CN105746509B - 一种杀线虫剂微胶囊及其制备方法 - Google Patents
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Abstract
本发明公开了一种杀线虫剂微胶囊,由如下质量百分比的原料制备而成:囊芯0.5‑1%、有机溶剂20‑35%、壁材0.5‑2%、乳化剂1‑6%、水56‑78%;所述囊芯为杀线虫剂。本发明采用在环境中易降解的高分子物质作为微胶囊的囊壁材料,材料易得,且环境相容性好,选用易回收再利用的有机溶剂,并通过高剪切乳化机强制乳化后制得了一种可控释放的新型杀线虫剂微胶囊,该杀线虫剂持效性能优异,具有耐光照,耐酸碱,缓释等特点,而且节约防治成本,具有较高的经济价值。本发明利用溶剂蒸发法可以制备出不同粒径大小的杀线虫剂微胶囊,制备过程操作简单,周期短,且有机溶剂可以回收再利用。
Description
技术领域
本发明属于农药制备技术领域,尤其涉及一种杀线虫剂微胶囊及其制备方法。
背景技术
根结线虫是植物病原线虫中种类最多,分布最广,危害最重的线虫种类之一,其寄主包括农作物、林木、花卉、蔬菜等3000种植物,尤其是茄科、葫芦科、十字花科等蔬菜受害较为严重。化学防治是根结线虫最有效的防治方法,也是线虫综合防治的主体,而熏蒸性杀线剂溴甲烷由于杀灭有益线虫,且破会大气中臭氧层而被禁用。此外,由于毒性高,残留量大,国内已禁止涕灭威、甲基异柳磷、呋喃丹等非熏蒸性杀线剂在蔬菜上使用,因此,开发低毒、高效杀线虫剂势在必行。
目前,使用杀线虫剂防治根结线虫的主要剂型是乳油和颗粒剂,持效期短,需要重复施药,操作繁琐,增加防治成本,且危害人畜和土壤中有益生物,污染环境;此外,杀线虫剂容易在紫外光或土壤环境(如腐植酸,微生物)等因素影响下发生分解,而分解产物并不完全具有生物活性,从而限制了杀线虫剂利用率与药效的发挥。因此,利用温和条件将杀线虫剂微胶囊化是解决上述问题的有效途径。
发明内容
本发明的目的在于克服现有技术的不足,提供一种杀线虫剂微胶囊及其制备方法。
为了实现本发明的目的,采用的技术方案如下:
一种杀线虫剂微胶囊,由如下质量百分比的原料制备而成:囊芯0.5-1%、有机溶剂20-35%、壁材0.5-2%、乳化剂1-6%、水56-78%;
所述的所述囊芯为杀线虫剂;所述杀线虫剂选自噻唑膦、灭线磷、阿维菌素、甲维盐、吡虫啉和棉隆之中的一种或者多种的组合;
所述的壁材为聚乳酸、乙基纤维素、聚甲基丙烯酸甲酯、壳聚糖衍生物之中的一种;
所述的有机溶剂选自丙酮、乙酸乙酯、二氯甲烷中的一种或几种;
所述的乳化剂可以是苯乙烯基苯酚聚氧乙烯醚、烷基酚甲醛树脂聚氧乙烯醚、三苯乙烯基苯酚聚氧乙烯聚氧丙烯醚、三苯乙烯基苯酚聚氧丙烯聚氧乙烯醚、苯乙烯基苯酚甲醛树脂聚氧乙烯-聚氧丙烯嵌段型聚醚、苯乙烯苯酚甲醛树脂聚氧乙烯聚氧丙烯醚、聚氧乙烯失水山梨醇脂肪酸酯、蓖麻油聚氧乙烯醚、烷基糖苷之中的一种或者多种的组合;所述的苯乙烯基苯酚聚氧乙烯醚为农乳600#;所述的烷基酚甲醛树脂聚氧乙烯醚为农乳700#;所述的三苯乙烯基苯酚聚氧乙烯聚氧丙烯醚为农乳1601#;所述的三苯乙烯基苯酚聚氧丙烯聚氧乙烯醚为农乳1602#;所述的苯乙烯基苯酚甲醛树脂聚氧乙烯-聚氧丙烯嵌段型聚醚为宁乳33#;所述的苯乙烯苯酚甲醛树脂聚氧乙烯聚氧丙烯醚为宁乳34#;所述的聚氧乙烯失水山梨醇脂肪酸酯为Tween20、Tween60、Tween80中的任一种;所述的蓖麻油聚氧乙烯醚为EL-20、EL-40、EL-60、EL-80中的任一种;
所述杀线虫剂选自噻唑膦、灭线磷、阿维菌素、甲维盐、吡虫啉和棉隆之中的一种或者多种的组合。
如上所述的杀线虫剂微胶囊,其制备方法包括如下步骤:
1)将杀线虫剂、壁材与有机溶剂混合,制成透明溶液A;
2)将乳化剂与水混合,搅拌均匀,制成透明溶液B;
3)将步骤1)所得透明溶液A和步骤2)所得透明溶液B混合,用高速剪切机高速剪切,得到乳状液;
4)将步骤3)所得乳状液通过旋转蒸发仪去除其中的有机溶剂,得到悬浮液;
5)将步骤4)得到的悬浮液经过过滤、洗涤和干燥,使微球逐渐固化,即得所述杀线虫剂微胶囊;
在步骤3)中,高剪切乳化机以10000-15000rpm的搅拌速度强制乳化4-15min;在步骤4)中,所得乳状液利用旋转蒸发仪将溶剂蒸出的温度优选为20-60℃。
本发明具有的有益效果是:
本发明采用在环境中易降解的高分子物质作为微胶囊的囊壁材料,材料易得,且环境相容性好,选用易回收再利用的有机溶剂,并通过高剪切乳化机强制乳化后制得了一种可控释放的新型杀线虫剂微胶囊,该杀线虫剂持效性能优异,具有耐光照,耐酸碱,缓释等特点,而且节约防治成本,具有较高的经济价值。本发明利用溶剂蒸发法可以制备出不同粒径大小的杀线虫剂微胶囊,制备过程操作简单,周期短,且有机溶剂可以回收再利用。
与传统剂型相比,本发明的杀线虫剂微胶囊具有以下突出优点:1)改善稳定性,避免因环境因素(如光照、雨水、微生物等)造成有效成分的降解和流失。2)延长持效期,减少施药数量和频率,提高利用率,节约农药用量。3)扩大使用范围,降低对人畜及其有益生物的毒性作用。
附图说明
图1杀线虫剂微胶囊制备工艺流程图;
图2杀线虫剂微胶囊的光学显微镜照片;
图3杀线虫剂微胶囊的扫描电子显微镜照片。
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,以下结合附图及实施例,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子仅仅用以解释本发明,并不用于限定本发明。
实施例1
1)称取0.20g杀线虫剂原药,溶于6.00g二氯甲烷中,搅拌至原药完全溶解,随后加入0.25g乙基纤维素于溶液中,搅拌至乙基纤维素完全溶解,制成含杀线虫剂和乙基纤维素的透明溶液A;
2)称取12.75g去离子水于烧杯中,加入0.80g乳化剂EL-40,随后磁力搅拌至乳化剂完全溶解,制成含乳化剂的透明溶液B;
3)将步骤1)所得透明溶液A和步骤2)所得透明溶液B混合,用高速剪切机高速(10000rpm)剪切4min,得到乳状液;
4)将步骤3)所得乳状液在40℃条件下通过旋转蒸发仪去除其中的二氯甲烷,得到含微球的悬浮液;
5)将步骤4)得到的含微球悬浮液经过过滤、去离子水洗涤和干燥,使微球逐渐固化,即得所述杀线虫剂微胶囊。
实施例2
1)称取0.20g杀线虫剂原药,溶于5.00g二氯甲烷中,搅拌至原药完全溶解,随后加入0.15g乙基纤维素于溶液中,搅拌至乙基纤维素完全溶解,制成含杀线虫剂和乙基纤维素的透明溶液A;
2)称取13.85g去离子水于烧杯中,加入0.80g乳化剂EL-40,随后磁力搅拌至乳化剂完全溶解,制成含乳化剂的透明溶液B;
3)将步骤1)所得透明溶液A和步骤2)所得透明溶液B混合,用高速剪切机高速(10000rpm)剪切6min,得到乳状液;
4)将步骤3)所得乳状液在40℃条件下通过旋转蒸发仪去除其中的二氯甲烷,得到含微球的悬浮液;
5)将步骤4)得到的含微球悬浮液经过过滤、去离子水洗涤和干燥,使微球逐渐固化,即得所述杀线虫剂微胶囊。
实施例3
1)称取0.20g杀线虫剂原药,溶于4.00g二氯甲烷中,搅拌至原药完全溶解,随后加入0.15g乙基纤维素于溶液中,搅拌至乙基纤维素完全溶解,制成含杀线虫剂和乙基纤维素的透明溶液A;
2)称取15.25g去离子水于烧杯中,加入0.40g乳化剂EL-40,随后磁力搅拌至乳化剂完全溶解,制成含乳化剂的透明溶液B;
3)将步骤1)所得透明溶液A和步骤2)所得透明溶液B混合,用高速剪切机高速(10000rpm)剪切4min,得到乳状液;
4)将步骤3)所得乳状液在40℃条件下通过旋转蒸发仪去除其中的二氯甲烷,得到含微球的悬浮液;
5)将步骤4)得到的悬浮液经过过滤、去离子水洗涤和干燥,使微球逐渐固化,即得所述杀线虫剂微胶囊。
实施例4
1)称取0.20g杀线虫剂原药,溶于5.00g二氯甲烷中,搅拌至原药完全溶解,随后加入0.20g乙基纤维素于溶液中,搅拌至乙基纤维素完全溶解,制成含杀线虫剂和乙基纤维素的透明溶液A;
2)称取13.40g去离子水于烧杯中,加入1.20g乳化剂EL-40,随后磁力搅拌至乳化剂完全溶解,制成含乳化剂的透明溶液B;
3)将步骤1)所得透明溶液A和步骤2)所得透明溶液B混合,用高速剪切机高速(10000rpm)剪切4min,得到乳状液;
4)将步骤3)所得乳状液在40℃条件下通过旋转蒸发仪去除其中的二氯甲烷,得到含微球的悬浮液;
5)将步骤4)得到的悬浮液经过过滤、去离子水洗涤和干燥,使微球逐渐固化,即得所述杀线虫剂微胶囊。
对上述4个实施例得到的产品进行平均粒径,包封率和载药量等性能的测定,结果如表1:
表1杀线虫剂微胶囊的性能测定结果
由此可知,该微胶囊具有光滑而致密的外观形貌,平均粒径可调,同时具有较高的包封率和载药量。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (1)
1.一种杀线虫剂微胶囊的制备方法,其特征在于,由如下质量百分比的原料制备而成:囊芯0.5-1%、有机溶剂20-35%、壁材0.5-2%、乳化剂1-6%、水56-78%;囊芯为选自噻唑膦、灭线磷、阿维菌素、甲维盐中的杀线虫剂的一种;壁材为乙基纤维素;有机溶剂选自丙酮、乙酸乙酯、二氯甲烷中的一种或几种;乳化剂选自EL-40;
由如下步骤组成:
1)将杀线虫剂、壁材与有机溶剂混合,制成透明溶液A;
2)将乳化剂与水混合,搅拌均匀,制成透明溶液B;
3)将步骤 1)所得透明溶液A和步骤 2)所得透明溶液B混合,用高速剪切机高速剪切,得到乳状液;
4)将步骤 3)所得乳状液通过旋转蒸发仪去除其中的有机溶剂,得到悬浮液;
5)将步骤 4)得到的悬浮液经过过滤、洗涤和干燥,使微球逐渐固化,即得所述杀线虫剂微胶囊;
在步骤3)中,高剪切乳化机以10000-15000 rpm的搅拌速度强制乳化4-6 min;
在步骤4)中,所得乳状液利用旋转蒸发仪将溶剂蒸出的温度为40℃。
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