CN107691434A - 农药微胶囊悬浮液的加工方法 - Google Patents

农药微胶囊悬浮液的加工方法 Download PDF

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Publication number
CN107691434A
CN107691434A CN201710800899.9A CN201710800899A CN107691434A CN 107691434 A CN107691434 A CN 107691434A CN 201710800899 A CN201710800899 A CN 201710800899A CN 107691434 A CN107691434 A CN 107691434A
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China
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parts
micro capsule
capsule suspension
pesticide micro
processing method
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CN201710800899.9A
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Inventor
肖尧
盛勇
沙桐
许立
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Zhong Hua Yunlong company limited
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Chengdu Research And Development Centre Of Zhong Hua Chemical Fertilizer Co Ltd
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Priority to CN201710800899.9A priority Critical patent/CN107691434A/zh
Publication of CN107691434A publication Critical patent/CN107691434A/zh
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Abstract

本发明公开了一种农药微胶囊悬浮液及其加工方法，其加工方法是将二异氰酸酯、丙烯酸羟乙酯和二元醇混合，并进行反应，再加入乙酸乙酯和农药，混合均匀得到油相；将多元醇或多元胺与乳化剂加入水中，混合均匀得到水相；将油相和水相混合并进行乳化和反应，得到农药微胶囊悬浮液。这种农药微胶囊悬浮液适用对象范围广，可用于大部分常见农药的微胶囊化；采用界面聚合法合成高度交联聚氨酯作为壁材，大大降低外界环境因素对囊心农药的影响；通过特殊分子结构设计，聚氨酯壁材在自然条件下可逐渐降解，降低了对土壤以及环境的污染；该农药微胶囊以低毒性的乙酸乙酯为有机溶剂溶解农药作为油相，大大降低了生产和使用过程中对人体和环境造成的危害。

Description

农药微胶囊悬浮液的加工方法
技术领域
本发明涉及缓释农药领域，具体地说涉及农药微胶囊悬浮液的加工方法。
背景技术
农药微胶囊是指通过化学、物理或物理化学的方法，以某种固体材料为囊壁，将含有农药的囊心包裹其中而形成的微型胶囊；同时在悬浮稳定剂、乳化剂的帮助下分散、悬浮于连续相液体中，从而得到农药微胶囊悬浮液。微胶囊囊壁将囊心与外界隔离，在适当条件下，囊心中的农药随着壁材被破坏而释放。如果所选壁材具有半渗透性，则农药通过溶解、扩散、渗透等过程，透过囊壁释放至外界环境中。与常规农药相比，农药微胶囊具有以下优点：①保护农药敏感成分，减少外界环境例如水分、光照、微生物的影响，提高农药稳定性；②减弱或掩蔽不友好气味，降低对人畜的吸入性危害；③提供缓释效果，提高农药利用率，减少农药用量，延长有效期；④减少施药数量和频率，降低农业工作者劳动强度，减轻农药对人体和环境的危害。
制备农药微胶囊主要采用化学法，其中又以原位聚合法和界面聚合法最为常用，综合性能最佳。原位聚合法是将固态或液态农药溶解于有机溶剂中作为囊心（油相），在乳化剂的帮助下于水中高速剪切乳化形成水包油乳液。只溶解在有机溶剂或者水中的可聚合组分，在一定反应条件下生成不溶性聚合物，并沉积在囊心表面形成囊壁；再添加适量助剂，得到农药微胶囊悬浮液。该方法最大的缺陷是不能保证反应生成的不溶性聚合物一定沉积于囊心表面形成囊壁，而有可能仅仅悬浮于有机溶剂或水中，从而导致农药包覆率较低。申请号为200610114438.8和201410762586.5的两篇中国专利均是采用原位聚合法以二氧化硅为壁材制备农药微胶囊，未能解决农药包覆率低的问题。界面聚合法与原位聚合法有相似之处，不同之处在于至少含两种反应组分，分别溶解于有机溶剂和水中，在油-水界面处接触并在一定条件下反应形成囊壁。与原位聚合法相比，界面聚合法更能保证在油-水界面形成囊壁，从而更为完整地包裹囊心，得到农药微胶囊。界面聚合法常见的囊壁材料主要包括聚酯、聚脲、聚氨酯以及聚酰胺，这几种聚合物一般为非交联体系，可能溶解于囊心的有机溶剂中，因此不能保证反应结束后得到完整的固体囊壁，从而导致农药微胶囊性能变差。
作为一种高分子材料，聚氨酯用作农药微胶囊壁材最大的弊端是难以降解。农药微胶囊施用于土壤后，残留的聚氨酯如果无法降解，势必给土壤带来一定程度的污染，同时影响作物的生长以及粮食产量。
发明内容
本发明的目的在于提供一种农药微胶囊悬浮液的加工方法，该微胶囊悬浮液采用界面聚合法制备，以高度交联聚氨酯为壁材；同时以低毒性的乙酸乙酯为有机溶剂溶解农药，降低了对相关人员的危害，尤为重要的是，通过特殊分子结构设计，聚氨酯壁材在自然条件下可逐渐降解，解决了现有聚氨酯壁材难以降解，对环境的污染严重的问题。
为解决上述的技术问题，本发明采用以下技术方案：
一种农药微胶囊悬浮液的加工方法，包括：
油相的制备：将二异氰酸酯、丙烯酸羟乙酯和二元醇混合，得到混合液并进行反应，再加入乙酸乙酯和农药，混合均匀得到油相；
水相的制备：将多元醇或多元胺、乳化剂、水溶性引发剂和N,N’-亚甲基双丙烯酰胺加入水中，混合均匀得到水相；
油相水相混合：将油相和水相混合乳化后进行反应，得到农药微胶囊悬浮液。
作为优选的，原料按重量计包括：
农药 10-100份；
乳化剂 10-200份；
乙酸乙酯 200-2000份；
水 300-5000份；
二异氰酸酯 10-100份；
丙烯酸羟乙酯 1-50份；
二元醇 10-400份；
多元醇或多元胺 1-50份；
N,N’-亚甲基双丙烯酰胺 0.001-0.5份；
水溶性引发剂 0.001-0.5份。
作为优选的，所述乳化剂为烷基酚聚氧乙烯醚、壬基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、烷基硫酸盐、烷基磺酸盐、烷基苯磺酸盐、吐温和司盘中的一种或多种。
作为优选的，二异氰酸酯为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、二苯基甲烷二异氰酸酯、甲苯二异氰酸酯、二环己基甲烷二异氰酸酯、对苯二异氰酸酯中的一种。
作为优选的，所述二元醇为聚乙二醇、聚丙二醇、聚四氢呋喃醚二醇、聚己二酸丁二酯二醇、聚己二酸乙二酯二醇、聚己内酯二醇、三乙醇胺、聚碳酸酯二醇、丙二醇、丁二醇、己二醇中的一种。
作为优选的，所述多元醇为丙三醇、己三醇、三羟甲基乙烷、三羟甲基丙烷、季戊四醇中的一种。
作为优选的，所述多元胺为二乙烯三胺、三乙烯四胺、四乙烯五胺中的一种；
优选的，所述水溶性引发剂为过硫酸钾或过硫酸铵。
作为优选的，所述混合液在50-90℃搅拌反应1-10小时。
作为优选的，油相水相混合步骤中，所述乳化是在20-50℃搅拌1-120分钟，得到乳液C。
作为优选的，所述乳液C于20-70℃搅拌反应0.1-10小时，得到农药微胶囊悬浮液。
与现有技术相比，本发明的有益效果至少是如下之一：
本发明的农药微胶囊悬浮液制备方法适用对象范围广，可用于大部分常见农药例如毒死蜱、辛硫磷、马拉硫磷、吡虫啉、杀虫双、杀虫单、抗蚜威、噻虫嗪、噻虫胺、阿维菌素的微胶囊化。
本发明的农药微胶囊悬浮液制备方法采用界面聚合法，以N,N’-亚甲基双丙烯酰胺和多元醇或多元胺为交联剂合成高度交联聚氨酯作为壁材，因而农药微胶囊包覆效果好，包覆率高，大大降低外界环境因素对囊心农药的影响。
引入N,N’-亚甲基双丙烯酰胺作为交联剂之一，在自然光中的紫外光（波长范围200-360nm）作用下，部分聚合物分子链中的碳-碳单键断裂，进一步引起聚合物连锁解聚，使聚氨酯逐渐降解，降低对土壤的污染和危害。
本发明的农药微胶囊悬浮液以低毒性的乙酸乙酯为有机溶剂溶解农药作为油相，进一步降低了对人体和环境的危害。
附图说明
图1为本申请实施例7中得到的农药微胶囊悬浮液放大400倍的光学显微镜照片。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1：
将100份二苯基甲烷二异氰酸酯、20份丙烯酸羟乙酯和200份聚己内酯二醇于90℃搅拌反应1小时，再加入2000份乙酸乙酯配成溶液。将100份阿维菌素溶解于上述乙酸乙酯溶液中得到油相。将160份吐温、40份司盘、12份丙三醇、0.2份N,N’-亚甲基双丙烯酰胺以及0.08份过硫酸钾溶解于5000份水中得到水相。将油相加入水相中，于50℃高速搅拌乳化1分钟得到乳液。将乳液于70℃搅拌反应0.1小时，得到阿维菌素微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为82.0%，聚氨酯壁材降解时间为173天。
实施例2：
将80份甲苯二异氰酸酯、50份丙烯酸羟乙酯和220份聚己二酸丁二酯二醇于50℃搅拌反应10小时，再加入1800份乙酸乙酯配成溶液。将100份马拉硫磷溶解于上述乙酸乙酯溶液中得到油相。将160份壬基酚聚氧乙烯醚、20份脂肪醇聚氧乙烯醚、15份二乙烯三胺、0.5份N,N’-亚甲基双丙烯酰胺以及0.12份过硫酸钾溶解于4000份水中得到水相。将油相加入水相中，于20℃高速搅拌乳化120分钟得到乳液。将乳液于20℃搅拌反应10小时，得到马拉硫磷微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为84.2%，聚氨酯壁材降解时间为61天。
实施例3：
将100份异佛尔酮二异氰酸酯、2份丙烯酸羟乙酯和400份聚四氢呋喃醚二醇于90℃搅拌反应4小时，再加入1000份乙酸乙酯配成溶液。将85份辛硫磷溶解于上述乙酸乙酯溶液中得到油相。将300份脂肪醇聚氧乙烯醚、30份季戊四醇、0.1份N,N’-亚甲基双丙烯酰胺以及0.05份过硫酸钾溶解于1800份水中得到水相。将油相加入水相中，于35℃高速搅拌乳化15分钟得到乳液。将乳液于65℃搅拌反应6.5小时，得到辛硫磷微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为92.7%，聚氨酯壁材降解时间为272天。
实施例4：
将90份二环己基甲烷二异氰酸酯、20份丙烯酸羟乙酯和70份聚碳酸脂二醇于80℃搅拌反应3.5小时，再加入1600份乙酸乙酯配成溶液。将90份毒死蜱溶解于上述乙酸乙酯溶液中得到油相。将120份脂肪醇聚氧乙烯醚、30份烷基苯磺酸盐、50份三乙烯四胺、0.03份N,N’-亚甲基双丙烯酰胺以及0.5份过硫酸钾溶解于4500份水中得到水相。将油相加入水相中，于25℃高速搅拌乳化30分钟得到乳液。将乳液于30℃搅拌反应0.5小时，再于60℃搅拌反应5小时，得到毒死蜱微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为61.6%，聚氨酯壁材降解时间为90天。
实施例5：
将18份异佛尔酮二异氰酸酯、2份丙烯酸羟乙酯和30份聚四氢呋喃醚二醇于90℃搅拌反应3小时，再加入400份乙酸乙酯配成溶液。将12份辛硫磷溶解于上述乙酸乙酯溶液中得到油相。将30份脂肪醇聚氧乙烯醚、3份季戊四醇、0.01份N,N’-亚甲基双丙烯酰胺以及0.007份过硫酸钾溶解于900份水中得到水相。将油相加入水相中，于30℃高速搅拌乳化10分钟得到乳液。将乳液于65℃搅拌反应5小时，得到辛硫磷微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为85.7%，聚氨酯壁材降解时间为235天。
实施例6：
将8份甲苯二异氰酸酯、3份丙烯酸羟乙酯和30份聚己二酸丁二酯二醇于80℃搅拌反应2小时，再加入500份乙酸乙酯配成溶液。将15份噻虫胺溶解于上述乙酸乙酯溶液中得到油相。将16份壬基酚聚氧乙烯醚、8份烷基磺酸盐、1.5份二乙烯三胺、0.03份N,N’-亚甲基双丙烯酰胺以及0.012份过硫酸钾溶解于1200份水中得到水相。将油相加入水相中，于20℃高速搅拌乳化30分钟得到乳液。将乳液于20℃搅拌反应0.2小时，再于65℃搅拌反应5小时，得到噻虫胺微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为77.2%，聚氨酯壁材降解时间为126天。
实施例7：
将10份二苯基甲烷二异氰酸酯、2份丙烯酸羟乙酯和20份聚己内酯二醇于70℃搅拌反应2.5小时，再加入400份乙酸乙酯配成溶液。将10份阿维菌素溶解于上述乙酸乙酯溶液中得到油相。将16份吐温、4份司盘、1.2份丙三醇、0.02份N,N’-亚甲基双丙烯酰胺以及0.008份过硫酸钾溶解于1000份水中得到水相。将油相加入水相中，于40℃高速搅拌乳化20分钟得到乳液。将乳液于55℃搅拌反应8小时，得到阿维菌素微胶囊悬浮液，如图1所示。
此实施例中微胶囊的农药包覆率为81.7%，聚氨酯壁材降解时间为186天。
实施例8：
将14份对苯二异氰酸酯、7份丙烯酸羟乙酯和20份聚丙二醇于75℃搅拌反应6小时，再加入700份乙酸乙酯配成溶液。将30份吡虫啉溶解于上述乙酸乙酯溶液中得到油相。将40份烷基酚聚氧乙烯醚、2份己三醇、0.04份N,N’-亚甲基双丙烯酰胺以及0.02份过硫酸钾溶解于1500份水中得到水相。将油相加入水相中，于45℃高速搅拌乳化10分钟得到乳液。将乳液于60℃搅拌反应6小时，得到吡虫啉微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为58.7%，聚氨酯壁材降解时间为102天。
实施例9：
将30份二环己基甲烷二异氰酸酯、10份丙烯酸羟乙酯和50份聚碳酸脂二醇于70℃搅拌反应4小时，再加入800份乙酸乙酯配成溶液。将35份杀虫单溶解于上述乙酸乙酯溶液中得到油相。将40份脂肪醇聚氧乙烯醚、10份烷基硫酸盐、4份三乙烯四胺、0.01份N,N’-亚甲基双丙烯酰胺以及0.02份过硫酸钾溶解于2000份水中得到水相。将油相加入水相中，于25℃高速搅拌乳化20分钟得到乳液。将乳液于20℃搅拌反应0.5小时，再于60℃搅拌反应5小时，得到杀虫单微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为65.7%，聚氨酯壁材降解时间为385天。
实施例10：
将30份六亚甲基二异氰酸酯、8份丙烯酸羟乙酯和20份聚乙二醇于85℃搅拌反应3小时，再加入500份乙酸乙酯配成溶液。将20份抗蚜威溶解于上述乙酸乙酯溶液中得到油相。将20份脂肪醇聚氧乙烯醚、10份吐温、4份四乙烯五胺、0.04份N,N’-亚甲基双丙烯酰胺以及0.03份过硫酸钾溶解于900份水中得到水相。将油相加入水相中，于25℃高速搅拌乳化20分钟得到乳液。将乳液于25℃搅拌反应1小时，再于70℃搅拌反应2小时，得到抗蚜威微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为79.5%，聚氨酯壁材降解时间为148天。
实施例11：
将10份二苯甲甲烷二异氰酸酯、1份丙烯酸羟乙酯和40份聚己内酯二醇于70℃搅拌反应3小时，再加入200份乙酸乙酯配成溶液。将10份杀虫双溶解于上述乙酸乙酯溶液中得到油相。将9份吐温、1份司盘、1份丙三醇、0.02份N,N’-亚甲基双丙烯酰胺以及0.001份过硫酸钾溶解于300份水中得到水相。将油相加入水相中，于40℃高速搅拌乳化30分钟得到乳液。将乳液于55℃搅拌反应8.5小时，得到杀虫双微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为88.3%，聚氨酯壁材降解时间为205天。
实施例12：
将24份六亚甲基二异氰酸酯、7份丙烯酸羟乙酯和10份聚乙二醇于85℃搅拌反应3.5小时，再加入300份乙酸乙酯配成溶液。将13份抗蚜威溶解于上述乙酸乙酯溶液中得到油相。将20份脂肪醇聚氧乙烯醚、4份四乙烯五胺、0.001份N,N’-亚甲基双丙烯酰胺以及0.02份过硫酸钾溶解于700份水中得到水相。将油相加入水相中，于25℃高速搅拌乳化10分钟得到乳液。将乳液于25℃搅拌反应0.5小时，再于65℃搅拌反应3小时，得到抗蚜威微胶囊悬浮液。
此实施例中微胶囊的农药包覆率为83.4%，聚氨酯壁材降解时间为595天。
本申请实施例中微胶囊的农药包覆率通过如下方法测定：
将制备得到的微胶囊悬浮液（其中农药含量为M）直接干燥，取0.5g干燥后固体，用30ml乙醇浸没，得到悬浊液，于70℃加热5分钟。将悬浊液转移至100ml容量瓶定容；取40ml定容后的悬浊液，保持转速10000r/min离心10分钟。移取1ml离心后上清液，定容至50ml。用紫外-可见分光光度计测定溶液中农药对应波长处的吸光度，再由标准曲线方程计算农药含量M1。制备不含农药的同种配方的微胶囊悬浮液，重复上述操作，得到空白样的对应含量M2。包覆率K由如下公式计算：
K=(M-M1+M2)/M·100%
本申请实施例中聚氨酯壁材降解时间测定方法：参照国家标准“降解塑料的定义、分类、标志和降解性能要求”（GB/T20197-2006）。
根据上述12个实施例，实施例2中聚氨酯壁材降解时间仅为61天，远远优于其他实施例，而实施例3中微胶囊的农药包覆率达到了92.7%，也远优于其他的实施例，而且在现有技术中也处于领先地位，综合包覆率和聚氨酯壁材的降解时间两项指标，认为实施例2中的方案较优。
尽管这里参照本发明的多个解释性实施例对本发明进行了描述，但是，应该理解，本领域技术人员可以设计出很多其他的修改和实施方式，这些修改和实施方式将落在本申请公开的原则范围和精神之内。更具体地说，在本申请公开和权利要求的范围内，可以对主题组合布局的组成部件和/或布局进行多种变型和改进。除了对组成部件和/或布局进行的变形和改进外，对于本领域技术人员来说，其他的用途也将是明显的。

Claims (10)

1.一种农药微胶囊悬浮液的加工方法，其特征在于，包括：
油相的制备：将二异氰酸酯、丙烯酸羟乙酯和二元醇混合，得到混合液并进行反应，再加入乙酸乙酯和农药，混合均匀得到油相；
水相的制备：将多元醇或多元胺、乳化剂、水溶性引发剂和N, N’-亚甲基双丙烯酰胺加入水中，混合均匀得到水相；
油相水相混合：将油相和水相混合乳化后进行反应，得到农药微胶囊悬浮液。
2.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，原料按重量计包括：
农药 10-100份；
乳化剂 10-200份；
乙酸乙酯 200-2000份；
水 300-5000份；
二异氰酸酯 10-100份；
丙烯酸羟乙酯 1-50份；
二元醇 10-400份；
多元醇或多元胺 1-50份；
N, N’-亚甲基双丙烯酰胺 0.001-0.5份；
水溶性引发剂 0.001-0.5份。
3.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，所述乳化剂为烷基酚聚氧乙烯醚、壬基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、烷基硫酸盐、烷基磺酸盐、烷基苯磺酸盐、吐温和司盘中的一种或多种。
4.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，二异氰酸酯为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、二苯基甲烷二异氰酸酯、甲苯二异氰酸酯、二环己基甲烷二异氰酸酯、对苯二异氰酸酯中的一种。
5.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，所述二元醇为聚乙二醇、聚丙二醇、聚四氢呋喃醚二醇、聚己二酸丁二酯二醇、聚己二酸乙二酯二醇、聚己内酯二醇、聚碳酸酯二醇、丙二醇、丁二醇、己二醇中的一种。
6.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，所述多元醇为丙三醇、己三醇、三乙醇胺、三羟甲基乙烷、三羟甲基丙烷、季戊四醇中的一种。
7.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，所述多元胺为二乙烯三胺、三乙烯四胺、四乙烯五胺中的一种；
优选的，所述水溶性引发剂为过硫酸钾或过硫酸铵。
8.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，所述混合液在50-90℃搅拌反应1-10小时。
9.根据权利要求1所述的农药微胶囊悬浮液的加工方法，其特征在于，油相水相混合步骤中，所述乳化是在20-50℃搅拌1-120分钟，得到乳液C。
10.根据权利要求9所述的农药微胶囊悬浮液的加工方法，其特征在于，所述乳液C于20-70℃搅拌反应0.1-10小时，得到农药微胶囊悬浮液。
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