CN106458783A - 微胶囊化的硝化抑制剂组合物 - Google Patents
微胶囊化的硝化抑制剂组合物 Download PDFInfo
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- CN106458783A CN106458783A CN201580026973.5A CN201580026973A CN106458783A CN 106458783 A CN106458783 A CN 106458783A CN 201580026973 A CN201580026973 A CN 201580026973A CN 106458783 A CN106458783 A CN 106458783A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C1/00—Ammonium nitrate fertilisers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/10—Dispersions; Emulsions
- A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/10—Dispersions; Emulsions
- A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
- A61K9/1075—Microemulsions or submicron emulsions; Preconcentrates or solids thereof; Micelles, e.g. made of phospholipids or block copolymers
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
-
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- C05—FERTILISERS; MANUFACTURE THEREOF
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Abstract
本发明涉及改善的硝化抑制剂组合物及其在农业应用中的用途。用于本发明组合物的(三氯甲基)吡啶化合物包括具有取代有至少一个三氯甲基的吡啶环的化合物及其无机酸盐。适宜的化合物包括吡啶环上除了三氯甲基之外还包含氯或甲基取代基的那些,且包括甲基吡啶例如卢剔啶、可力丁和皮考啉的氯化产物在内。
Description
优先权要求
本申请要求2014年5月2日提交的美国临时专利申请61/988,056的权益,该临时申请的公开内容完全通过参考并入本申请。
技术领域
本发明涉及改善的硝化抑制剂组合物及其在农业应用中的用途。
背景技术和发明内容
(三氯甲基)吡啶化合物例如三氯甲基吡啶已经与肥料组合用作硝化抑制剂,如U.S.3,135,594中所描述,其通过参考并入本申请。这些化合物可使施用的铵态氮保持为铵形式(固化氮),这可增强作物性能。期望在播种时节可广泛施用这些化合物与氮肥料,但是由于可能存在的挥发性损失,这些施用方法通常不令人满意。另外,已经将三氯甲基吡啶添加到固定氮中,其默认是必须注入到土壤中的。
其它三氯甲基吡啶制剂已经施用于土壤的表面,但是必须在施用后8小时内用机械方法加入到或浇灌到土壤中以克服挥发性损失。终于,用木质素磺酸盐包封的三氯甲基吡啶的胶囊制剂的快速或倾泻释放也已经公开于U.S.4,746,513,其通过参考并入本申请。但是,尽管三氯甲基吡啶的释放可通过包封延缓,但是胶囊一旦与水分接触即可释放所有的三氯甲基吡啶,表现出与现有施用方法同样的稳定性和挥发性缺点。另外,这些制剂难以制备以及制备成本高,且不能与液体尿素硝铵(“UAN”)肥料一起使用。
如公开于U.S.5,925,464的缩聚包封已经用于包封农业活性成分,特别是通过使用聚氨酯而非聚脲密封剂来增强活性成分的处理安全性和储存稳定性。
但是,仍需要递送硝化抑制剂例如(三氯甲基)吡啶,其与未包封的硝化抑制剂制剂相比在田地环境中表现出较大的长期稳定性,同时保持效力水平。
第一组实施方式包括微胶囊悬浮剂制剂,其包含:(a)悬浮相,所述悬浮相包括多个微胶囊,所述微胶囊的体积中值粒度为约1至约10微米,其中所述微胶囊包括:(1)微胶囊壁,其通过聚合异氰酸酯和多胺之间进行界面缩聚反应以形成聚脲壳来制备,其重量百分比为所述微胶囊悬浮剂制剂总重量的约0.2至约40%,和(2)基本上液体的芯,所述基本上液体的芯包封在所述聚脲壳内,其中所述基本上液体的芯包括至多约60wt%的硝化抑制剂,在这些实施方式的一些中,所述硝化抑制剂是2-氯-6-(三氯甲基)吡啶,并且在这些实施方式中所述基本上液体的芯包括至多1.0wt%的固体2-氯-6-(三氯甲基)吡啶,在大于或等于15℃的温度测定;和(b)水相,其中所述水相包括至少约1.0wt%的芳族溶剂,在一些优选的实施方式中,在形成所述微胶囊之后将芳族溶剂添加到水相中。
第二组实施方式包括根据第一组实施方式的微胶囊悬浮剂制剂,并且进一步包括:存在于所述水相中的至少一种离子稳定剂。
第三组实施方式包括根据第一或第二组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂是至少一种选自以下的化合物:轻芳烃,脱萘轻芳烃,重芳烃,和脱萘重芳烃。
第四组实施方式包括根据第三组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂是脱萘C10-13重芳烃。
第五组实施方式包括根据第四组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约1重量%至约10重量%的脱萘C10-13重芳烃。
第六组实施方式包括根据第四组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2重量%至约5重量%的脱萘C10-13重芳烃。
第七组实施方式包括根据第四组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2.5重量%至约3.0重量%的脱萘C10-13重芳烃。
第八组实施方式包括根据第三组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂是C10-13重芳烃。
第九组实施方式包括根据第八组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约1重量%至约10重量%的C10-13重芳烃。
第十组实施方式包括根据第八组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2重量%至约5重量%的C10-13重芳烃。
第十一组实施方式包括根据第八组实施方式的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2.5重量%至约3.0重量%的C10-13重芳烃。
第十二组实施方式包括根据第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、或第十一组实施方式的微胶囊悬浮剂制剂,其中所述微胶囊的体积中值粒度为约1至约5微米。
第十三组实施方式包括根据第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、或第十二组实施方式的微胶囊悬浮剂制剂,其中所述悬浮相a)与所述水相b)的比率为约1:0.75至约1:100。
第十四组实施方式包括根据第十三组实施方式的微胶囊悬浮剂制剂,其中所述悬浮相a)与所述水相b)的比率为约1:1至约1:7。
第十五组实施方式包括根据第十三组实施方式的微胶囊悬浮剂制剂,其中所述悬浮相a)与所述水相b)的比率为约1:1至约1:4。
第十六组实施方式包括根据第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四、或第十五组实施方式的微胶囊悬浮剂制剂,其中所述聚合异氰酸酯是聚亚甲基聚苯基异氰酸酯。
第十七组实施方式包括根据第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四、第十五、或第十六组实施方式的微胶囊悬浮剂制剂,其进一步包括氮肥料。
第十八组实施方式根据第十七组实施方式,其中所述氮肥料是尿素硝铵。
第十九组实施方式包括抑制生长介质中铵态氮硝化的方法,其包括以下步骤:将第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四、第十五、第十六、第十七、第十八、和第十九组实施方式的微胶囊悬浮剂制剂施用于植物生长介质。
第二十组实施方式根据第十九组实施方式,其中将所述制剂加入到所述生长介质中。
第二十一组实施方式根据第二十组实施方式,其中将所述制剂施用于生长介质表面。
第二十二组实施方式包括抑制硝化的方法,其中将第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四、第十五、或第十六组实施方式的制剂与农药组合施用或与农药先后施用。
第二十三组实施方式包括根据第二十二组实施方式的方法,其中将所述制剂与氮肥料一起施用。
第二十四组实施方式根据第二十三组实施方式,其中所述氮肥料是尿素硝铵。微胶囊悬浮剂制剂,其包含:悬浮相,所述悬浮相包括多个微胶囊,所述微胶囊的体积中值粒度为约1至约10微米,其中所述微胶囊包括:(1)微胶囊壁,其通过聚合异氰酸酯和多胺之间进行界面缩聚反应以形成聚脲壳来制备,其重量百分比为所述微胶囊悬浮剂制剂总重量的约0.2至约40%,和(2)基本上液体的芯,所述基本上液体的芯包封在所述聚脲壳内,其中所述基本上液体的芯包括占整个微胶囊至多约40wt%的2-氯-6-(三氯甲基)吡啶,和(b)水相,其中所述水相包括至少约1.0wt%的芳族溶剂,其中在形成所述微胶囊之后将所述至少约1.0wt%的芳族溶剂添加到水相中。
本申请进一步公开了微胶囊悬浮剂制剂,其包含:多个体积中值粒度为约1至约10微米的微胶囊的悬浮相,其中所述微胶囊包括:通过聚合异氰酸酯和多胺之间进行界面缩聚反应以形成聚脲壳来制备的微胶囊壁,其重量百分比为所述微胶囊悬浮剂制剂总重量的约0.2至约15%,和包封在聚脲壳内的化合物,其中所述化合物是2-氯-6-(三氯甲基)吡啶;和包括离子稳定剂和分散的芳族溶剂的水相。
在一些实施方式中,分散的芳族溶剂是至少一种选自以下的化合物:轻芳烃,脱萘轻芳烃,重芳烃,和脱萘重芳烃。在其它实施方式中,分散的芳族溶剂是脱萘C10-13重芳烃。再在其它实施方式中,制剂包含约1重量%至约10重量%的脱萘C10-13重芳烃。再在其它实施方式中,制剂包含约2重量%至约5重量%的脱萘C10-13重芳烃。
在一些实施方式中,制剂包含约2.5重量%至约3.0重量%的脱萘C10-13重芳烃。再在其它实施方式中,分散的芳族溶剂是C10-13重芳烃。再在其它实施方式中,制剂包含约1重量%至约10重量%的C10-13重芳烃。
而且,在示例性的实施方式中,制剂包含约2重量%至约5重量%的C10-13重芳烃。或者,制剂包含约2.5重量%至约3.0重量%的C10-13重芳烃。
在进一步的实施方式中,微胶囊的体积中值粒度为约1至约5微米。在其它实施方式中,悬浮相a)与水相b)的比率为约1:0.75至约1:100。再在其它实施方式中,悬浮相a)与水相b)的比率为约1:1至约1:7。在进一步的实施方式中,悬浮相a)与水相b)的比率为约1:1至约1:4。
本申请也公开了微胶囊悬浮剂,其中聚合异氰酸酯是聚亚甲基聚苯基异氰酸酯。在一些实施方式中,多胺选自乙二胺和二亚乙基三胺。
再进一步公开了肥料组合物,其包含:氮肥料和上述的微胶囊悬浮剂制剂。在其它实施方式中,氮肥料是尿素硝铵。
本申请也公开了抑制生长介质中铵态氮硝化的方法,其包括将上述微胶囊悬浮剂制剂施用于所述生长介质。在进一步的实施方式中,将制剂加入到所述生长介质中。再在进一步的实施方式中,将制剂施用于生长介质表面。在其它实施方式中,将制剂与农药组合施用或与农药先后施用。
再在进一步的实施方式中,将制剂与氮肥料一起施用。氮肥料可以是尿素硝铵。
本发明的微胶囊悬浮剂制剂是稳定的并且允许在作物中延缓加入氮,由此提供农艺和环境益处。已经出乎意料地发现,微胶囊化的(三氯甲基)吡啶化合物例如三氯甲基吡啶的组合物与未包封的三氯甲基吡啶的组合物相比具有较好的性能,甚至当加入到土壤中时也是如此。
具体实施方式
用于本发明组合物的(三氯甲基)吡啶化合物包括具有取代有至少一个三氯甲基的吡啶环的化合物及其无机酸盐。适宜的化合物包括吡啶环上除了三氯甲基之外还包含氯或甲基取代基的那些,且包括甲基吡啶例如卢剔啶、可力丁和皮考啉的氯化产物在内。适宜的盐包括盐酸盐、硝酸盐、硫酸盐和磷酸盐。用于本发明实践的(三氯甲基)吡啶化合物通常是溶解于溶剂中的油性液体或结晶固体。其它适宜的化合物描述于U.S.3,135,594。优选的(三氯甲基)吡啶是2-氯-6-(三氯甲基)吡啶,也称为三氯甲基吡啶,并且是产品N-SERVETM(Dow AgroSciences LLC的商标)的活性成分。
化合物例如三氯甲基吡啶的效用已经通过将这样的化合物与适宜的溶剂一起包封在微胶囊中而被极大地增强。特别有用的微胶囊包括由聚脲壳包围的三氯甲基吡啶/疏水溶剂基本上液体的芯。选择具有适当体积和壳厚度的微胶囊,组合物可悬浮在、储存在水相中以及在水相中施用。这种有用的制剂公开于2009年2月26日提交的美国专利申请序列号12/393,661,2009年9月10日公布的公开号U.S.2009-0227458 Al;2008年1月18日提交的美国专利申请序列号12/009,432,2008年7月24日公布的公开号U.S.2008-0176745 Al,现在颁发为美国专利号8,377,849,其在2013年2月19日颁发;和2007年1月22日提交的美国临时申请序列号60/881,680,它们完全通过参考明确并入本申请,等同于它们各自单独通过参考并入本申请。
尽管上述微胶囊含水悬浮剂比在水溶液中的未包封的三氯甲基吡啶在某些条件下更稳定,但是已经发现三氯甲基吡啶的晶体可在储存过程中在三氯甲基吡啶的微胶囊悬浮剂的水相中形成。结晶三氯甲基吡啶在三氯甲基吡啶的含水微胶囊悬浮剂中的形成在长期的储存过程中似乎利于在约-50℃至约150℃、更特别为约00℃至100℃(摄氏度)的极窄的温度范围内进行。结晶三氯甲基吡啶在微胶囊悬浮剂的本体水相中的重量百分比随时间累积。根据如何处理微胶囊悬浮剂,在水相中存在可测量含量的结晶三氯甲基吡啶可能产生极小或不产生任何后果或问题。如果通过用包含内置筛的喷雾器将悬浮剂喷雾通过针尖喷嘴,则在微胶囊悬浮剂的水相中存在甚至约0.1wt%或以上的结晶三氯甲基吡啶可能是特别成问题的。
为了抑制或至少可预见地减慢在水相中形成三氯甲基吡啶晶体,本申请公开了一种微胶囊悬浮剂制剂组合物,其包括至少1wt%存在于微胶囊悬浮剂的水相中的芳族溶剂。在一些实施方式中,在结晶三氯甲基吡啶在水相中累积到成问题含量之前,将溶剂添加到微胶囊悬浮剂的水相中。在一些实施方式中,在结晶三氯甲基吡啶在悬浮剂的水相中累积到成问题含量之后,将溶剂添加到悬浮剂的水相中。
可用于将结晶(三氯甲基)吡啶化合物溶解于微胶囊的有机相的典型溶剂的实例包括芳族溶剂,特别是烷基取代的苯如二甲苯或丙基苯馏分,以及混合的萘和烷基萘馏分;矿物油;煤油;脂肪酸的二烷基酰胺,特别是脂肪酸的二甲基酰胺如辛酸的二甲基酰胺;氯化的脂族和芳族烃如1,1,1-三氯乙烷和氯苯;二醇衍生物的酯,例如二甘醇的正丁醚、乙醚、或甲醚的乙酸酯,以及一缩二丙二醇的甲醚的乙酸酯;酮,例如异佛尔酮和三甲基环己酮(二氢异佛尔酮);和乙酸酯产物例如乙酸己酯或乙酸庚酯。优选的有机液体是二甲苯,烷基取代的苯如丙基苯馏分,和烷基萘馏分。
通常,如果需要,所用的溶剂量通常为约40wt%(优选为约50wt%)至约70wt%(优选为至约60wt%),基于(三氯甲基)吡啶/溶剂溶液的总重量。(三氯甲基)吡啶在(三氯甲基)吡啶/溶剂溶液中的量通常为约30wt%(优选为约40wt%)至约60wt%(优选为至约50wt%),基于(三氯甲基)吡啶/溶剂溶液的重量。
用于本发明的微胶囊可以通过聚合异氰酸酯和多胺之间进行缩聚反应以形成聚脲壳来制备。微胶囊化的方法是本领域公知的,任何这样的方法可以用于本发明以得到胶囊悬浮剂制剂。通常,胶囊悬浮剂制剂可以通过首先混合聚合异氰酸酯与(三氯甲基)吡啶/溶剂溶液来制备。然后将该混合物与包括乳化剂的水相合并以形成两相体系。通过剪切直到达到所需粒度将有机相乳化到水相中。然后在搅拌下逐滴添加交联多胺水溶液,从而在含水悬浮剂中形成(三氯甲基)吡啶的包封颗粒。
所需的粒度和腔室壁厚度(cell wall thickness)将取决于实际应用。微胶囊的体积中值粒度通常为约1至约10微米,胶囊壁厚度通常为约10至约125纳米。在其中立即将本发明制剂加入到生长介质的一种实施方式中,所需粒度可以为约2至约10微米,腔室壁为约10至约25纳米。在需要土壤表面稳定性的另一种实施方式中,所需粒度可以为约1-5微米,腔室壁厚度为约75至约125纳米。
其它常规添加剂也可以加入到制剂中,例如乳化剂,分散剂,增稠剂,生物灭杀剂,农药,盐和成膜聚合物。
分散剂和乳化剂包括环氧烷烃与酚类和有机酸的缩合产物,烷基芳基磺酸盐,山梨聚糖酯的聚环氧烷烃衍生物,混杂醚醇,石油磺酸皂,木质素磺酸盐,聚乙烯醇等。表面活性剂的用量通常为约1至约20重量%,基于微胶囊悬浮剂制剂。
在本发明微胶囊悬浮剂制剂中悬浮相与水相的比率取决于(三氯甲基)吡啶化合物在最终制剂中的所需浓度。通常该比率将为约1:0.75至约1:100。通常,所需比率为约1:1至约1:7,优选为约1:1至约1:4。
(三氯甲基)吡啶化合物的存在可抑制铵态氮在土壤或生长介质中的硝化作用,由此防止源自氮肥料、有机氮组分、或有机肥料等的铵态氮快速损失。
通常,施用本发明的微胶囊悬浮剂制剂,使得(三氯甲基)吡啶化合物以约0.5至约1.5kg/公顷的施用率、优选以约0.58至约1.2kg/公顷的施用率施用于土壤或生长介质。优选量可容易通过施用偏好、考虑因素例如土壤pH、温度、土壤类型和施用模式确定。
本发明的微胶囊悬浮剂制剂可以按有益于有用作物的任何方式施用。在一种实施方式中,将微胶囊悬浮剂制剂以带施或条施的方式施用于生长介质。在另一种实施方式中,在播种或移植所需作物植物之前,将制剂施用于或施用遍及生长介质。再在另一种实施方式中,可以将制剂施用于生长植物的根部区域。
另外,可以在施用氮肥料时施用微胶囊悬浮剂制剂。可以在施用肥料之前、之后、或同时施用制剂。
本发明的微胶囊悬浮剂制剂具有的附加益处是,可以在不向土壤中混入另外的水或机械操作达数天至数周的情况下将其施用于土壤表面。或者,如果需要,可以在施用后立即将本发明的制剂加入到土壤。
本发明的微胶囊悬浮剂制剂具有的(三氯甲基)吡啶化合物浓度为约1wt%(优选为约10wt%、更优选为约15wt%)至约50wt%(通常至约35wt%、优选至约30wt%、更优选至约25wt%),基于微胶囊悬浮剂制剂的总重量,优选的范围为约5至约40wt%的三氯甲基吡啶。然后将微胶囊悬浮剂制剂与溶剂或水混合,以获得所需的施用率。
土壤处理组合物可以如下制备:将微胶囊悬浮剂制剂分散在肥料例如铵或有机氮肥料。所得肥料组合物可以原样使用或可以改性,如通过用另外的氮肥料或惰性固体载体稀释以获得包含用于处理土壤的所需量活性剂的组合物。
土壤可以按任何便利的方式用本发明微胶囊悬浮剂制剂制备,包括:与土壤机械混合;施用于土壤表面,然后拖成或切成所需厚度的土壤;或例如通过注射、喷雾、洒粉或灌溉运输至土壤。在灌溉施用中,可以将适当量的制剂引入到灌溉水中,以便将(三氯甲基)吡啶化合物分配到至多6英寸(15.24cm)的所需深度。
出乎意料地,一旦加入到土壤,本发明的微胶囊悬浮剂制剂即可超过其他三氯甲基吡啶制剂,特别是未包封的类型。原以为包封的组合物不会像未包封类型一样有效地释放足够的三氯甲基吡啶,其中从胶囊扩散将会太慢以至于无法提供生物效果,但实际上观察到了相反的效果。
由于三氯甲基吡啶在本发明微胶囊悬浮剂制剂中的缓释,可以获得几种优点。首先,可以减少三氯甲基吡啶的量,因为其可以在延长的时间段内更有效地释放进土壤。另外,本发明的微胶囊悬浮剂制剂可以施用于并留在天然纳入土壤的表面上,而无需在期望的情况下进行机械混入。
在微胶囊悬浮剂制剂的一些实施方式中,后添加(即,在微胶囊形成之后)芳族溶剂到水相中可降低在某些温度储存条件晶体在水相中的形成和/或生长。在一种实施方式中,后添加芳族溶剂可提供在冷温度储存条件中较好的晶体生长减少。在示例性的实施方式中,这样的后添加芳族溶剂包括一种或多种油,并且在形成微胶囊之后存在于制剂的水相中。术语“油”在本申请描述通常不与水溶混的溶剂。
在一些实施方式中,已经包含三氯甲基吡啶的晶体但在水相中没有芳族溶剂的微胶囊悬浮剂制剂可以通过添加至水相而用一种或多种芳族溶剂处理,可以将所得混合物在环境温度搅拌一定时间段,可以为30分钟至5小时,基于微胶囊悬浮剂的总体积,直到三氯甲基吡啶的晶体已经消失。
在未将一种或多种芳族溶剂添加到水相的情况下,本申请的微胶囊悬浮剂制剂可以在温和的冷储存温度(约100℃)在水相中形成三氯甲基吡啶晶体。三氯甲基吡啶晶体的纯度可以为约99%。经过一段时间,这样的晶体可能占总微胶囊悬浮剂制剂的至多0.5wt%。但是,晶体也可以在其它温度形成,例如00℃,-50℃,和150℃。基于溶剂的晶体生长抑制剂例如芳族溶剂可以提供较好的物理稳定性,特别是在温和的冷储存温度在约100℃,以防止在微胶囊悬浮剂的水相中形成晶体。
说明性地,可以在形成微胶囊悬浮剂之后添加的芳族溶剂包括:Aromatic100Fluid,也称为溶剂石脑油或轻芳烃;Aromatic 150Fluid,也称为溶剂石脑油,重芳烃,高闪点芳族石脑油类型II,重芳烃溶剂石脑油,烃,C10芳烃,>1%萘,A150,S150(Solvesso150);和Aromatic 200Fluid,也称为溶剂石脑油,重芳烃,高闪点芳族石脑油类型II,重芳烃溶剂石脑油,烃,C10-13芳烃,>1%萘,A200,和S200(Solvesso 200)。
在一些实施方式中,可以在形成微胶囊悬浮剂之后添加到制剂的芳族溶剂包括:脱萘的那些,或包含少于约1%萘的那些。所述溶剂可以在晶体形成之前作为预防措施添加到微胶囊悬浮剂制剂中,或在晶体形成之后作为补救措施添加到微胶囊悬浮剂制剂中,从而除去或减少晶体的存在。
另外,本发明的微胶囊悬浮剂制剂可以与农药或农药混合物及其协同混合物组合或联用,所述农药包括杀啮齿动物剂,杀菌剂,杀真菌剂,除草剂,杀昆虫剂,杀螨剂,杀线虫剂,硝化抑制剂例如双氰胺,尿素酶抑制剂例如N-(正丁基)硫代磷酰三胺等。在这样的应用中,本发明的微胶囊悬浮剂制剂可以与所需农药罐混合,或者可以将它们先后施用。
示例性的除草剂包括但不限于刈草胺(acetochlor),甲草胺(alachlor),氯氨基吡啶酸(aminopyralid),莠去津(atrazine),解草嗪(benoxacor),溴苯腈(bromoxynil),氟酮唑草(carfentrazone),绿磺隆(chlorsulfuron),炔草酯(clodinafop),二氯吡啶酸(clopyralid),麦草畏(dicamba),氯甲草-甲基(diclofop-methyl),二甲吩草胺(dimethenamid),噁唑禾草灵(fenoxaprop),氟酮磺隆(flucarbazone),氟噻草胺(flufenacet),氟唑啶草(flumetsulam),氟烯草酸(flumiclorac),氯氟吡氧乙酸(fluroxypyr),草铵膦(glufosinate-ammonium),草甘膦(glyphosate),氯吡嘧磺隆(halosulfuron-methyl),咪草酯(imazamethabenz),咪草啶酸(imazamox),灭草烟(imazapyr),灭草喹(imazaquin),咪草烟(imazethapyr),异噁氟草酮(isoxaflutole),二氯喹啉酸(quinclorac),MCPA,MCP胺,MCP酯,精甲霜灵(mefenoxam),甲基磺草酮(mesotrione),异丙甲草胺(metolachlor),S-异丙甲草胺(S-metolachlor),嗪草酮(metribuzin),甲磺隆(metsulfuron-methyl),烟嘧磺隆(nicosulfuron),百草枯(paraquat),胺硝草(pendimethalin),氨氯吡啶酸(picloram),氟嘧磺隆(primisulfuron),丙苯磺隆(propoxycarbazone),氟磺隆(prosulfuron),吡草醚-乙基(pyraflufen-ethyl),砜嘧磺隆(rimsulfuron),西玛津(simazine),磺酰磺隆(sulfosulfuron),噻吩磺隆脱甲基酸(thifensulfuron),topramezone,苯草酮(tralkoxydim),野麦畏(triallate),醚苯磺隆(triasulfuron),苯磺隆(tribenuron),三氯吡氧乙酸(triclopyr),氟乐灵(trifluralin),2,4-D,2,4-D胺,2,4-D酯等。
示例性的杀昆虫剂包括但不限于1,2-二氯丙烷(1,2-dichloropropane),1,3-二氯丙烯(1,3-dichloropropene),阿维菌素(abamectin),高灭磷(acephate),灭螨醌(acequinocyl),吡虫清(acetamiprid),家蝇磷(acethion),乙酰虫腈(acetoprole),氟酯菊酯(acrinathrin),丙烯腈(acrylonitrile),棉铃威(alanycarb),涕灭威(aldicarb),砜灭威(aldoxycarb),艾氏剂(aldrin),丙烯除虫菊(allethrin),阿洛氨菌素(allosamidin),除害威(allyxycarb),α-氯氰菊酯(alpha-cypermethrin),α-蜕皮素(alpha-ecdysone),赛果(amidithion),amidoflumet,灭害威(aminocarb),胺吸磷(amiton),虫螨脒(amitraz),新烟碱(anabasine),三氧化二砷(arsenous oxide),艾噻达松(athidathion),艾扎丁(azadirachtin),唑啶磷(azamethiphos),益棉磷(azinphos-ethyl),保棉磷(azinphos-methyl),偶氮苯(azobenzene),三唑锡(azocyclotin),偶氮磷(azothoate),六氟硅酸钡(barium hexafluorosilicate),熏虫菊(barthrin),benclothiaz,唑虫威(bendiocarb),丙硫克拜威(benfuracarb),苯噁磷(benoxafos),杀虫磺(bensultap),苯螨特(benzoximate),苯甲酸苄酯(benzyl benzoate),β-氟氯氰菊酯(beta-cyfluthrin),β-氯氰菊酯(beta-cypermethrin),联苯肼酯(bifenazate),联苯菊酯(bifenthrin),乐杀螨(binapacryl),反式丙烯除虫菊(bioallethrin),bioethanomethrin,生物氯菊酯(biopermethrin),双二氟虫脲(bistrifluron),硼砂(borax),硼酸(boric acid),溴苯烯磷(bromfenvinfos),溴-DDT(bromo DDT),溴烯杀(bromocyclen),溴硫磷(bromophos),乙基溴硫磷(bromophos-ethyl),溴螨酯(bromopropylate),合杀威(bufencarb),噻嗪酮(buprofezin),畜虫威(butacarb),特嘧硫磷(butathiofos),丁叉威(butocarboxim),丁酯磷(butonate),氧丁叉威(butoxycarboxim),硫线磷(cadusafos),砷酸钙(calcium arsenate),石硫合剂(calciumpolysulfide),毒杀芬(camphechlor),氯灭杀威(carbanolate),甲萘威(carbaryl),虫螨威(carbofuran),二硫化碳(carbon disulfide),四氯化碳(carbon tetrachloride),三硫磷(carbophenothion),丁硫克百威(carbosulfan),巴丹(cartap),灭螨猛(chinomethionat),氯虫酰胺(chlorantraniliprole),氯杀螨(chlorbenside),冰片丹(chlorbicyclen),氯丹(chlordane),开蓬(chlordecone),氯苯脒(chlordimeform),壤土氯磷(chlorethoxyfos),氟唑虫清(chlorfenapyr),杀螨醇(chlorfenethol),杀螨酯(chlorfenson),敌螨丹(chlorfensulphide),毒虫畏(chlorfenvinphos),定虫隆(chlorfluazuron),氯甲磷(chlormephos),乙酯杀螨醇(chlorobenzilate),氯仿(chloroform),伊托明(chloromebuform),螟铃畏(chloromethiuron),氯化苦(chloropicrin),丙酯杀螨醇(chloropropylate),氯腈肟磷(chlorphoxim),氯吡唑磷(chlorprazophos),毒死蜱(chlorpyrifos),甲基毒死蜱(chlorpyrifos-methyl),氯甲硫磷(chlorthiophos),环虫酰胺(chromafenozide),瓜菊酯I(cinerin I),瓜菊酯I(cinerinII),左旋反灭虫菊酯(cismethrin),除线威(cloethocarb),四螨嗪(clofentezine),氯氰碘柳胺(closantel),噻虫胺(clothianidin),乙酰亚砷酸铜(copper acetoarsenite),砷酸铜(copper arsenate),环烷酸铜(copper naphthenate),油酸铜(copper oleate),库马磷(coumaphos),畜虫磷(coumithoate),克罗米通(crotamiton),丁烯磷(crotoxyphos),cruentaren A和B,育畜磷(crufomate),氟铝酸钠(cryolite),苯腈磷(cyanofenphos),杀螟磷(cyanophos),果虫磷(cyanthoate),环戊烯菊酯(cyclethrin),乙氰菊酯(cycloprothrin),cyenopyrafen,丁氟螨酯(cyflumetofen),氟氯氰菊酯(cyfluthrin),三氟氯氰菊酯(cyhalothrin),三环锡(cyhexatin),氯氰菊酯(cypermethrin),苯醚氰菊酯(cyphenothrin),灭蝇胺(cyromazine),赛灭磷(cythioate),右旋柠檬烯(d-limonene),棉隆(dazomet),DBCP,DCIP,DDT,一甲呋喃丹(decarbofuran),溴氰菊酯(deltamethrin),田乐磷(demephion),田乐磷-O(demephion-O),田乐磷-S(demephion-S),内吸磷(demeton),甲基内吸磷(demeton-methyl),内吸磷-O(demeton-O),内吸磷-O-甲基(demeton-O-methyl),内吸磷-S(demeton-S),内吸磷-S-甲基(demeton-S-methyl),内吸磷-S-甲基硫(demeton-S-methylsulphon),杀螨硫隆(diafenthiuron),氯亚磷(dialifos),除线特(diamidafos),二嗪农(diazinon),异氯硫磷(dicapthon),除线磷(dichlofenthion),敌敌畏(dichlorvos),苯氟磺胺(dichlofluanid),敌敌畏(dichlorvos),开乐散(dicofol),N-(3-甲基苯基)氨基甲酸甲酯(dicresyl),百治磷(dicrotophos),环虫腈(dicyclanil),狄氏剂(dieldrin),除螨灵(dienochlor),氟螨嗪(diflovidazin),氟脲杀(diflubenzuron),丙羟茶碱(dilor),四氟甲醚菊酯(dimefluthrin),甲氟磷(dimefox),地麦威(dimetan),乐果(dimethoate),苄菊酯(dimethrin),甲基毒虫畏(dimethylvinphos),敌蝇威(dimetilan),消螨酚(dinex),消螨通(dinobuton),敌螨普(dinocap),敌螨普-4(dinocap-4),敌螨普-6(dinocap-6),敌螨通(dinocton),硝戊酯(dinopenton),丙硝酚(dinoprop),戊硝酚(dinosam),硝辛酯(dinosulfon),呋虫胺(dinotefuran),硝丁酯(dinoterbon),噁茂醚(diofenolan),杀抗松(dioxabenzofos),二氧威(dioxacarb),敌噁磷(dioxathion),二苯砜(diphenyl sulfone),双硫仑(disulfiram),乙拌磷(disulfoton),噻喃磷(dithicrofos),DNOC,苯氧炔螨(dofenapyn),多拉克汀(doramectin),促蜕皮甾酮(ecdysterone),甲氨基阿维菌素(emamectin),EMPC,烯炔菊酯(empenthrin),硫丹(endosulfan),因毒磷(endothion),异狄氏剂(endrin),苯硫磷(EPN),保幼醚(epofenonane),爱普瑞菌素(eprinomectin),高氰戊菊酯(esfenvalerate),etaphos,苯虫威(ethiofencarb),乙硫磷(ethion),乙虫腈(ethiprole),益果(ethoate-methyl),灭克磷(ethoprophos),乙基-DDD(ethyl DDD),甲酸乙酯(ethyl formate),1,2-二溴乙烷(ethylene dibromide),1,2-二氯乙烷(ethylene dichloride),环氧乙烷(ethyleneoxide),醚菊酯(etofenprox),特苯噁唑(etoxazole),乙嘧硫磷(etrimfos),EXD,氨磺磷(famphur),克线磷(fenamiphos),抗螨唑(fenazaflor),喹螨醚(fenazaquin),杀螨锡(fenbutatin oxide),皮蝇磷(fenchlorphos),乙苯威(fenethacarb),五氟苯菊酯(fenfluthrin),杀螟硫磷(fenitrothion),丁苯威(fenobucarb),苯硫威(fenothiocarb),fenoxacrim,双氧威(fenoxycarb),吡氯氰菊酯(fenpirithrin),甲氰菊酯(fenpropathrin),唑螨酯(fenpyroximate)、除螨酯(fenson),丰索磷(fensulfothion),倍硫磷(fenthion),倍硫磷-乙基(fenthion-ethyl),氟硝二苯胺(fentrifanil),氰戊菊酯(fenvalerate),锐劲特(fipronil),氟啶虫酰胺(flonicamid),嘧螨酯(fluacrypyrim),氟佐隆(fluazuron),氟虫酰胺(flubendiamide),噻唑螨(flubenzimine),氟氯双苯隆(flucofuron),氟螨脲(flucycloxuron),氟氰菊酯(flucythrinate),联氟螨(fluenetil),嘧虫胺(flufenerim),氟虫脲(flufenoxuron),氟丙苄醚(flufenprox),氟氯苯菊酯(flumethrin),氟杀螨(fluorbenside),氟胺氰菊酯(fluvalinate),地虫磷(fonofos),伐虫脒(formetanate),安果(formothion),胺甲威(formparanate),丁苯硫磷(fosmethilan),甲基毒死蜱(fospirate),伐线丹(fosthietan),伐线丹(fosthietan),呋线威(furathiocarb),糠醛菊酯(furethrin),糠醛(furfural),γ-三氟氯氰菊酯(gamma-cyhalothrin),γ-HCH(gamma HCH),卤醚菊酯(halfenprox),特丁苯酰肼(halofenozide),HCH,HEOD,七氯(heptachlor),庚虫磷(heptenophos),速杀硫磷(heterophos),氟铃脲(hexaflumuron),噻螨酮(hexythiazox),艾氏剂(HHDN),灭蚁腙(hydramethylnon),氰化氢(hydrogen cyanide),蒙五一二(hydroprene),喹啉威(hyquincarb),新烟碱类(imicyafos),吡虫啉(imidacloprid),咪炔菊酯(imiprothrin),茚虫威(indoxacarb),碘甲烷(iodomethane),IPSP,isamidofos,氯唑磷(isazofos),碳氯灵(isobenzan),水胺硫磷(isocarbophos),异艾氏剂(isodrin),丙胺磷(isofenphos),异丙威(isoprocarb),稻瘟灵(isoprothiolane),叶蚜磷(isothioate),噁唑磷(isoxathion),齐墩螨素(ivermectin),茉莉菊酯I(jasmolin I),茉莉菊酯II(jasmolin II),碘硫磷(jodfenphos),保幼激素I(juvenile hormone I),保幼激素II(juvenile hormone II),保幼激素III(juvenilehormone III),克来范(kelevan),蒙七七七(kinoprene),λ-三氟氯氰菊酯(lambda-cyhalothrin),砷酸铅(lead arsenate),lepimectin,溴苯磷(leptophos),林丹(lindane),啶虫磷(lirimfos),氟丙氧脲(lufenuron),噻唑磷(lythidathion),马拉硫磷(malathion),苄丙二腈(malonoben),叠氮磷(mazidox),灭蚜磷(mecarbam),甲基灭蚜磷(mecarphon),灭蚜松(menazon),二噻磷(mephosfolan),氯化亚汞(mercurous chloride),灭芥(mesulfen),甲亚砜磷(mesulfenfos),氰氟虫腙(metaflumizone),威百亩(metam),虫螨畏(methacrifos),甲胺磷(methamidophos),杀扑磷(methidathion),灭虫威(methiocarb),丁烯胺磷(methocrotophos),灭多虫(methomyl),蒙五一五(methoprene),甲氧滴滴涕(emthoxychlor),甲氧苯酰肼(methoxyfenozide),溴甲烷(methyl bromide),异硫氰酸甲酯(methyl isothiocyanate),甲基氯仿(methyl chloroform),二氯甲烷(methylene chloride),氧卞氟菊酯(metofluthrin),速灭威(metolcarb),噁虫酮(metoxadiazone),速灭磷(mevinphos),自克威(mexacarbate),米尔螨素(milbemectin),米尔贝肟(milbemycin oxime),丙胺氟磷(mipafox),灭蚁灵(mirex),MNAF,久效磷(monocrotophos),茂果(morphothion),莫西克丁(moxidectin),萘肽磷(naftalofos),二溴磷(naled),萘(naphthalene),烟碱(nicotine),氟蚁灵(nifluridide),华光霉素(nikkomycins),硝胺烯啶(nitenpyram),硝虫噻嗪(nithiazine),腈叉威(nitrilacarb),双苯氟脲(novaluron),多氟脲(noviflumuron),氧乐果(omethoate),甲氨叉威(oxamyl),砜吸磷(oxydemeton-methyl),异砜磷(oxydeprofos),砜拌磷(oxydisulfoton),对-二氯苯(paradichlorobenzene),对硫磷(parathion),甲基对硫磷(parathion-methyl),氟幼脲(penfluron),五氯酚(pentachlorophenol),苄氯菊脂(permethrin),芬硫磷(phenkapton),苯醚菊酯(phenothrin),稻丰散(phenthoate),甲拌磷(phorate),伏杀磷(phosalone),棉安磷(phosfolan),亚胺硫磷(phosmet),对氯硫磷(phosnichlor),磷胺(phosphamidon),磷化氢(phosphine),乙丙磷威(phosphocarb),肟硫磷(phoxim),甲基肟硫磷(phoxim-methyl),甲胺嘧磷(pirimetaphos),抗蚜威(pirimicarb),乙基虫螨磷(pirimiphos-ethyl),甲基虫螨磷(pirimiphos-methyl),亚砷酸钾(potassiumarsenite),硫氰酸钾(potassium thiocyanate),pp'-DDT,炔酮菊酯(prallethrin),早熟素I(precocene I),早熟素II(precocene II),早熟素III(precocene III),酰胺嘧啶啉(primidophos),灭螨醇(proclonol),丙溴磷(profenofos),profluthrin,蜱虱威(promacyl),猛杀威(promecarb),丙虫磷(propaphos),克螨特(propargite),烯虫磷(propetamphos),残杀威(propoxur),乙噻唑磷(prothidathion),丙硫磷(prothiofos),发果(prothoate),protrifenbute,吡唑硫磷(pyraclofos),嘧啶威(pyrafluprole),吡菌磷(pyrazophos),反灭虫菊(pyresmethrin),除虫菊酯I(pyrethrin I),除虫菊酯II(pyrethrin II),哒螨酮(pyridaben),啶虫丙醚(pyridalyl),打杀磷(pyridaphenthion),pyrifluquinazon,嘧胺苯醚(pyrimidifen),嘧啶磷(pyrimitate),吡啶醇(pyriprole),蚊蝇醚(pyriproxyfen),苦木(quassia),喹噁啉(quinalphos),喹噁啉(quinalphos),甲基喹噁啉(quinalphos-methyl),喹塞昂(quinothion),quantifies,碘醚柳胺(rafoxanide),苄呋菊酯(resmethrin),鱼藤酮(rotenone),鱼泥汀(ryania),沙巴草(sabadilla),八甲磷(schradan),赛拉菌素(selamectin),灭虫硅醚(silafluofen),亚砷酸钠(sodiumarsenite),氟化钠(sodium fluoride),六氟硅酸钠(sodium hexafluorosilicate),硫氰酸钠(sodium thiocyanate),苏果(sophamide),多虫菌素(spinetoram),艾克敌(spinosad),螺螨酯(spirodiclofen),螺甲螨酯(spiromesifen),螺虫乙酯(spirotetramat),磺苯醚隆(sulcofuron),舒非仑(sulfiram),氟虫胺(sulfluramid),硫特普(sulfotep),硫黄(sulfur),氟化硫(sulfuryl fluoride),乙丙硫磷(sulprofos),τ-氟胺氰菊酯(tau-fluvalinate),噻螨威(tazimcarb),滴滴滴(TDE),双苯酰肼(tebufenozide),吡螨胺(tebufenpyrad),嘧丙磷(tebupirimfos),伏虫隆(teflubenzuron),七氟菊酯(tefluthrin),双硫磷(temephos),特普(TEPP),环戊烯丙菊酯(terallethrin),特丁磷(terbufos),四氯乙烷(tetrachloroethane),杀虫畏(tetrachlorvinphos),三氯杀螨砜(tetradifon),胺菊酯(tetramethrin),杀螨霉素(tetranactin),杀螨好(tetrasul),θ-氯氰菊酯(theta-cypermethrin),噻虫啉(thiacloprid),噻虫嗪(thiamethoxam),噻氯磷(thicrofos),抗虫威(thiocarboxime),硫环杀(thiocyclam),硫双灭多威(thiodicarb),特氨叉威(thiofanox),甲基乙拌磷(thiometon),硫磷嗪(thionazin),克杀螨(thioquinox),杀虫双(thiosultap),敌贝特(thuringiensin),唑虫酰胺(tolfenpyrad),四溴菊酯(tralomethrin),四氟菊酯(transfluthrin),反氯菊酯(transpermethrin),苯螨噻(triarathene),醚苯磺隆(triazamate),三唑磷(triazophos),敌百虫(trichlorfon),异皮蝇磷(trichlormetaphos-3),壤虫磷(trichloronat),氯苯乙丙磷(trifenofos),杀虫隆(triflumuron),混杀威(trimethacarb),硫烯酸酯(triprene),蚜灭多(vamidothion),蚜灭多(vamidothion),氟吡唑虫(vaniliprole),氟吡唑虫(vaniliprole),二甲威(XMC),灭杀威(xylylcarb),ζ-氯氰菊酯(zeta-cypermethrin),和zolaprofos。
另外,可以使用上述农药的任何组合。
另外,可以使用Rynaxypyr(TM),是得自DuPont的一种新型作物保护化学物质,具有防治靶标害虫的功效。
在整个说明书使用的术语“约”表示所述值的±10%,例如术语‘约1.0’包括从0.9至1.1的数值。
提供以下实施例来说明本发明。实施例不意在限制本发明的范围,也不应这样理解它们。除非另有规定,否则量以重量份或重量百分比计。
实施例
胶囊悬浮剂制剂
胶囊悬浮剂制剂的重量百分比总结于表I。总批量基于使用的三氯甲基吡啶的重量,其通常为约25g。乳化剂和交联胺作为具有指定浓度的水溶液添加。微胶囊悬浮剂制剂技术是本领域已知的。另外,本领域也公知,添加顺序和制备微胶囊悬浮剂制剂的过程可以生产具有不同物理特征例如粘度的制剂。以下制备过程是制备过程的一种说明性实例,不应认为其限制本发明。
将油溶性单体PAPI 27(聚亚甲基聚苯基异氰酸酯)(Dow Chemical)添加到广口瓶中。然后以50%三氯甲基吡啶原料溶液的形式添加Nitrapyrin(Dow AgroSciences)和Aromatic 200(Exxon)。将所得有机相与如表I所示的乳化剂的水溶液合并。将所得两相混合物用Silverson L4RT-A高速混合机乳化,所述混合机装备有3/4英寸混合管和通用乳化头。如下实现乳化:首先在相对低速(~1000rpm)混合,其中混合管的末端位于水相中以吸收有机相,直到充分乳化。然后不连续地增加速度,在每次增加之后测量粒度。持续这一过程,直到获得所需粒度。然后逐滴添加水溶性胺(二亚乙基三胺(DETA,Aldrich)或乙二胺(EDA,Aldrich)溶液(10wt%在水中),同时以降低的速率搅拌。在添加完成之后,将所得胶囊悬浮剂再搅拌一分钟。在形成胶囊后,按照表I所示添加Kelzan S(作为1.5%水溶液)、Veegum(作为5%水溶液)、Proxel GXL以及余量水,用Silverson混合机进行最终的均化。
表I示例性组合物1、2、3、4、5、6、和7的主要组分。
1Gohsenol GL-03(聚乙烯醇,购自Nippon Gohsei)
2Kelzan S-黄原胶(购自CP Kelco)
3Proxel GXL(l,2-苯并异噻唑-3(2H)-酮,购自Arch Chemicals,Inc.)
4Kraftsperse 25M(购自MeadWestvaco)
5Tergitol 15-S-7(购自The Dow Chemical Company)
6Veegum(水辉石粘土)(购自R.T.Vanderbilt Co.,Inc.)
7EDA-乙二胺(购自Aldrich)
8DETA-二亚乙基三胺(购自Aldrich)
胶囊的粒度测量
胶囊悬浮剂粒度分布使用装备有小体积样品单元的Malvern Mastersizer 2000光散射粒度仪确定。每种制剂的体积中值分布("VMD")报告于表II。
表II粒度和腔室壁厚度
实施例 | 粒度(μm) | 厚度(nm) | 胺 |
1 | 5 | 10 | EDA |
2 | 10 | 10 | EDA |
3 | 5 | 25 | EDA |
4 | 10 | 25 | EDA |
5 | 2 | 10 | DETA |
6 | 2 | 100 | EDA |
7 | 2 | 100 | EDA |
与实施例7的制剂不同之处在于三氯甲基吡啶的浓度为100g/L,在实施例7中三氯甲基吡啶在制剂中的浓度为140g/1,基于表I中的计算的密度。
EDA-乙二胺
DETA-二亚乙基三胺
计算壁厚度
达到目标壁厚度所需的胶囊壁组分的量的计算基于将球体体积与其半径关联的几何公式。如果假设为芯-壳形态,其中芯由非成壁的非水溶性组分(三氯甲基吡啶,溶剂)构成,而壳由可聚合材料(油溶性和水溶性单体)制成,则方程(1)成立,其涉及芯的体积(Vc)以及芯的体积加上壳的体积(Vs)与它们相应的半径的比率,其中rs是包括壳的胶囊的半径,ls是壳的厚度。
求解方程(1)得到壳的体积:
用质量(mi)和密度(di)替换它们各自的体积(ms/ds=Vs和mc/dc=Vc,其中下标s或c分别表示壳或芯),求解壳的质量得到:
通过比较方程(2)和(3)可以看出密度比ds/dc的作用是当质量用于计算产生具有所需尺寸和壁厚度的胶囊所需的壁组分的量时,应用常数修正系数。因此,为了精确计算ms,芯和壳的密度必须是已知的,或者至少由各组分的密度的加权平均数估算。但是,这些计算的首要目的是将胶囊壁厚度用作便利的概念工具,因此期望其在设计新的胶囊制剂时可有助于理解胶囊性能行为。认为近似值也足以应付这一目的。出于这种考虑,进行简化,将ds/dc的值设置为1,得到方程(4)。
进行替换mc=mo-mOSM、ms=mo+(fWSM/OSM))mOSM-mc、和fWSM/OSM=mWSM/mOSM(水溶性单体与油溶性单体的比率),其中mo是油组分(三氯甲基吡啶,溶剂,油溶性单体)的总质量,mOSM是油溶性单体的质量,mWSM是水溶性单体的质量,求解mOSM得到:
对于mOSM的确定,mWSM的整个量用于计算。在本发明的研究中,对于所有胶囊悬浮剂制剂,使用水溶性单体相对于油溶性单体的1:1的当量比。
相反,对于所有胶囊悬浮剂制剂,胶囊壁厚度ls使用VMD粒度计算得到rs的值和方程(6)。这些值包括在表II中。
测试示例性组合物1、2、3、4、和5的功效
收集总样品Drummer粉质粘壤土(sicl)土壤,使其风干并将其压碎以穿过2-mm筛。在土壤制备之后,将约25克处理土壤放进烧杯中并用包含10mg N(作为(NH4)2SO4)和0.0ppm、0.25ppm或0.50ppm三氯甲基吡啶(基于土壤样品的重量)的7.5ml水使用实施例制剂1-5的每一种进行处理。然后将处理的土壤均匀散布在油表面上并立即用另外25克土壤覆盖。以每种比率重复三次,以及添加三次50克土壤样品,但不添加肥料或抑制剂,将N-Serve 24(Dow AgroSciences)处理的土壤重复三次。一旦液体吸收进土壤,将各种材料混合以达到肥料/实施例制剂的均匀分布。混合后,添加水以使土壤达到田间含水量。不密封烧杯,但是将其覆盖以减少蒸发并保持在室温约25℃。以5天的时间间隔测量从各烧杯损失的水量,如果损失超过2.5ml则将其替换。
在开始温育后的第7天、第14天、第21天、第28天、第35天、第42天、第49天、和第56天,将包含在每个单独烧瓶中的土壤干燥,研磨,和混合。分析子样品的NH4-N,如描述于Mulvaney,R.L.1996;“Nitrogen-Inorganic Forms”,pp.1123-1184。In D.L.Sparks(ed.)Methods of soil analysis:Part 3/SSSA Book Ser.5.SSSA,Madison,WI。如果在任何处理的所有重复中少于30%的N都保持为铵,则停止对该处理的分析。重复的平均值提供于表III和表IV。
表III 0.5ppm三氯甲基吡啶
表IV 0.25ppm三氯甲基吡啶
比较相同比率的微胶囊化的制剂与三氯甲基吡啶N-Serve 24(购自DowAgroSciences)制剂。在第5周,测试的所有五个包封制剂在使用0.5ppm三氯甲基吡啶时性能超过N-Serve 24,证明在相同比率它们可提供较好的残留氮稳定化性能。
包括离子稳定剂的示例性组合物6和7
示例性组合物6和7的水相还包括离子稳定剂。在这些组合物中,使用的离子稳定剂是二辛基磺基琥珀酸钠(Geropon SDS,购自Rhodia)。任何其它适宜的离子稳定剂可以替代或连同二辛基磺基琥珀酸钠使用。
重复四次将示例性组合物6和7、以及N-Serve 24(0.5lb a.i./英亩;0.58kg/公顷)与尿素硝铵(UAN)(160lb/英亩;181.5kg/公顷)的组合、以及重复四次将尿素硝铵(160lb N/英亩;181.5kg/公顷)与0次硝化抑制剂处理施用于不含植被的Drummer粉质粘壤土样品。
在施用示例性制剂之后,制剂中立即混入水分。一旦混入发生,处理物易受到天然降雨和环境影响。
对于每种处理,收集土壤样品并如前提及在开始温育后的第21天、第28天、第35天、第42天、第49天、和第56天按照Mulvaney所述分析其NH4-N。在首次加入处理之后,在第8周从0-3英寸(0-7.6cm)深度收集样品,在第7和第8周从3-6英寸(7.6cm-15.2cm)深度收集另外的样品。在施用当天,从0-3英寸(0-7.6cm)深度收集样品用于NH4-N分析。
硝化抑制剂保持氮为铵态的有效性通过分析土壤样品是否存在铵分子(NH4)来测量。重复的平均值报告于表V。
表V测量对照和示例性组合物6和7的NH4在土壤中的含量
UAN-尿素硝铵
在进一步的分析中,实施例6和7的硝化抑制作用结合那些制剂的表面稳定性。在施用于土壤当天单独的UAN处理和UAN+N-Serve处理混入水分,而两个实施例制剂在混入前铺在土壤表面达一周。当有下雨情形即将发生时,可保护等待水分混入的小块土地免于水分。结果列于表VI。
表VI使用示例性组合物6和7和对照确定的延迟混入
现在参照表V和VI。与N-Serve 24相比,示例性组合物6和7都是更有效的硝化抑制剂。
示例性组合物8和9的制备和组分
用于示例性组合物的胶囊悬浮剂制备的组分的重量百分比列于表VII。总批量为2.1kg(示例性组合物8)或185g(示例性组合物9)。将油溶性单体PAPI 27(聚亚甲基聚苯基异氰酸酯,Dow Chemical)添加到广口瓶中。然后以三氯甲基吡啶技术浓缩原料溶液的形式添加N-Serve TG(Dow AgroSciences;90wt%三氯甲基吡啶)和Aromatic 200(Exxon)。将所得均匀有机相与由Kraftsperse 25M、Tergitol 15-S-7、Geropon SDS、和Proxcel GXL组成的水溶液合并。
将所得两相混合物用Silverson L4RT-A高速混合机乳化,所述混合机装备有%英寸混合管和通用乳化头。如下实现乳化:首先在相对低速(~1000rpm)混合,其中混合管的末端位于水相中以吸收有机相,直到充分乳化。然后不连续地增加速度,在每次增加之后测量粒度。持续这一过程,直到获得所需粒度(2.5微米)。
接着,逐滴添加水溶性胺乙二胺水溶液(在实施例8中,20wt%;在示例性组合物9、10、和11中,30wt%),同时以降低的速率搅拌混合物。在添加水溶性胺之后,将所得胶囊悬浮剂搅拌另外的时间段,以使聚脲壳形成反应进一步进行至完全。在胶囊形成之后,最终阶段包括添加Avicel(作为5wt%水溶液),Kelzan(作为1.5wt%水溶液),Proxel GXL和余量水,如表VII所示,使用Silverson混合机进行最后的均化。包括三氯甲基吡啶、aromatic200、PAPI 27和乙二胺的分散相为49.55wt%(实施例8)或55.94wt%(实施例9)。
示例性组合物10的制备和组分
用于示例性组合物的胶囊悬浮剂制备的组分的重量百分比列于表VII。总批量为100千克。N-Serve TG(Dow AgroSciences,90wt%三氯甲基吡啶)和Aromatic 200(Exxon)的均匀溶液如下制备:使N-Serve TG熔融,并将其添加到溶剂中。向其中添加油溶性单体PAPI 27并混合在一起以产生油相。水相如下制备:将Kraftsperse 25M、Tergitoll5-S-7、Geropon SDS、Proxel GXL、Antifoam 100TND和水混合成均匀溶液。
将油相和水相以1.25:1.0比率一起计量通过转子/定子均化器单元,以产生具有所需粒度(2.5微米)的乳液。持续该过程,直到油相消失。将批料冷却至低于15℃,然后加入胺。在搅拌下将30重量%的胺添加到批料中。将反应容器搅拌最低量的2小时,然后添加粘度组分。粘度相由5w/w%的A vicel、1.5w/w%的Kelzan S、1%的Proxel GXL和水组成。如果需要,添加另外的水以实现目标检测,然后将批料包装以用于最终用途。
示例性组合物11的制备和组分
用于制备示例性组合物中胶囊悬浮剂的组分的重量百分比列于表VII。总批量为400千克。N-Serve TG(Dow AgroSciences,90wt%三氯甲基吡啶)和Aromatic 200(Exxon)的均匀溶液如下制备:使N-Serve TG熔融,并将其添加到溶剂中。向其中添加油溶性单体PAPI 27并混合在一起以产生油相。水相如下制备:将Kraftsperse 25M、Tergitoll5-S-7、Geropon SDS、Proxel GXL、Antifoam 100TND和水混合成均匀溶液。
将油相和水相以1.25:1.0比率一起计量通过转子/定子均化器单元,以产生具有所需粒度(2.5微米)的乳液。持续该过程,直到油相消失。将批料冷却至低于15℃,然后加入胺。如下将30重量%的胺添加到批料中:使用侧流循环流将乳液以100升每分钟的速率泵送。在少于10分钟内、优选少于5分钟内添加胺,以建立胶囊壁。将反应容器搅拌最低量的2小时,然后添加粘度组分。粘度相由5w/w%的A vicel、1.5w/w%的Kelzan S、1%的ProxelGXL和水组成。如果需要,添加另外的水以实现目标检测,然后将批料包装以用于最终用途。
表VII示例性组合物8、9、10、和11的主要组分
1Kraftsperse 25M(购自MeadWestvaco)
2Tergitol 15-S-7(购自The Dow Chemical Company)
3Geropon SDS(二辛基磺基琥珀酸钠,购自Rhodia)
4Antifoam 100IND(购自Harcros Chemicals Inc.)
5Proxel GXL(l,2-苯并异噻唑-3(2H)-酮,购自Arch Chemicals,Inc.)
6EDA-乙二胺(购自Aldrich)在a20wt%水溶液中;b50wt%水溶液中;和c30wt%水溶液中
7Avicel(购自FMC Biopolymer)
8Kelzan S-黄原胶(购自CP Kelco)
确定在悬浮剂中形成微胶囊之后向悬浮剂的水相中添加芳族溶剂的效果
将部分(~195克悬浮剂制剂)的本发明微胶囊悬浮剂制剂称重并放入250mL玻璃瓶中。将具体量(基于重量百分比)的各种芳族溶剂直接添加到包含微胶囊悬浮剂制剂的玻璃瓶中。
将瓶在线型振动器上搅动30-45分钟以制备均匀的微胶囊悬浮剂制剂,即,以将后添加的芳族溶剂溶解或分散在整个微胶囊悬浮剂制剂中。一旦得到均匀制剂,则将样品瓶放进处于约0℃或处于约10℃的冰箱中。在各时间点在每个瓶中采样,测试样品是否在水相存在晶体。
进行湿式筛过程,以确定在10℃和0℃储存样品中作为总微胶囊悬浮剂制剂的重量百分比的晶体形成量。将约20克每一个微胶囊悬浮剂制剂的样品添加到包含100至200克自来水的玻璃烧杯中。使用玻璃搅拌棒搅拌溶液,然后将其倾倒通过75μm目筛。将烧杯用另外的水冲洗,也将冲洗液倾倒通过筛。将自来水倒在筛中的样品上达约30秒以将不牢固的聚集物冲洗通过过滤器。将留在筛上的残留物冲洗到称量滤纸上并真空过滤。使滤纸与样品在真空罩中干燥至少4小时,然后重新称量。使用以下方程计算残留物百分比:残留物百分比(%)=(干燥后的滤纸和残留(g)-滤纸重量(g))/(筛分的总样品(g))。分析分离自微胶囊悬浮剂制剂的三氯甲基吡啶晶体的化学鉴定,并通过使用内标技术的气相色谱分析其纯度。
在2-周和4-周时间间隔,重复在10℃和0℃储存的每个样品的过程,记录残留物重量百分比,将其列于以下表VIII。表VIII中显示的筛分结果表明,Aromatic 200ND(脱萘)在10℃和0℃储存4周之后显著减少了晶体形成和改善结晶稳定性,与未添加晶体抑制剂的对照相比。
表VIII.列出推定的基于溶剂的晶体抑制剂,在形成微胶囊之后将其添加到微胶囊悬浮剂。将包括推定溶剂的悬浮剂(和对照制剂)在10℃和0℃储存,并检测其是否在水相中存在晶体。将包括推定晶体抑制剂的所有样品与不包括任何推定晶体抑制剂的对照微胶囊悬浮剂制剂进行对比测试。(痕量:<0.001%)。
1未添加基于溶剂的晶体抑制剂
2HALLCOMID M-8-10是[N,N-二甲基辛酰胺(N,N-二甲基辛酰胺)和N,N-二甲基癸酰胺(N,N-二甲基癸酰胺)]。CAS Reg.No.1118-92-9,14433-76-2。
参照表VIII。通过在0℃和10℃储存4周之后水相中缺失晶体证实,Aromatic200ND显示最好的结果。环己酮和Hallcomid M-8-10不像Aromatic 200ND表现的一样好。实际上,表VIII表明在0℃储存4周之后,在使用推定晶体抑制剂环己酮和Hallcomid M-8-10制备的样品中三氯甲基吡啶晶体的量(基于重量百分比)增多,相对于不包括添加到悬浮剂水相的另外溶剂的对照组。
这些结果出乎意料地展示了,环己酮可作为三氯甲基吡啶的特别有效的溶剂(在环境温度(24℃)溶解约60wt%三氯甲基吡啶)。环己酮也可在环境温度(24℃)比Aromatic100溶解更多的三氯甲基吡啶,Aromatic 100在环境温度(24℃)仅溶解约51wt%三氯甲基吡啶。
而且,已知Hallcomid M-8-10在环境温度可溶解约50wt%三氯甲基吡啶,在0℃溶解约40wt%三氯甲基吡啶,在-10℃溶解约35wt%三氯甲基吡啶。而Aromatic 150在环境温度仅溶解约43wt%三氯甲基吡啶,在0℃溶解约25wt%三氯甲基吡啶,在-10℃溶解约29wt%三氯甲基吡啶。
基于其与Aromatic 100和150的相似性,预期Aromatic 200ND就溶解或减少三氯甲基吡啶晶体来说与其它芳族溶剂的性能在大约相同水平(即,与环己酮或Hallcomid M-8-10相比较不成功)。正如表VIII中总结的结果表明,证明Aromatic 200ND出乎意料地为较好的晶体形成抑制剂,与该实验测试的其它溶剂相比。
测试Aromatic 200防止在微胶囊悬浮剂的水相中形成三氯甲基吡啶晶体的能力
制备微胶囊悬浮剂制剂,其油相包含在Aromatic 200中的44.7%、47.1%和49.1%三氯甲基吡啶。参见表IX中每种制剂中各组分的清单。将得自每种制剂的样品置于瓶中,将瓶在冰箱中储存,其中冰箱保持在约10℃。在不同时间在每个瓶中采样,使用湿式筛试验测试每个样品是否存在晶体形成。
表IX.用在Aromatic 200油相中包含44.7%、47.1%、和49.1%三氯甲基吡啶制备的微胶囊制剂。在10℃储存之后的湿式筛结果。将测试的所有样品与具有2.00%后包封Aromatic 200添加的对照微胶囊制剂(三氯甲基吡啶,在Aromatic 200油相中包含47.1%三氯甲基吡啶)进行比较。
1Kraftsperse 25M(购自MeadWestvaco)
2Tergitol 15-S-7(购自The Dow Chemical Company)
3Geropon SDS(二辛基磺基琥珀酸钠,购自Rhodia)
4Antifoam 100IND(购自Harcros Chemicals Inc.)
5Proxel GXL(l,2-苯并异噻唑-3(2H)-酮,购自Arch Chemicals,Inc.)
6EDA-乙二胺(购自Aldrich)30wt%水溶液
7Avicel(购自FMC Biopolymer)
8Kelzan S-黄原胶(购自CP Kelco)
9Propylene glycol(购自Aldrich)
10Metasperse 500L(购自Croda Inc.)
用油相微胶囊中含有另外的Aromatic 200制备的微胶囊制剂(44.7%三氯甲基吡啶在油相中,2%另外的Aromatic 200,与用在油相中的47.1%三氯甲基吡啶制备的制剂相比)在10℃储存6周之后产生三氯甲基吡啶晶体。相比之下,用在油相中含有47.1%三氯甲基吡啶且含有后包封添加的2.00%的Aromatic 200制备的微胶囊制剂在10℃储存12周之后未显示形成三氯甲基吡啶晶体。
确定将Aromatic 200添加到微胶囊化的三氯甲基吡啶的悬浮剂(其已经表现出在水相中存在三氯甲基吡啶)的效果
如果不与商购制剂InstinctTM(购自Dow AgroSciences)(其与通过使表IX的第3或5栏组分反应形成的制剂可比较地类似,其表现为水相中包括的三氯甲基吡啶晶体)相同则与其类似的微胶囊悬浮剂制剂,通过添加约2wt%Aromatic 200到水相中来进行处理。将所得混合物在环境温度搅拌30分钟至5小时。在混合之后,没有三氯甲基吡啶的晶体存在于制剂的水相中。这些结果表明,将少量的Aromatic 200添加到微胶囊化的三氯甲基吡啶例如InstinctTM的悬浮剂的水相既可防止在水相中形成三氯甲基吡啶晶体,也可以用于显著减少或甚至消除在这样的悬浮剂的水相中存在的预形成晶体三氯甲基吡啶。
尽管附图和前述说明书已经详细说明和描述了新颖技术,但是认为其在性质上是说明性和非限制性的,应理解仅显示和描述了优选的实施方式,在新颖技术精神内的所有变化和修改均应受到保护。同样,尽管使用具体实施例、理论论据、理由、和例证说明新颖技术,但是这些说明和所附讨论决不应解释为限制该技术。本申请参考的所有专利、专利申请、和引用的文本、科技论文、出版物等全部通过参考并入本申请。
Claims (24)
1.微胶囊悬浮剂制剂,其包含:
(a)悬浮相,所述悬浮相包括多个微胶囊,所述微胶囊的体积中值粒度为约1至约10微米,其中所述微胶囊包括:
(1)微胶囊壁,其通过聚合异氰酸酯和多胺之间进行界面缩聚反应以形成聚脲壳来制备,其重量百分比为所述微胶囊悬浮剂制剂总重量的约0.2至约40%,和
(2)基本上液体的芯,所述基本上液体的芯包封在所述聚脲壳内,其中所述基本上液体的芯包括占整个微胶囊至多约60wt%的2-氯-6-(三氯甲基)吡啶,并且其中在至少15℃的温度,所述基本上液体的芯包括至多1.0wt%的固体2-氯-6-(三氯甲基)吡啶;和
(b)水相,其中所述水相包括至少约1.0wt%的芳族溶剂,基于所述微胶囊悬浮剂制剂的总重量。
2.根据权利要求1的微胶囊悬浮剂制剂,其进一步包括:存在于所述水相中的至少一种离子稳定剂。
3.根据权利要求1的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂是至少一种选自以下的化合物:轻芳烃,脱萘轻芳烃,重芳烃,和脱萘重芳烃。
4.根据权利要求3的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂是脱萘C10-13重芳烃。
5.根据权利要求4的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约1重量%至约10重量%的脱萘C10-13重芳烃。
6.根据权利要求4的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2重量%至约5重量%的脱萘C10-13重芳烃。
7.根据权利要求4的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2.5重量%至约3.0重量%的脱萘C10-13重芳烃。
8.根据权利要求3的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂是C10-13重芳烃。
9.根据权利要求8的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约1重量%至约10重量%的C10-13重芳烃。
10.根据权利要求8的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2重量%至约5重量%的C10-13重芳烃。
11.根据权利要求8的微胶囊悬浮剂制剂,其中存在于所述水相中的芳族溶剂包含约2.5重量%至约3.0重量%的C10-13重芳烃。
12.根据权利要求1的微胶囊悬浮剂制剂,其中所述微胶囊的体积中值粒度为约1至约5微米。
13.根据权利要求1的微胶囊悬浮剂制剂,其中所述悬浮相a)与所述水相b)的比率为约1:0.75至约1:100。
14.根据权利要求1的微胶囊悬浮剂制剂,其中所述悬浮相a)与所述水相b)的比率为约1:1至约1:7。
15.根据权利要求1的微胶囊悬浮剂制剂,其中所述悬浮相a)与所述水相b)的比率为约1:1至约1:4。
16.根据权利要求1的微胶囊悬浮剂制剂,其中所述聚合异氰酸酯是聚亚甲基聚苯基异氰酸酯。
17.一种肥料组合物,其包含:氮肥料和根据权利要求1的微胶囊悬浮剂制剂。
18.根据权利要求17的肥料组合物,其中所述氮肥料是尿素硝铵。
19.抑制生长介质中铵态氮硝化的方法,其包括以下步骤:将根据权利要求1的微胶囊悬浮剂制剂施用于植物生长介质。
20.根据权利要求19的方法,其中将所述制剂加入到所述生长介质中。
21.根据权利要求19的方法,其中将所述制剂施用于生长介质表面。
22.根据权利要求19的方法,其中将所述制剂与农药组合施用或与农药先后施用。
23.根据权利要求19的方法,其中将所述制剂与氮肥料一起施用。
24.根据权利要求23的方法,其中所述氮肥料是尿素硝铵。
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