是溴氰菊酯的土壤流动性。然而,W02011042495中没有提供生物学数据,因此没有迹象表明活性物质的土壤流动性、生物活性和/或生物利用度之间的关系。WO 2018/141594描述了向水不溶性除草剂制剂中添加土壤活化剂(mobilizer)。该物质是烷基C厂C3苯基乙氧基化物型(C2-Ca-EO)1-100的袁面活性剂。表面活性剂可以掺入制剂中(例如在SC中)或作为桶混添加剂添加。此外,WO 2018/141594原则上还提及了微囊化除草剂制剂作为可以使用的可能制剂,但同样没有数据支持。
WO 2017/149069描述了聚醚改性的短链硅氧烷作为土壤应用的附加助剂,以提高农艺产量,而与活性物质的制剂类型和物理性质无关。
WO 01/94001描述了额外包含袁面改性成分的微胶囊,还包括拟除虫菊酯的实例。这些物质与微胶囊壳化学键合,以改善土壤中胶囊的特性。这已被证明能够因此提高土壤流动性。
现有技术的缺点
尽管现有技术描述了以颗粒制剂形式提供用于土壤施用的拟除虫菊酯的可能性,但这些制剂仅具有低活性成分浓度,因此需要高施用率,这也由于佐剂和其他配方助剂导致对土壤的高应力。
此外,现有技术中还描述了用于以胶囊化制剂形式提供拟除虫菊酯作为液体制剂的各种选择。然而,尚不清楚这在多大程度上适用于土壤有效性较差的活性成分,例如不能以固体制剂用于土壤应用的溴氰菊酯。
此外,现有技术中没有描述适用于土壤和叶面应用的制剂:特别是没有已知的制剂可以有效地土壤应用溴氰菊酯。
总而言之,可以说该领域的专家目前认为溴氰菊酯特别不适合土壤应用。
目的
因此,本发明的目的是提供一种合适的制剂,其对于拟除虫菊酯活性成分,特别是溴氰菊酯具有尽可能高的活性成分负载量和低施用率,普遍确保足够的生物利用度以及足够的长期土壤应用活性。
本发明的目的还在于提供一种仅用少量制剂助剂和惰性材料对土壤施加应力的制剂。
本发明的目的还在于提供一种适用于土壤和叶面应用的制剂。
技术方案
该目的通过本发明的胶囊悬浮浓缩物(CS)得以解决。出人意料地发现,本发明的制剂普遍适用于拟除虫菊酯类化合物的土壤应用,而与它们的物理化学性质无关。本发明的CS确保活性成分足够高的有效性和足够的活性持续时间。出人意料地发现,无论土壤条件如何(如土壤中的水分含量和有机物质的比例),本发明的制剂都显示出良好的生物活性。
还能够证明本发明的胶囊悬浮液也适用于叶面应用。
发明内容
因此,本发明提供胶囊悬浮浓缩物,其包含
A)颗粒分散相,其包含
1')至少一种具有异氰酸酯反应基团的化合物a1-1')和异氰酸酯或异氰酸酯混合物a1.2)的反应产物,
2)在有机、水不溶性溶剂a2.2)中的拟除虫菊酯a2.1),
3')一种或多种添加剂a3.1')以及
B)包含至少一种保护胶体b1.1)和任选地其他添加剂b1.2)的液体水相,
其中分散相A)的颗粒的平均粒径优选为1-50gm
以及其中
a1-2)的比例为按重量计0.1%至2%,
农业化学活性成分a2.1)的比例为按重量计1%至50%,
有机溶剂a2.2')的比例为按重量计1%至90%,
添加剂a3.1)的比例为按重量计0.5%至5%,
保护胶体b1.1)的比例为按重量计0.1%至5%,以及
添加剂b1.2)的比例为按重量计0.1%至15%。
当a.1.1不是添加的胺或醇,a.1.1是异氰酸酯水解释放的胺。
根据a1.1的化合物也可称为交联剂。因此,除非另有定义,交联剂是用于本发明的目的的根据a1.1的化合物。
本发明还提供了本发明的胶囊悬浮液在拟除虫菊酯和特别是溴氰菊酯的土壤应用中的用途。
粒径根据CIPAC(CIPAC=国际农药分析协作委员会;www.cipac.org)方法MT 187确定。在该方法中,粒径分布通过激光衍射确定。为此,在环境温度下将代表性量的样品分散在脱气水中(样品的自饱和),声处理(通常为60秒),然后在Malvern Mastersizer系列仪器中进行测量。借助多元素检测器以不同的角度测量散射光,并记录相关的数值。借助弗劳恩霍夫模型根据散射数据计算特定粒径等级的比例,并由此计算体积加权粒径分布。报告值通常是d50和d90值=活性成分的粒径(颗粒总体积的50%和90%)。中值粒径是指d50值。
分散相A)的颗粒的粒径d50优选为1-50pm(微米)、特别优选1-20pm,非常特别优选2—15gm。
本发明同样提供了一种制备本发明的胶囊悬浮浓缩物的方法,其特征在于包括以下工艺步骤:
I.制备有机相A')
II.制备水相B)
III.制备在B')中的A')的乳液
IV.任选地添加组分a1.1)(当a1.1.不是水时)
V.加热步骤
VI.完成。
在步骤(I)中,将活性成分a2.1)和其他添加剂a3.1)溶解在有机溶剂a2.2)中,同时搅拌。本发明的方法的步骤(I)通常在0℃至80℃,优选0℃至50℃,更优选2℃至40℃的温度下进行。然后将异氰酸酯a1.2)添加到所得混合物中。添加可以例如通过直接添加到混合物中或借助通常用于此类目的的设备(例如静态混合器)连续计量加入,添加在与水相B)合并之前不久进行。
在步骤(II)中,将至少一种保护胶体b1.1)和任选的其他添加剂b1.2)溶解在水中,同时搅拌。该步骤通常在0℃至80℃,优选15℃至80℃的温度下进行。
在步骤(III)中,将有机相A)加入到水相B)中并制备乳液。可以使用所有通常用于此类目的的产生强剪切力的设备来制备。实例包括转子/定子混合器和喷射分散器。步骤(III)通常在0℃至80℃,优选10℃至75℃的温度下进行。乳液的制备可以分批或连续进行。
在根据本发明的方法的步骤(IV)中,由步骤(III)获得的乳液在步骤(IV)中与二胺、多胺、二醇、多元醇和/或氨基醇a1.1)在搅拌下混合。胺或醇组分a1.1)在此方便地以水溶液形式添加。然而,在根据本发明的方法中,优选仅使用水作为组分a1.1),如上所述,其在本发明的上下文中理解为组分a1.1由异氰酸酯与水的水解形成。因此,此处的“水"是指水解产物(胺)。
在步骤(V)中,将混合物在搅拌下加热一定时间,以确保反应已经完成。时间段通常为0至24小时,优选0.5至8小时,更优选1至5小时,该反应优选在0℃至80℃,优选20℃至75℃的温度下进行。
在步骤(VI)中,胶囊悬浮液在导致胶囊形成的反应结束时达到室温,然后任选地在搅拌下进一步与添加剂b1.2')混合。添加剂b1.2')原则上可以根据需要在步骤(II)或步骤(VI)中添加。
本发明的方法优选在大气压下进行。
在根据本发明的方法的实施中,来自组分a1.2)的NCO基团与来自组分a1.1)的NCO-反应基团的比例可以在特定范围内变化。优选地,每1mol异氰酸酯使用0至1.5当量添加的胺或醇组分。优选地,不使用交联剂,即a1-1)通过异氰酸酯与水(或为根据上述定义的“水")的水解形成。
在另一个实施方案中,每1mol异氰酸酯使用0.1至1.5当量添加的胺或醇组分。
根据所使用的成壳成分a1.1)和a.1.2)的量和所得的粒径,可以根据胶囊的平均粒径(d50)和成壳材料的用量粒径计算出胶囊的理论壁的厚度,聚合物的密度设置为1(1g/cm3)。在本发明的胶囊悬浮浓缩物的胶囊中计算的壁的厚度优选为0.001至4lam,更优选0.01至2lam,且特别优选0.01至1lam·
在a1.1)与a1.2)的反应中,异氰酸酯基团和异氰酸酯反应基团的数均官能度x的总和为2苎x苎6,优选2<X<4.5,特别优选2.0苎x苎3.5,非常特别优选2.2<X<2.8o
作为根据本发明的方法中的特征的“数均官能度x"如下所示。这里的关键是具有更高官能度的化合物;将低官能度的化合物减2后得到的值加到高官能度的化合物中。例如,如果a1-1)的(平均)官能度为2.1,a1.2)为2.6,则得出:2.1-2=0.1。这个差值加到2.6上:2.6+0.1=2.7。因此,数均官能度为2.7。或者,如果a1)为2.7,a2)为2.3,则所得的数均官能度为2.7+2.3-2=3.0。
具有异氰酸酯反应基团的有用化合物a1.1')包括脂族、芳族、环族和脂环族伯二胺和仲二胺,以及多胺。实例包括乙二胺(EDA)、二乙烯三胺(DETA)、单异丙胺、4一氨基吡啶(4-AP)、正丙胺、乙烯基或丙烯亚胺基聚氮丙啶、三乙烯四胺(TETA)、四乙烯五胺、2,4,4'-三氨基二苯醚、双(六亚甲基)三胺、三亚甲基二哌啶(TMDP)、碳酸胍(GUCA)、苯二胺、甲苯二胺、五亚甲基六胺、2,4-.=-氨基一6甲基-1,3,5-三嗪、1,2一二氨基环己烷、4,4’一二氨基二苯甲烷、1,5一二氨基萘异佛尔酮二胺、二氨基丙烷、二氨基丁烷、哌嗪、氨基乙烯哌嗪(AEP)、聚(丙二醇)双(2一氨基丙基醚)或O,O’一双(2一氨基丙基)聚丙二醇嵌段聚乙二醇嵌段聚丙二醇、六亚甲基二胺、双(3一氨基丙基)胺、双(2一甲基氨基乙基)甲胺、1,4-二氨基环己烷、3一氨基一1一甲基氨基丙烷、N一甲基双(3一氨基丙基)胺、1,4-二氨基一正丁烷和1,6一二氨基一正己烷。优选六亚甲基二胺和二亚乙基三胺。
具有异氰酸酯反应基团的有用化合物a1)同样包括伯和仲、脂族和芳族二醇和多元醇。实例包括:乙二醇、丙二醇(1,2)、丙二醇(1,3)、丁二醇(1,4)、戌二醇(1,5)、己二醇(1,6)、甘油和二甘醇。优选使用甘油和丙烷-1,2-.二醇。
具有异氰酸酯反应基团的化合物a1.1')还包括氨基醇。实例包括三乙醇胺、单乙醇胺、三异丙醇胺、二异丙胺、N一甲基乙醇胺、N一甲基二乙醇胺。
在一个非常特别优选的实施方案中,仅将水用作异氰酸酯反应组分a1.1)。其与(聚/二)异氰酸酯原位反应生成(聚/二)胺,然后其本身具有异氰酸酯反应性·
同样可以使用a1.1')的混合物。
异氰酸酯或异氰酸酯混合物a1.2)是单、二和/或多异氰酸酯混合物,或异氰酸酯混合物的反应产物。合适的化合物a1.2')是例如丁烯1,4-二-异氰酸酯、六亚甲基1,6一二异氰酸酯(HDI')、异佛尔酮二异氰酸酯(IPDI')、2,2,4-和/或2,4,4-三甲基六亚甲基二异氰酸酯、异构双(4,4t一异氰酸环己基)甲烷(H12-MDI')及其与任何异构体含量的混合物、1,4-二-异氰酸环己酯、1,8一二异氰酸4一异氰酸甲基辛酯(壬烷三异氰酸酯)、1,4一二异氰酸亚苯酯、2,4-和/或2,6一甲苯一二异氰酸酯(TDI')、亚萘基1,5-二-异氰酸酯、二苯基甲烷2,2'-和/或2,4’和/或4,4’一二异氰酸酯(MDI)、1,3一和/或1,4一双(2一异氰酸根合丙基-2-基)苯(TMXDI)、1,3-叉iZ(异氰酸根合甲基)苯(xDI)、具有1至8个碳原子的烷基的2,6-.=-异氰酸根合己酸烷基酯(赖氨酸二异氰酸酯)及其混合物。含有改性的化合物,如脲基甲酸酯、脲二酮、氨基甲酸乙酯、异氰脲酸酯、缩二脲、亚氨基憾二嗪二酮或憾二嗪三酮结构,并且基于所述二异氰酸酯也是适合于组分a1.2)的结构单元,多环化合物也是如此,例如聚合MDI(pMDI,例如来自Covestro AG的Dow或Desmodur四44V20产品的PAPI-27)以及上述的结合。
优选使用异氰酸酯(NCO)官能度为2至6,优选2.0至4.5,特别优选2.3至4.2,非常特别优选2.3至3.8的改性剂。特别优选的是NCO官能度为2.4至3的改性剂。
优选使用选自HDI、IPDI、H12-MDI、TDI和MDI的二异氰酸酯进行改性。特别优选HDI、TDI和MDI及其衍生物。特别优选地,MDI以聚合MDI的形式使用,例如PAPI-270
异氰酸酯或多异氰酸酯或共混物的优选NCO含量为按重量计3%至50%,特别优选按重量计10%至40%,特别优选按重量计15%至35%,非常特别优选按重量计20%至35%。异氰酸酯基团也可以在它们与异氰酸酯反应基团反应之前以部分或完全封闭的(blocked)形式存在,以这种方式它们不能立即与异氰酸酯反应基团反应。这确保了在达到特定温度(封闭温度)之前不会发生反应。典型的封闭剂可以在现有技术中找到并且被选择为在60至220℃的温度下,它们会再次从异氰酸酯基团中消除,这取决于物质,只有那时才与异氰酸酯反应基团反应。有结合到聚氨基甲酸乙酯中的封闭剂,也有作为溶剂或增塑剂保留在聚氨基甲酸乙酯中的封闭剂,或作为气体从聚氨基甲酸乙酯中释放出来的封闭剂。有时会使用“封闭NCO值"这一表述。当在本发明中使用表述"NCO值"时,这常指未封闭NCO值。通常的封闭程度高达<0.5%。典型的封闭剂的实例是己内酰胺,甲基乙基酮肟,吡唑类,例如3,5-二甲基1,2-nt:唑或吡唑,三唑类,例如1,2,4-三唑、二异丙胺、丙二酸二乙酯、二乙胺、苯酚及其衍生物,以及咪唑。
组分a1.2')也可以以上述化合物的混合物或预聚物的形式使用。在这种情况下,例如,含有异氰酸酯基团且NCO含量为按重量计3%至50%的化合物与含有异氰酸酯反应基团且OH值为10mg KOH/g至150mg KOH/g的化合物反应。
特别优选仅使用一种异氰酸酯而不使用混合物。
有用的有机溶剂a2.2')包括所有与水不混溶(相分离)但容易溶解所用农业化学活性成分的常规有机溶剂。优选的实例包括任选地被卤化的脂肪烃和芳香烃,例如甲苯、二甲苯、Solvesso 100、IOOND、150、150ND或200、200ND(矿物油)、四氯甲烷、氯仿、二氯甲烷和二氯乙烷,酯类,例如乙酸乙酯,以及烷烃甲酰胺,例如N,N-二-甲基辛酰胺和N,N-.=-甲基癸酰胺。还有基于例如菜籽油、玉米仁油、椰子油等的植物油和改性油(例如通过甲基化、乙基化以及氢化和水合)。特别优选使用矿物油,非常特别优选使用基于二烷基萘的溶剂(例如二异丙基萘),以及1一甲基萘和2一甲基萘以及萘的混合物(例如Solvesso 200ND产品,CAS No.:64742-94-5)。
原则上也可以使用有机溶剂a2.2')的混合物。优选仅使用一种溶剂。
有用的其他添加剂a3.1')包括所有油溶性表面活性添加剂。特别优选烷基乙氧基化物、烷基丙氧基乙氧基化物、脱水山梨糖醇和甘油的脂肪酸酯以及有机改性三硅氧烷。非常特别优选烷基乙氧基化物和烷基丙氧基乙氧基化物。特别优选具有末端羟基官能团的烷基乙氧基化物和烷基丙氧基乙氧基化物。实例包括Vibrant、Synergen W06、Genapol EP2584和Genapol X 060。
本发明的胶囊悬浮浓缩物的水相B')除了水之外还包含至少一种保护胶体b1.1)并且可以包含其他添加剂b1.2),例如乳化剂、防腐剂、消泡剂、冷稳定剂、增稠剂、pH稳定剂和中和剂·
有用的保护胶体b1-1')(分散相A的乳化剂)包括通常用于此目的的所有物质。优选的实例包括天然和合成的水溶性聚合物,例如明胶、淀粉和纤维素衍生物,特别是纤维素酯和纤维素醚,例如甲基纤维素,以及聚乙烯醇、部分水解的聚乙酸乙烯酯(皂化度<98%)、木质素磺酸盐(例如NA、88或Kraftsperse 25S)、改性萘磺酸盐(例如D-425)、聚乙烯吡咯烷酮和聚丙烯酰胺。特别优选使用聚乙烯醇、部分水解的聚乙酸乙烯酯和木质素磺酸盐。非常特别优选聚乙烯醇、部分水解的聚乙酸乙烯酯和木质素磺酸盐。
有用的增稠剂b1.2)包括有机增稠剂和无机增稠剂。有用的有机增稠剂包括有机天然或生物技术改性或有机合成的增稠剂。典型的合成增稠剂是(croda)和Thixin或Thixatrol系列(Elementis)。这些通常基于丙烯酸酯。典型的有机增稠剂基于黄原胶或纤维素(例如羟乙基纤维素或羧甲基纤维素)或其结合。其他典型代表物基于纤维素或木质素。优选使用基于黄原胶的天然改性增稠剂。典型代表物例如是(Solvay)和(Kelco Corp.),以及(Cargill)。无机增稠剂通常基于二氧化硅或粘土矿物。
有用的防腐剂b1.2)包括作物保护组合物中通常为此目的而存在的所有物质,例如二氯酚、苯甲醇半缩甲醛、5一氯一2一甲基-4-异噻唑啉一3一酮【CAS No.26172-55-4】、2一甲基一4一异噻唑啉-3-酮【CAS No.2682-20-4】或1.2-苯并异噻唑一3(2H)一酮【CASNo.2634-33-5】。实例包括Acticide SPX(Thor)、Proxel GXL(Lonza)、Preventol D7或Kathon CG/ICP。
有用的消泡剂b1.2)包括作物保护组合物中通常可用于此目的的所有物质。优选硅烷衍生物,例如聚二甲基硅氧烷和硬脂酸镁。484、426R、SRE(Solvay,Silioxane Emulsion)和1571(Momentive)被用作典型产品。
充当冷稳定剂b1.2)的物质可以是作物保护组合物中通常可用于此目的的所有物质。实例包括尿素、甘油和丙二醇。
有用的中和剂b1.2')包括常用的酸和碱。实例包括磷酸、柠檬酸、氢氧化钠溶液和氨水溶液。
本发明的胶囊悬浮浓缩物的组成可以在特定范围内变化。基于整个制剂的分散相A)的比例通常为按重量计10%至90%,优选按重量计30%至70%,更优选按重量计40%至60%o
基于整个制剂的a1.2')的比例通常为按重量计0.1%至8%,优选按重量计0.2%至4.5%,更优选按重量计0.5%至4%。
在一个替代的优选实施方案中,a1.2)基于整个制剂的比例通常为按重量计0.1%至2%,优选按重量计0.2%至2%,更优选按重量计0.5%至2%。
基于整个制剂的农业化学活性成分a2.1')的比例通常为按重量计1%至50%,优选按重量计5%至40%,更优选按重量计5%至15%。
基于整个制剂的有机溶剂a2.2')的比例通常为按重量计1%至90%,优选按重量计10%至60%,更优选按重量计25%至40%。
基于整个制剂的添加剂a3.1)的比例通常为按重量计0.1%至10%,优选按重量计0.5%至5%,更优选按重量计1%至5%,非常特别优选按重量计2%至5%o
基于整个制剂的保护胶体b1.1)的比例通常为按重量计0.1%至5%,优选按重量计0.2%至3%,更优选按重量计0.2%至1%,添加剂b1.2)的比例通常为按重量计0.1%至15%,优选按重量计0.2%至10%,更优选按重量计0.3%至3%o
a1.2)与总有机相A)的比例优选为40:1至60:1,更优选45:1至60:1,特别优选45:1至55:1。如果有机相A)中的a1-1)是水,则与异氰酸酯反应所需的水不计入有机相。
关于各成分的上述比例,本领域技术人员将清楚,各成分的优选范围可以自由地相互结合,因此这些具有各成分不同优选范围的组合物也被认为是已披露。
然而,除非另有说明,否则特别优选相同水平的优选范围,即例如所有优选或更优选的范围,具体的公开内容并非旨在取代这些一般结合,而是增加于其中。
这同样适用于本说明书中其他位置的优选范围的其他说明。
在优选的实施方案中,a1.2)的比例为按重量计0.1%至8%,
农业化学活性成分a2.1)的比例为按重量计1%至50%,
有机溶剂a.2.2)的比例为按重量计1%至90%,
添加剂a3.1')的比例为按重量计0.1%至10%,
保护胶体b1.1')的比例为按重量计0.1%至5%,
以及添加剂b1.2)的比例为按重量计0.1%至15%o
在一个替代的实施方案中,a1.2)的比例为按重量计0.2%至4.5%,
农业化学活性成分a2.1)的比例为按重量计5%至40%,
有机溶剂a.2.2)的比例为按重量计10%至60%,
添加剂a3.1')的比例为按重量计0.5%至5%,
保护胶体b1.1')的比例为按重量计0.2%至3%,
以及添加剂b1.2)的比例为按重量计0.2%至10%。
在替代的实施方案中,a1.2)的比例为按重量计0.5%至4.0%,
农业化学活性成分a2.1)的比例为按重量计5%至15%,
有机溶剂a.2.2)的比例为按重量计25%至40%,
添加剂a3.1)的比例为按重量计2%至5%,
保护胶体b1.1)的比例为按重量计0.2%至1%,
以及添加剂b1.2)的比例为按重量计0.3%至3%o
在一个优选的实施方案中,a1.2)的比例为按重量计0.1%至2%,
农业化学活性成分a2.1)的比例为按重量计1%至50%,
有机溶剂a.2.2)的比例为按重量计1%至90%,
添加剂a3.1')的比例为按重量计0.5%至5%,
保护胶体b1.1')的比例为按重量计0.1%至5%,
以及添加剂b1.2)的比例为按重量计0.1%至15%o
在一个替代的实施方案中,a1.2)的比例为按重量计0.2%至2%,
农业化学活性成分a2.1)的比例为按重量计5%至40%,
有机溶剂a.2.2)的比例为按重量计10%至60%,
添加剂a3.1)的比例为按重量计1%至5%,
保护胶体b1.1')的比例为按重量计0.2%至3%,
以及添加剂b1.2)的比例为按重量计0.2%至10%o
在一个替代的实施方案中,a1.2)的比例为按重量计0.5%至2%,
农业化学活性成分a2.1)的比例为按重量计5%至15%,
有机溶剂a.2.2')的比例为按重量计25%至40%,
添加剂a3.1')的比例为按重量计2%至5%,
保护胶体b1.1')的比例为按重量计0.2%至1%,
以及添加剂b1.2)的比例为按重量计0.3%至3%·
优选地,农业化学活性成分a2.1)与异氰酸酯或异氰酸酯混合物a1.2)的比例为1:1至30:1,优选1:1至15:1,更优选2:1至10:1o
当氨基官能化合物用作组分a1.1)时,氨基异氰酸酯反应基团a1.1)与异氰酸酯混合物a1.2)的比例为0至1.5,优选0至1,更优选0至0.5,特别优选0至0.3。非常特别优选地,其为0,即不使用氨基官能化合物a1.1),而水代替用作异氰酸酯反应基团。
此外,上述实施方案中的有机溶剂a2.2)优选为矿物油,更优选为基于二烷基萘(例如二异丙基萘)、1一甲基萘和2一甲基萘以及萘的混合物(例如Solvesso 200ND产品,CAS号:64742-94-5)的溶剂,非常特别优选1一甲基萘和2一甲基蔡以及萘的混合物作为溶剂。
原则上可以将根据本发明的制剂与其他制剂混合以结合两种或更多种活性成分。例如,本发明可以与水基制剂例如SC、SL或其他CS结合。
拟除虫菊酯是基于天然杀虫剂中存在的主要活性物质的合成杀虫剂。
优选合适的拟除虫菊酯,其选自氟丙菊酯(acrinathrin)、烯丙菊酯(allethrin)、d一顺式一反式烯丙菊酯(d-cis-trans allethrin)、d一反式烯丙菊酯(d-transallethrin)、联苯菊酯(bifenthrin)、生物烯丙菊酯(bioallethrin)、生物烯丙菊酯S一环戌烯基异构体(bioallethrin S-cyclopentenyl isomer)、生物苄呋菊酯(bioresmethrin)、乙氰菊酯(cycloprothrin)、氟氯氰菊酯(cyfiuthrin)、p一氟氯氰菊酯(beta-cyfiuthrin)、三氟氯氰菊酯(cyhalothrin)、久一三氟氯氰菊酯(1ambda-cyhalothrin)、Y一三氟氯氰菊酯(gamma-cyhalothrin)、氯氰菊酯(cypermethrin)、旺一氯氰菊酯(alpha-cypermethrin)、p一氯氰菊酯(beta-cypermethrin)、0一氯氰菊酯(theta-cypermethrin)、‘一氯氰菊酯(zeta-cypermethrin)、苯醚氰菊酯【(1R)一反式异构体】(cyphenothrin【(1R)-trans isomer】)、溴氰菊酯(deltamethrin)、烯炔菊酯【(EZ)一(1R)异构体】(empenthrin【(EZ)一(1R)isomer】)、氰戌菊酯(esfenvalerate)、醚菊酯(etofenprox)、甲氰菊酯(fenpropathrin)、氰戌菊酯(fenvalerate)、氟氰戌菊酯(nucythrinate)、氟氯苯菊酯(numethrin)、氟胺氰菊酯(tau-fiuvalinate)、苄螨醚(halfenprox)、咪炔菊酯(imiprothrin)、噻嗯菊酯(kadethrin)、momfluorothrin、氯菊酯(permethrin)、苯醚菊酯【(1R)一反式异构体】(phenothrin【(1R)-trans isomer】)、炔丙菊酯(prallethrin)、除虫菊酯(pyrethrins)(除虫菊(pyrethrum))、卞呋菊酯(resmethrin)、氟硅菊酯(silafiuofen)、七氟菊酯(tefiuthrin)、胺菊酯(tetramethrin)、胺菊酯【(1R)异构体】(tetramethrin【(1R)isomer】)、四溴菊酯(tralomethrin)、四氟苯菊酯(transfiuthrin')和甲氧氯(methoxychlor')o
更优选为溴氰菊酯、p一氟氯氰菊酯、氯氰菊酯和久一三氟氯氰菊酯,特别优选溴氰菊酯。
此外,在替代的实施方案中,胶囊悬浮浓缩物可以包含其他杀虫剂、杀螨剂和/或杀线虫剂,例如也是由上述药物与另一种制剂混合的结果。
可用于本发明的上下文中的杀虫剂、杀螨剂和/或杀线虫剂——在此通常以其通用名称来指代——是已知的并记载于例如“The Pesticide Manual",16th ed.,BritishCrop Protection Council 2012,或可在网站(例如WWW.alanwood.net/pesticides)上检索。该分类以提交该专利申请时适用的IRAC作用方式分类方案为基础。
(1)乙酰胆碱酯酶(Ace锣lcholinesterase)(AChE)抑制剂,优选氨基甲酸酯,选自:棉铃威(alanycarb)、涕灭威(aldicarb)、憾虫威(bendiocarb)、丙硫克百威(benfuracarb)、丁酮威(butocarboxim)、丁酮砜威(butoxycarboxim)、甲萘威(carbaryl)、克百威(carbofuran)、丁硫克百威(carbosulfan)、乙硫苯威(ethiofencarb)、仲丁威(fenobucarb)、伐虫脒(formetanate)、呋线威(furathiocarb)、异丙威(isoprocarb)、甲硫威(methiocarb)、灭多威(methomyl)、速灭威(metolcarb)、杀线威(0xamyl)、抗蚜威(pirimicarb)、残杀威(propoxur)、硫双威(thiodicarb)、久效威(thiofanox)、唑蚜威(triazamate)、混杀威(trimethacarb)、XMC和灭杀威(xylylcarb);或有机磷酸酯类,选自乙酰甲胺磷(acephate)、甲基吡恶磷(azamethiphos)、益棉磷(azinphos-ethyl)、保棉磷(azinphos-methyl)、硫线磷(cadusafos)、氯氧磷(chlorethoxyfos)、毒虫畏(chlorfenvinphos)、氯甲硫磷(chlormephos)、甲基毒死蜱(chlorpyrifos-methyl)、蝇毒磷(coumaphos)、杀螟腈(cyanophos)、甲基内吸磷(demeton-S-methyl)、二嗪农(diazinon)、敌敌畏(dichlorvos/DDVP)、百治磷(dicrotophos)、乐果(dimethoate)、甲基毒虫畏(dimethylvinphos)、乙拌磷(disulphoton)、苯硫磷(EPN)、乙硫磷(ethion)、灭线磷(ethoprophos)、伐灭磷(famphur)、苯线磷(fenamiphos)、杀螟硫磷(fenitrothion)、倍硫磷(fenthion)、噻唑酮磷(fosthiazate)、庚烯磷(heptenophos)、imicyafos、异柳磷(isofenphos)、o一(甲氧基氨基硫代磷酰基)水杨酸异丙酯(isopropyl o一(methoxyaminothiophosphoryl)salicylate)、恶唑磷(iSOXathion)、马拉硫磷(malathion)、灭蚜磷(mecarbam)、甲胺磷(methamidophos)、杀扑磷(methidathion)、速灭磷(mevinphos)、久效磷(monocrotophos)、二溴磷(naled)、氧乐杲(omethoate)、亚矾磷(oxydemeton-methyl)、甲基对硫磷(parathion-methyl)、稻丰散(phenthoate)、甲拌磷(phorate)、伏杀硫磷(phosalone)、亚胺硫磷(phosmet)、磷胺(phosphamidon)、辛硫磷(phoxim)、嘧啶磷(pirimiphos-methyl)、丙溴磷(profenofos)、胺丙畏(propetamphos)、丙硫磷(prothiofos)、吡唑硫磷(pyraclolos)、哒嗪硫磷(pyridaphenthion)、喹憾磷(quinalphos)、治螟磷(sulfotep)、丁基嘧啶磷(tebupirimfos)、双硫磷(temephos)、特丁硫磷(terbufos)、杀虫畏(tetrachlorvinphos)、甲基乙拌磷(thiometon)、三唑磷(triazophos)、敌百虫(triclorfon)和蚜灭磷(vamidothion)o
(2)GABA门控氯化物通道阻断剂,优选环戌二烯一有机氯类,选自氯丹(chlordane)和硫丹(endosulfan);或苯基吡唑类(phenylpyrazoles(fiproles)),选自乙虫腈(ethiprole)和氟虫腈(fipronil)。
(4)烟碱乙酰胆碱受体(nAChR)竞争性调节剂,优选新烟碱类(neonicotinoids),选自啶虫脒(acetamiprid)、噻虫胺(clothianidin)、呋虫胺(dinotefuran)、吡虫啉(imidacloprid)、烯啶虫胺(nitenpyram)、噻虫啉(thiacloprid)和噻虫嗪(thiamethoxam),或烟碱(nicotine),或亚砜亚胺类(sulfoximine),选自氟啶虫胺腈(sulfoxaflor),或丁烯羟酸内酯类(butenolide),选自氟吡呋喃酮(nupyradifurone),或介离子类(mesoionic),选自三氟苯嘧啶(triflumezopyrim')。
(5)烟碱乙酰胆碱受体(nAChR)变构调节剂,优选多杀霉素类(spinosyns),选自乙基多杀菌素(spinetoram)和多杀菌素(spinosad)。
(6)谷氨酸门控氯化物通道(GluCl)变构调节剂,优选阿维菌素类(avermectins)/米尔贝霉素类(milbemycins),选自阿维茵素(abamectin)、甲氨基阿维菌素苯甲酸盐(emamectin benzoate)、雷皮菌素(1epimectin)和米尔倍霉素(milbemycin')o
(7')保幼激素类似物类,优选保幼激素类似物,选自烯虫乙酯(hydroprene)、烯虫炔酯(kinoprene)和烯虫酯(methoprene)、或苯氧威(fenoxycarb)或吡丙醚(pyriproxifen)。
(8)各类非特异性(多位点)抑制剂,优选卤代烃,选自甲基溴和其他卤代烃:或氯化苦(chloropicrine)或磺酰基氟化物(sulphuryl fluoride)或硼砂(borax)或吐酒石(tartar emetic)或异氰酸甲酯生成剂,选自棉隆(diazomet)和威百亩(metam)。
(9)弦音器TRPV通道调节剂,选自吡蚜酮(pymetrozine)和氟啶虫酰胺(nonicamid)。
(10)螨生长抑制剂,选自四螨嗪(ciofentezine)、噻螨酮(hexythiazox)和氟螨嗪(diflovidazin')和乙螨唑(etoxazole')。
(11)昆虫肠膜的微生物干扰剂,选自苏云金芽孢杆菌以色列亚种溻aci!!us thuringiensis subspecies israelensis)、球形芽孢杆菌溻aci!!us sphaericus)、苏云金芽胞杆菌鲇泽亚种溻aci!!us thuringiensis subspecies aizawaO、苏云金芽孢杆菌库尔斯塔克亚种溻aci!!us踊跖吻曙缸珊妇subspecies kurstakO、苏云金芽孢杆菌拟步行甲亚种溻aci!!us thuringiensis subspecies tenebrionis),以及B.t.植物蛋白,选自:CrylAb、CrylAc、CrylFa、CrylA.105、Cry2Ab、Vip3A、mCry3A、Cry3Ab、Cry3Bb和Cry34Abl/35Abl。
(12)线粒体ATP合酶抑制剂,优选ATP干扰剂类,选自丁醚脲(diafenthiuron),或有机锡化合物,选自三唑锡(azocyclotin)、三环锡(cyhexatin)以及苯丁锡(fenbutatinoxide),或炔螨特(propargite)或三氯杀螨砜(tetradifon)。
(13)通过破坏质子梯度的氧化磷酸化解偶联剂,选自虫螨腈(chlorfenapyr)、二硝甲酚(DNOC)和氟虫胺(sulfiuramid)。
(14)烟碱乙酰胆碱受体通道阻断剂,选自杀虫磺(bensultap)、杀螟丹盐酸盐(cartap hydrochloride)、杀虫环(thiocylam)和杀虫双(thiosultap-sodium)。
(15)0型几丁质生物合成抑制剂,选自双三氟虫脲(bistrifiuron)、氟啶脲(chlofiuazuron)、除虫脲(difiubenzuron)、氟环脲(nucycloxuron)、氟虫脲(nufenoxuron)、氟铃脲(hexaflumuron)、虱螨脲(1ufenuron)、氟酰脲(novaluron)、多氟脲(novifiumuron)、氟苯脲(tefiubenzuron)和杀铃脲(trifiumuron)。
(16)1型几丁质生物合成抑制剂,选自噻嗪酮(buprofezin)。
(17)蜕皮干扰剂类(特别是双翅目(Diptera)),选自灭蝇胺(cyromazine)。
(18)蜕皮激素受体激动剂,选自环虫酰肼(chromafenozide)、氯虫酰肼(halofenozide)、甲氧虫酰肼(methoxyfenozide)和虫酰肼(tebufenozide)。
(19)章鱼胺受体激动剂,选自双甲脒(amitraz)。
(20)线粒体复合体III电子转移抑制剂,选自灭蚁腙(hydramethylnone)、灭螨醌(acequinocyl)和嘧螨酯(nuacrypyrim)。
(21)线粒体复合体I电子转移抑制剂,优选METI杀螨剂,选自喹螨醚(fenazaquin)、唑螨酯(fenpyroximate)、嘧螨醚(pyrimidifen)、哒螨灵(pyridaben)、吡螨胺(tebufenpyrad)和唑虫酰胺(tolfenpyrad),或鱼藤酮(rotenone)(雨藤(Derris))。
(22)电位依赖性钠通道阻断剂,选自茚虫威(indoxacarb)和氰氟虫胺(metaflumizone)。
(23)乙酰辅酶A羧化酶抑制剂,优选特窗酸(tetronic acid)和特胺酸(tetramicacid)衍生物,选自螺螨酯(spirodiclofen)、螺甲螨酯(spiromesifen)和螺虫乙酯(spirotetramate)o
(24)线粒体复合体IV电子转移抑制剂,优选膦类化合物,选自磷化铝、磷化钙、膦和磷化锌,或氰化物,例如氰化钙、氰化钾和氰化钠。
(25)线粒体复合体II电子转移抑制剂,优选p一开托利(beta-ketonitrile)衍生物,选自唑螨氰(cyenopyrafen)和丁氟螨酯(cyfiumetofen),或羧酰替苯胺类(carboxanilides),选自pyfiubumide。
(28)兰尼碱(ryanodine)受体调节剂,优选二酰胺,选自氯虫酰胺(chlorantraniliprole)、溴氰虫酰胺(cyantraniliprole)和氟虫酰胺(nubendiamide)。
(29)弦音器调节剂(具有未定义的目标结构),选自氟啶虫酰胺(nonicamid)。
(30)其他活性化合物,选自acynonapyr、双丙环虫酯(Afidopyropen)、阿福拉纳(Afoxolaner)、印楝素(Azadirachtin)、Benclothiaz、苯螨特(Benzoximate)、benzpyrimoxan、联苯肼酯(Bifenazate)、溴虫氟苯双酰胺(Brofianilide)、溴螨酯(Bromopropylate)、灭螨猛(Chinomethionat)、右旋反式氯丙炔菊酯(Chloroprallethrin)、冰晶石(Cryolite)、环溴虫酰胺(Cyclaniliprole)、环氧虫啶(Cycloxaprid)、氯氟氰虫酰胺(Cyhalodiamide)、二氯噻吡嘧啶(Dicloromezotiaz)、三氯杀螨醇(Dicof01)、dimpropyridaz、£一甲氧苄氟菊酯(epsilon Metofiuthrin)、£-Momfluthrin、Flometoquin、三氟咪啶酰胺便luazaindolizine)、联氟砜便luensulfone)、嘧虫胺便lufenerim)、氟茵螨酯(Flufenoxystrobin)、丁虫腈(Flufiprole)、Fluhexafon、氟吡菌酰胺(Fluopyram)、flupyrimin、氟雷拉纳(Fluralaner)、Fluxametamide、呋喃虫酰肼(Fufenozide)、戊吡虫胍(Guadipyr)、七氟甲醚菊酯(Heptafiuthrin)、氯噻啉(Imidaclothiz)、异茵脲(Iprodione)、isocycloseram、K一联苯菊酯(kappa Bifenthrin)、K一七氟菊酯(kappa Tefiuthrin)、洛替拉纳(Lotilaner)、荚氟菊酯(Meperfiuthrin)、oxazosul锣l、哌虫啶(Paichongding)、三氟甲吡醚(Pyridalyl)、氟虫吡喹(Pyrifiuquinazon)、嘧螨胺(Pyriminostrobin)、螺螨双酯(Spirobudiclofen)、甲氧哌啶乙酯(spiropidion)、四氟醚菊酯(Tetramethylfiuthrin)、四唑虫酰胺(Tetraniliprole')、四氮虫酰胺(Tetrachlorantraniliprole')、Tigolaner、Tioxazafen、硫氟肟醚(Thiofiuoximate)和碘甲烷(Iodomethane);其他基于坚硬芽孢杆菌的制剂(I-1582,BioNeem,Votivo),以及以下化合物:1一{2一氟一4一甲基一5一【(2,2,2-三氟乙烷)亚磺酰基】苯基}一3一(三氟甲基)一1H-1,2,4一三唑-5-胺(由WO 2006/043635获知)(CAS885026-50-6)、{1’一【(2E)-3-(4一氯苯基)丙一2一烯一1一基】一5一氟螺环门l哚-3,4'一哌啶】一1(2H)一基}(2一氯吡啶-4-基)甲酮(由WO 2003/106457获知)(CAS 637360-23-7)、2一氯一N一【2一{1一【(2E)-3-(4一氯苯基)丙一2一烯一1一基】哌啶一4一基}一4一(三氟甲基)苯基】异烟酰胺(由WO2006/003494获知)(CAS 872999-66-1)、3一(4一氯-2,6-二甲基苯基)一4一羟基一8一甲氧基-1,8-二氮杂螺环【4.5】癸-3-烯-2-酮(由WO 2010/052161获知)(CAS1225292—17-0)、3一(4一氯-2,6-.二甲基苯基)一8一甲氧基一2一氧代一1,8一二氮杂螺环【4.5】癸-3-烯-4-基乙基碳酸酯(由EP 2647626获知)(CAS 1440516-42-6)、4一(丁-2-炔一1一氧基)一6一(3,5一二甲基哌啶-1-基)一5一氟嘧啶(由WO 2004/099160获知')(CAS 792914-58-0')、PFl364(由JP 2010/018586获知')(CAS登记号1204776-60-2)、(3E)一3一【1一【(6一氯-3-吡啶基)甲基】一2一毗啶亚基卜1,1,1-三氟一丙一2一酮(由W02013/144213获知)(CAS 1461743—15-6)、N一【3一(苄氧基氨基甲酰基)一4一氯苯基】一1一甲基-3-(五氟乙基)一4一(三氟甲基)一1H-吡唑一5一甲酰胺(由WO 2010/051926获知)(CAS 1226889-14-0)、5一溴一4一氯-N-【4一氯一2一甲基一6一(甲基氨基甲酰基)苯基】一2一(3一氯一2一吡啶基)吡唑一3一甲酰胺(由CN103232431获知)(CAS 1449220-44-3)、4一【5一(3,5一二氯苯基)一4,5-二-氢-5-(三氟甲基)一3一异憾唑基】一2一甲基-N-(顺式一1一氧化(oxido)一3_硫杂环丁基)一苯甲酰胺、4一【5一(3,5一二氯苯基)一4,5-二-氢-5-(三氟甲基)一3一异憾唑基】一2一甲基-N-(反式一1一氧化-3-硫杂环丁基)一苯甲酰胺和4一【(5S)-5-(3,5一二氯苯基)一4,5一二氢一5一(三氟甲基)一3一异憾唑基】一2一甲基-N-(顺式一1一氧化-3-硫杂环丁基')一苯甲酰胺(由WO 2013/050317A1获知')(CAS 1332628-83-7')、N一『3一氯-1-(3一吡啶基)一1H-qt:唑-4-基卜N一乙基一3一【(3,3,3-三氟丙基)亚磺酰基卜丙酰胺、(+)一N一【3一氯-1-(3一吡啶基)一1H-吡唑-4-基卜N一乙基一3一【(3,3,3-三氟丙基)亚磺酰基卜丙酰胺和(一)一N一【3一氯一1一(3一吡啶基)一1H一吡唑一4一基卜N一乙基一3一【(3,3,3一三氟丙基)亚磺酰基卜丙酰胺(由WO 2013/162715A2、WO2013/162716A2、US2014/0213448A1获知)(CAS 1477923-37-7)、5一II(2E)一3一氯一2一丙烯一1一基】氨基】一1一【2,6一二氯-4-(三氟甲基)苯基】一4一【(三氟甲基)亚磺酰基】一1H一吡唑一3一甲腈(由CN 101337937 A获知)(CAS 1105672-77-2)、3一溴一N一【4一氯一2一甲基一6一【(甲基氨基)硫代甲基】苯基】一1一(3一氯一2一吡啶基)一1H-,at:唑一5一甲酰胺(硫代苯甲酰胺(Liudaibeniiaxuanan'),由CN 103109816 A获知')(CAS1232543-85-9);N一【4一氯一2一II(1,1一二甲基乙基)氨基】羰基】一6一甲基苯基】一1一(3一氯-2-,'1t:啶基)一3一(氟甲氧基)一1H-qt;唑一5一甲酰胺(由WO 2012/034403A1获知)(CAS1268277-22-0)、N一【2一(5一氨基-1,3,4-噻二唑-2-基)一4一氯一6一甲基苯基】一3一溴一1一(3一氯一2一吡啶基')一1H一吡唑一5一甲酰胺(由WO 201I/085575A1获知')(CAS1233882-22-8)、4一【3一【2,6一二氯一4一【(3,3一二氯一2一丙烯一1一基)氧基】苯氧基】丙氧基】一2一甲氧基-6-(三氟甲基)一嘧啶(由CN 101337940 A获知)(CAS1108184-52-6):(2E)一和2(z)一2一【2一(4一氰基苯基)一1一【3一(三氟甲基)苯基】亚乙基卜N一【4一(二氟甲氧基)苯基卜肼甲酰胺(由CN 101715774 A获知)(CAS1232543-85-9):3一(2,2一二氯乙烯基)一2,2一二甲基-4-(1H一苯并咪唑-2-基)苯基一环丙烷甲酸酯(由CN 103524422 A获知)(CAS 1542271-46-4):(4aS)一7一氯一2,5一二氢一2一【【(甲氧基羰基)【4一【(三氟甲基)硫基】苯基】氨基】羰基卜茚并【1,2-eIll,3,4】憾二嗪-4a(3H)一羧酸甲酯(由CN102391261 A获知)(CAS1370358-69-2);6一脱氧-3-0一乙基-2,4-二.-O一甲基一1一【N一【4一【1一【4一(1,1,2,2,2-五氟乙氧基)苯基卜1H-1,2,4-三唑-3-基】苯基】氨基甲酸酯卜u-L-,It:喃甘露糖(由US 2014/0275503A1获知')(CAS 1181213—14-8'):8一(2一环丙基甲氧基-4-三氟甲基一苯氧基)一3一(6一三氟甲基一哒嗪一3一基)一3一氮杂双环【3.2.1】辛烷(CAS1253850-56-4)、(8一反式)一8一(2一环丙基甲氧基-4-三氟甲基一苯氧基)一3一(6一三氟甲基一哒嗪-3-基)一3一氮杂双环【3.2.1】辛烷(CAS 933798-27-7)、(8一顺式)一8一(2一环丙基甲氧基-4-三氟甲基一苯氧基)一3一(6一三氟甲基一哒嗪-3-基)一3一氮杂双环『3.2.11辛烷(由WO 2007/040280A1,WO 2007/040282A1获知')(CAS934001-66-8)、N一【3一氯-1-(3一吡啶基)一1H-毗;唑-4-基卜N一乙基一3一【(3,3,3-三氟丙基')硫基卜丙酰胺(由WO 2015/058021A1、WO 2015/058028A1获知')(CAS 1477919-27-9)和N一【4一(氨基硫代甲基)一2一甲基一6一【(甲基氨基)羰基】苯基】一3一溴-1-(3一氯一2一吡啶基)一1H-,It:唑一5一甲酰胺(由CN 103265527 A获知)(CAS 1452877-50-7)、5一(1,3一二憾烷-2-基)一4一114一(三氟甲基)苯基】甲氧基卜嘧啶(由WO 2013/115391A1获知)(CAS1449021-97-9)、3一(4一氯-2,6-二.甲基苯基)一8一甲氧基一1一甲基一1,8一二氮杂螺14.5】癸烷一2,4一二酮(由wo2014/187846A1知)(CAS 1638765-58-8)、3一(4一氯一2,6一二甲基苯基)一8一甲氧基一1一甲基一2一氧代一1,8一二氮杂螺14.5】癸一3一烯一4一基一碳酸乙酯(由o2010/066780A1、W02011151146A1获知)(CAS 1229023-00-0)、4一【(5S)-5-(3,5一二氯一4一氟苯基)一4,5一二氢一5一(三氟甲基)一3一异憾唑基】一N一【(4R)一2一乙基一3一氧代一4一异憾唑啉基】一2一甲基苯甲酰胺(由WO201I/067272、W02013/050302获知)(CAS 1309959-62-3)。
作物保护——处理类型
将植物和植物部位用本发明的胶囊悬浮液使用常规处理方法直接或通过作用于其周围环境、生长环境或储存空间进行处理,例如通过浸渍、喷雾、雾化、喷洒、蒸发、撒粉、弥雾、撤播、发泡、涂抹、铺展、注射、浇水(浸透)、滴灌,并且在繁殖材料的情况下,特别是在种子的情况下,额外通过干种子处理、液体种子处理、浆液处理,通过结壳,通过一种或多种涂层包衣等。还可以通过超低量法施用本发明的胶囊悬浮液或将根据本发明的施用形式或胶囊悬浮液本身注入土壤中。
一种优选的植物直接处理是叶面施用,即将本发明的胶囊悬浮液施用于叶面,在这种情况下,处理频率和施用率应根据有关害虫的侵染程度进行调整。
在活性成分具有系统性作用的情况下,本发明的胶囊悬浮液也通过根系进入植物中。然后通过本发明的胶囊悬浮液对植物生长环境的作用对植物进行处理。这可以通过例如浸透或通过混入土壤或营养液中来实现,即用本发明的胶囊悬浮液的液体形式浸溃植物所在地(例如土壤或水培系统),或通过土壤施用,即本发明的胶囊悬浮液以固体形式(例如以颗粒形式)引入植物所在地,或通过滴灌施用(通常也称为“化学灌溉"),即本发明的胶囊悬浮液与不同量的水在特定时期段内通过地袁或地下滴灌管一起引入植物附近的特定位置。在水稻作物的情况下,也可以通过将以固体施用形式(例如作为颗粒)的式(I)化合物计量到充满水的稻田中来实现。
根据本发明的土壤施用是本发明的胶囊悬浮液的优选施用形式。
在一个替代的实施方案中,本发明的胶囊悬浮液以叶面使用的形式施用。
本发明的胶囊悬浮浓缩物非常适合将存在的农业化学活性成分施用于植物和/或其生长环境。它们确保在相对较长的时间内以相应的所需量释放活性成分。本发明的胶囊悬浮浓缩物可以常规地按原样或预先用水稀释后使用。
通过常规方法进行施用,即,例如通过倾倒、喷雾或雾化。
本发明的胶囊悬浮浓缩物的施用率可以在相对宽的范围内变化。这由相关的农用化学活性成分及其在微胶囊制剂中的含量指导。
本发明的胶囊悬浮浓缩物可以通过已知方法生产,例如作为单独组分任选地与其他活性成分、添加剂和/或常规制剂助剂的混合制剂,然后用水稀释并以常规方式施用,或通过用水将单独配制或部分单独配制的各个组分联合稀释而制成桶混物。同样可以在不同时间施用(分开施用)单独配制的或部分单独配制的单独组分。也可以以多于一份的形式施用(顺序施用)单独组分或本发明的胶囊悬浮浓缩物。
本发明通过以下实施例进行说明。
塞逝
1-CS制剂的制备
有机相的制备:在搅拌下将活性成分溶解在有机溶剂中,任选地混合其他添加剂·然后以规定的比例加入多异氰酸酯·
水相的制备:将保护胶体溶解在水中,然后加入消泡剂。
将有机相加入到水相中并在转子/定子混合工具(ultraTurrax)的辅助下乳化直至达到所需的粒径。任选地,将胺组分额外添加到乳液中。将混合物加热至约70℃持续4小时以保证成壁聚脲反应完全。
然后将混合物冷却至室温并加入杀生物剂和增稠剂以调节所需的粘度。任选地,加入氨以确保所有异氰酸酯都已反应。
最终胶囊的粒径通过激光衍射(Malvern Mastersizer')测定。
2.温室内不同制剂类型的试验
方法说明:
活性试验在装有5.9kg pH值为7.1的砂壤土(含1.8%腐殖质)的长塑料容器中进行。形成一个5cm深的沟,并在其中间隔7cm放置四颗玉米种子(罗纳尔迪诺品种)。将试验制剂在4ml自来水中稀释并与700g砂壤土均匀混合。处理过的土壤被用来填充开沟并覆盖种子,这导致每个容器的总土壤重量为6.6kg。播种一天后,用移液管用450个带斑黄瓜叶甲(Diabrotica balteata')对每个容器进行侵染。将土壤含水量调整为具体田间容量的50%,并在第一个孵化的带斑黄瓜叶甲幼虫出现后增加至80%。生长条件为恒温25℃,相对湿度60-70%,钠蒸气灯照射14小时。试验设置每个处理包括三个重复试验。在侵染后21天,通过计算受损植物的数量和测量每个容器的鲜芽重量来评估试验。
因为从一个试验系列到下一个试验系列的绝对数可能会有很大差异,所以所有情况下的表格都只显示了同样在平行试验中进行的结果。在适当的情况下,显示了两个或更多个带有各自参考结果的表格。
不同制剂类型的比较:
# | 健康植物/% |
/ | 83-3 |
Nl | 25.0 |
N2 | 44.4 |
N3 | 0.05 |
N4 | 0.0 |
UTC未侵染 | 100 |
UTC已侵染 | 0.0 |
本发明的制剂#1表现出比所有比较实施例明显更佳的活性。
3.不同CS制剂的比较
(除非另有说明,适用以下试验条件:DLT施用条件始终为60 g/ha,观察期为侵染后21天)
a.AI浓度
# | 健康植物/% | 芽重/g |
2 | 100 | 89.7 |
J | 100 | 9l |
召 | 100 | 84.7 |
UTC未侵染 | 100 | 79.7 |
UTC已侵染 | 0 | 29-3 |
制剂中的AI浓度可以在相同的活性成分施用率下变化,同时具有同样良好的活性。
b.不同的活性成分
本发明的制剂与久一三氟氯氰菊酯、p一氟氯氰菊酯、氯氰菊酯的商业产品(胶囊悬浮液或颗粒剂)的比较
根据本发明的所有制剂在相同的AI施用率下表现出相较于具有相同活性成分的商业产品至少相当、大部分明显更好的有效性。
c.胶囊壳的组成
下文测试了具有不同胶囊厚度、异氰酸酯类型、交联和保护胶体的根据本发明的制剂。
# | 健康植物/% | 芽重/g |
S | 33-3 | 38.8 |
UTC未侵染 | 100 | 36.4 |
UTC已侵染 | 0 | 13.6 |
# | 健康植物/% | 芽重/g |
J | 66.7 | 41.2 |
9 | 16.7 | 42.2 |
/O | 1.0 | 28.0 |
ll | 1.0 | 14.86 |
12 | 0.0 | 31.6 |
13 | 25.0 | 39.2 |
UTC未侵染 | 100 | 34 |
UTC已侵染 | 0 | 21.6 |
# | 健康植物/% | 芽重/g |
9 | 83-3 | 72.8 |
J | 83-3 | 71.8 |
14 | 66.7 | 67.0 |
UTC未侵染 | 100 | 72.2 |
UTC已侵染 | 8 | 26.2 |
# | 健康植物/% | 芽重/g |
J | 100 | 26.4 |
15 | 100 | 37 |
/6 | 100 | 39-3 |
UTC未侵染 | 100 | 27.4 |
UTC已侵染 | 8 | 15.7 |
根据本发明的所有制剂都表现出活性。21天后的活性很大程度上取决于胶囊壳的性质。通过恰当选择壳体成分或通过混合不同的制剂,可以相应地调整所需的释放曲线。
d.佐剂的种类和用量
出人意料地发现佐剂需要存在于胶囊中以获得最佳活性,而桶混物添加剂没有表现出足够的活性。此外,具有末端羟基官能团的佐剂比具有甲氧基官能团的佐剂表现出更好的活性。
制剂干燥后在显tttt陇下对胶囊悬浮液进行光学评估:
保护胶体 | 0%Br<sub>e</sub>akThru Vibrant | 0.5%BTV | l%BTV | 2%BT V | 3%BT V |
<sup>K</sup>uraray <sup>P</sup>ova<sup>l</sup><sup>26</sup>-<sup>88</sup> | #<sup>27</sup>:. | #<sup>2S</sup>:. | #<sup>29</sup>:0 | #<sup>30</sup>:<sup>+</sup> | |
<sup>B</sup>orresperse <sup>NA</sup> | #<sup>J</sup>/:. | #/<sup>S</sup>. | #<sup>20</sup>:0 | #<sup>J</sup>:<sup>+</sup> |
评估方案:一=差,0=临界,+=好
e.土壤条件的影响
1.标准土,2.标准土+20%泥炭;
出人意料地发现该活性与土壤组成无关。
土壤含水量
施用场景:
A')将根据本发明的制剂引入最顶部土壤层(约40-50%的保水能力)=标准
B')将根据本发明的制剂引入最顶部土壤层(约40-50%的保水能力)并在潮湿条件下储存7天。
C')将根据本发明的制剂引入最顶部土壤层(约40-50%的保水能力)并将处理后的土壤干燥7天(<20%的吸水能力)。
D)将土壤干燥7天(<20%的吸水能力),将本发明的制剂施用到干燥的土壤中,然后在播种后重新浇水。
出人意料地发现该活性与土壤水分条件无关。
f.与商业产品的比较
# | 健康植物/% | 芽重/g |
9 | 83.3 | 72.8 |
DelCaps CS050 | 4.2 | 32.5 |
UTC未侵染 | 100 | 72.2 |
UTC已侵染 | 8 | 26.2 |
对于土壤施用,该商品显示出比根据本发明的制剂明显更差的活性。
g.不同批次的同一制剂的粒径的影响
# | 健康植物/% | 芽重/g |
J口 | 100 | 61.2 |
J凸 | 100 | 67.1 |
S<sub>口</sub> | 100 | 63.7 |
S凸 | 100 | 67.6 |
UTC未侵染 | 100 | 69.7 |
UTC已侵染 | 0 | 34.1 |
相对较小的粒径变化对活性没有影响。
4.户外试验
在户外试验中测试了根据本发明的制剂对比作为标准的Belem GR(活性成分:氯氰菊酯)对抗玉米中的线虫。胶囊制剂以60g a.i./ha的施用率进行喷雾(沟喷施用)(比较Belem MG 0.8以96g a.i./ha施用)到种子沟中。
报告的活性是4个单独结果的平均值。
# | 活性/% |
未处理 | 46.9 |
S | 73.8 |
J | 75.7 |
9 | 70.7 |
/O | 62.0 |
ll | 45.9 |
8+11 | 65.0 |
Bele<sub>m</sub>MG 0.8 | 6l-3 |
相较于标准,本发明的制剂表现出更好的活性。此外,可以通过混合具有不同释放的两种制剂(#8+#11)来调整释放速率。这将得到平均活性。
5.叶面施用
根据本发明的制剂在温室中对以下进行了预侵染试验:
卷心菜(Melissa)和灯笼椒(Feher)上的桃蚜(Myzus persicae)(MYZUPE);
棉花(Viky)上的棉蚜(Aphis gossypii)(APHIGO);
以及混合种群。
施用浓度为400l/ha,采用履带式喷雾器。在每种情况下进行三个重复试验。MYZUPE的试验在20℃下进行,APHIGO的试验在23℃下进行。在施用后1、4和7天(1、4、7天)后进行评估。
施用率:4001/ha,履带式喷雾器,接触式,每种情况下重复三次。
根据本发明的制剂表现出比SC025(N1)更好的活性。
焦且鱼塑壁
溴氰菊酯是来自Bayer AG,Leverkusen的活性物质。
p一氟氯氰菊酯是来自Bayer AG,Leverkusen的活性物质。
氯氰菊酯获自Agros Organics BVBA,Geel,Belgium。
Synergen w 06是来自Clariant Produkte(Deutschland)GmbH,Frankfurt的脂肪醇烷氧基化物。
Genapol EP 2584是来自Clariant Produkte(Deutschland)GmbH,Frankfurt的脂肪醇烷氧基化物。
Genapol X-060是来自Clariant Produkte(Deutschland)GmbH,Frankfurt的脂肪醇聚乙二醇醚。
Genapol XM 060是来自Clariant Produkte(Deutschland)GmbH,Frankfurt的基于Genapol X-060的具有末端甲基的脂肪醇聚乙二醇醚。
标准化学品:
黄原胶是水性体系的增稠剂(多家供应商)。
Solvesso 200ND是一种芳烃(多家供应商)。
二亚乙基三胺和氨是标准化学品,可以从多家供应商处获得。
选薹户鱼L
DelCaps 050CS是来自INNVIGO,Warsaw,Poland的含有胶囊化溴氰菊酯的产品。
Claims (16)
1.胶囊悬浮浓缩物,其包含:
A)颗粒分散相,其包含:
1)至少一种具有异氰酸酯反应基团的化合物a1.1)和异氰酸酯或异氰酸酯混合物a1.2)的反应产物,
2)在有机、水不溶性溶剂a2.2)中的拟除虫菊酯a2.1),
3)一种或多种添加剂a3.1)
以及
B)包含至少一种保护胶体b1.1)和任选地其他添加剂b1.2)的液体水相,
其中分散相A)的颗粒的平均粒径优选为1-50μm,以及其中
a1.2)的比例为按重量计0.1%至2%,
农业化学活性成分a2.1)的比例为按重量计1%至50%,
有机溶剂a2.2)的比例为按重量计1%至90%,
添加剂a3.1)的比例为按重量计0.5%至5%,
保护胶体b1.1)的比例为按重量计0.1%至5%,以及
添加剂b1.2)的比例为按重量计0.1%至15%。
2.根据权利要求1所述的胶囊悬浮浓缩物,其特征在于所述拟除虫菊酯选自溴氰菊酯、β-氟氯氰菊酯、氯氰菊酯和λ-三氟氯氰菊酯。
3.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于组分a3.1)包含至少一种选自以下的化合物:烷基乙氧基化物、烷基丙氧基乙氧基化物、脱水山梨糖醇和甘油的脂肪酸酯以及有机改性的三硅氧烷。
4.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于组分a1.1)是水。
5.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于所述分散相A)的颗粒的平均粒径为2至15μm。
6.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于a1.2)的比例为按重量计0.5%至2.0%,
农业化学活性成分a2.1)的比例为按重量计5%至15%,
有机溶剂a2.2)的比例为按重量计25%至40%,
添加剂a3.1)的比例为按重量计2%至5%,
保护胶体b1.1)的比例为按重量计0.2%至1%,以及
添加剂b1.2)的比例为按重量计0.3%至3%。
7.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于农业化学活性成分a2.1)与异氰酸酯或异氰酸酯混合物a1.2)的比例为2:1至10:1。
8.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于a1.2)与总有机相A)的比例优选为40:1至60:1,更优选45:1至60:1,特别优选45:1至55:1。
9.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于有机溶剂a2.2)选自二烷基萘以及1-甲基萘和2-甲基萘与萘的混合物。
10.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于基于整个制剂的分散相A)的比例为按重量计30%至70%。
11.根据前述权利要求中任一项所述的胶囊悬浮浓缩物,其特征在于基于整个制剂的农业化学活性成分a2.1)的比例为按重量计5%至15%。
12.制备根据权利要求1至11中任一项所述的胶囊悬浮浓缩物的方法,其特征在于包括以下工艺步骤:
1.制备有机相A)
2.制备水相B)
3.制备A)在B)中的乳液
4.任选地添加组分a1.1)(当a1.1.不是水时)
5.加热步骤
6.完成。
13.根据权利要求1至11中任一项所述的胶囊悬浮浓缩物用于叶面施用的用途。
14.根据权利要求1至11中任一项所述的胶囊悬浮浓缩物用于土壤施用的用途。
15.根据权利要求14所述的用途,其特征在于在相对长的时间段内进行释放。
16.根据权利要求1至11中任一项所述的胶囊悬浮浓缩物用于拟除虫菊酯,特别是溴氰菊酯的土壤施用。
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- 2020-02-24 EP EP20159164.1A patent/EP3868207A1/de not_active Withdrawn
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2021
- 2021-02-22 EP EP21706580.4A patent/EP4110060A1/de active Pending
- 2021-02-22 AU AU2021228885A patent/AU2021228885A1/en active Pending
- 2021-02-22 MX MX2022010335A patent/MX2022010335A/es unknown
- 2021-02-22 WO PCT/EP2021/054290 patent/WO2021170527A1/de active Application Filing
- 2021-02-22 CN CN202180016104.XA patent/CN115135153A/zh active Pending
- 2021-02-22 JP JP2022550174A patent/JP2023516575A/ja active Pending
- 2021-02-22 US US17/802,104 patent/US20230093563A1/en active Pending
- 2021-02-22 CA CA3172341A patent/CA3172341A1/en active Pending
- 2021-02-22 BR BR112022016725A patent/BR112022016725A2/pt unknown
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2022
- 2022-08-19 CO CONC2022/0011739A patent/CO2022011739A2/es unknown
- 2022-08-23 CL CL2022002301A patent/CL2022002301A1/es unknown
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WO2021170527A1 (de) | 2021-09-02 |
MX2022010335A (es) | 2022-09-19 |
CL2022002301A1 (es) | 2023-03-10 |
CO2022011739A2 (es) | 2022-08-30 |
EP3868207A1 (de) | 2021-08-25 |
BR112022016725A2 (pt) | 2022-10-11 |
CA3172341A1 (en) | 2021-09-02 |
AU2021228885A1 (en) | 2022-09-15 |
US20230093563A1 (en) | 2023-03-23 |
JP2023516575A (ja) | 2023-04-20 |
EP4110060A1 (de) | 2023-01-04 |
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