CN106614566A - 一种含丙环唑的杀菌型毒死蜱微囊悬浮剂及其制备方法 - Google Patents

一种含丙环唑的杀菌型毒死蜱微囊悬浮剂及其制备方法 Download PDF

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CN106614566A
CN106614566A CN201611230288.7A CN201611230288A CN106614566A CN 106614566 A CN106614566 A CN 106614566A CN 201611230288 A CN201611230288 A CN 201611230288A CN 106614566 A CN106614566 A CN 106614566A
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Abstract

本发明公开了一种含丙环唑的杀菌型毒死蜱微囊悬浮剂，及其制备工艺，其特征在于，以毒死蜱、聚碳酸亚丙酯、聚乙烯醇、聚乳酸、明胶、乳化硅油、海藻酸钠、有机膨润土、MCM‑41分子筛、KH550、聚丙烯酸、水滑石、丙环唑、液体石蜡、乳化剂OP‑10等为原料。本发明中有机膨润土与海藻酸钠共混改性，实现插层，提高疏水性及吸附效果，与生物可降解材料聚乳酸复合为壁材，制得药物缓释微胶囊。用KH550对MCM‑41分子筛进行改性作为载体，以带负电荷的聚丙烯酸为功能分子，通过静电吸附作用制备了缓释体系。以层状水滑石为主体，以微胶囊化的毒死蜱为客体分子，制备得到插层材料，得到一种毒死蜱微囊悬浮剂。

Description

一种含丙环唑的杀菌型毒死蜱微囊悬浮剂及其制备方法
技术领域
本发明涉及农药领域，具体涉及一种含丙环唑的杀菌型毒死蜱微囊悬浮剂，及其制备工艺。
背景技术
毒死蜱是广泛使用的有机磷杀虫剂，可作为高毒农药的替代品，可应用于卫生及农业害虫的防治，可有效防治粮食、蔬菜、果树等多种作物上的百余种害虫。毒死蜱异味大、相对易光解、对敏感作物易产生药害，为提高其安全性与持效期、降低对环境的污染，将其进行微囊化。
孟锐在其研究论文《可降解聚碳酸亚丙酯-毒死蜱微胶囊的制备及缓释性能评价》一文中，以聚碳酸亚丙酯(PPC)为壁材，聚乙烯醇(PVA)为连续相稳定剂，采用乳化溶剂挥发法制备了包裹毒死蜱的可降解微胶囊，微胶囊对毒死蜱具有明显的缓释效应。取毒死蜱原药，将PPC溶于二氯甲烷中作为有机相，以PVA作为连续相，将连续相与有机相混合后在高剪切乳化分散机下乳化分散，使之形成稳定的O/W型乳液，室温下搅拌4h，直至二氯甲烷完全挥发，使微胶囊固化，将微胶囊悬浊液离心分离，用蒸馏水洗涤数次后冷冻干燥，收集微胶囊干样。但是存在缓释性能不足。
本发明中聚乳酸是一种高分子聚合物，具有优良的生物相容性、可降解性，无毒害；海藻酸钠具有无毒、低成本、可生物降解、生物相容性好的特点，有机膨润土与海藻酸钠共混改性，实现插层，提高疏水性及吸附效果，与生物可降解材料聚乳酸复合为壁材，加入消泡剂乳化硅油，制得药物的缓释微胶囊。介孔硅材料具有规则孔道、高比表面积等特点，用KH550对MCM-41分子筛进行改性作为载体，以带负电荷的聚丙烯酸为功能分子，通过静电吸附作用制备了缓释体系。以层状水滑石为主体，以微胶囊化的毒死蜱为客体分子，以乙醇为溶剂，制备得到插层材料；以聚甲基丙烯酸甲酯为壁材，以聚乙烯醇为连续相，制得了毒死蜱微囊悬浮剂。
发明内容
本发明主要解决的技术问题是提供一种含丙环唑的杀菌型毒死蜱微囊悬浮剂及其制备工艺，依照该工艺制作的微囊悬浮剂低毒、杀菌性能好、缓释性能好，可生物降解。
本发明所要解决的技术问题采用以下的技术方案来实现：
毒死蜱5-8，聚碳酸亚丙酯27-38，聚乙烯醇16-23，聚乳酸8-15，明胶6-11，乳化硅油0.2-0.3，海藻酸钠5-9，有机膨润土3-7，MCM-41分子筛4-9，KH550 1-3，聚丙烯酸4-8，水滑石3-7，丙环唑3-6，液体石蜡4-10，乳化剂OP-10 2-4，丙二醇、二氯甲烷、乙醇、甲苯、蒸馏水适量。
一种含丙环唑的杀菌型毒死蜱微囊悬浮剂的制备方法，其特征在于，按以下步骤进行：
a. 将聚乳酸1:5-10溶于二氯甲烷，聚乙烯醇、明胶1:1:50-100溶于蒸馏水，两者混合高速分散乳化30-50s，加入乳化硅油，磁力搅拌2-3h，得A液；向海藻酸钠中1:20-30加入蒸馏水，搅拌溶解，1:10-15加入有机膨润土、乙醇，超声分散1-2h，得B液；将A、B液均匀混合待用；
b. 向MCM-41分子筛中1:20-30加入甲苯，搅拌下滴加KH550，在氮气保护下，加热回流、搅拌反应2-4h，冷却至室温后，1:30-40加入聚丙烯酸、蒸馏水，磁力搅拌2-3h，过滤，醇洗水洗3-5次，干燥；
c. 在氮气保护下，将水滑石1:20-30溶于乙醇中形成透明溶液，与a、b中所得物料混合，调pH为6-7，在60-80℃下反应4-8h，产物经过滤、水洗醇洗3-5次，在烘箱中于80-90℃干燥2-3h；
d. 将丙环唑和液体石蜡混合，加热至50-70℃搅拌溶解成油相，将乳化剂 OP-10 1:3-5:10-20与丙二醇、蒸馏水混合，升温至60-80℃搅拌溶解成水相，把油相加入水相中，搅拌均匀得水乳剂；
e. 将聚碳酸亚丙酯1:5-10溶于二氯甲烷中，加入毒死蜱，60-70℃振荡摇匀，与c、d中所得物料混合乳化分散5-10min，使之形成稳定的O/W型乳液，恒温水浴搅拌2-4h，即得到一种微囊悬浮剂。
本发明的反应机理如下：
（1）聚乳酸是一种高分子聚合物，具有优良的生物相容性、可降解性，无毒害；海藻酸钠具有无毒、低成本、可生物降解、生物相容性好的特点，有机膨润土与海藻酸钠共混改性，实现插层，提高疏水性及吸附效果，与生物可降解材料聚乳酸复合为壁材，加入消泡剂乳化硅油，制得药物的缓释微胶囊。
（2）介孔硅材料具有规则孔道、高比表面积等特点，用KH550对MCM-41分子筛进行改性作为载体，以带负电荷的聚丙烯酸为功能分子，通过静电吸附作用制备了缓释体系。
（3）以层状水滑石为主体，以微胶囊化的毒死蜱为客体分子，以乙醇为溶剂，制备得到插层材料；以聚甲基丙烯酸甲酯为壁材，以聚乙烯醇为连续相，制得了毒死蜱微囊悬浮剂。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例
一种含丙环唑的杀菌型毒死蜱微囊悬浮剂，由下述重量份(g)的原料制得：
毒死蜱8，聚碳酸亚丙酯38，聚乙烯醇16，聚乳酸15，明胶11，乳化硅油0.2，海藻酸钠9，有机膨润土7，MCM-41分子筛9，KH550 3，聚丙烯酸8，水滑石7，丙环唑6，液体石蜡10，乳化剂OP-10 4，丙二醇、二氯甲烷、乙醇、甲苯、蒸馏水适量。
一种含丙环唑的杀菌型毒死蜱微囊悬浮剂的制备方法，其特征在于，按以下步骤进行：
a. 将聚乳酸1:10溶于二氯甲烷，聚乙烯醇、明胶1:1:50溶于蒸馏水，两者混合高速分散乳化40s，加入乳化硅油，磁力搅拌2h，得A液；向海藻酸钠中1:20加入蒸馏水，搅拌溶解，1:15加入有机膨润土、乙醇，超声分散2h，得B液；将A、B液均匀混合待用；
b. 向MCM-41分子筛中1:20加入甲苯，搅拌下滴加KH550，在氮气保护下，加热回流、搅拌反应2h，冷却至室温后，1:30加入聚丙烯酸、蒸馏水，磁力搅拌3h，过滤，醇洗水洗3次，干燥；
c. 在氮气保护下，将水滑石1:25溶于乙醇中形成透明溶液，与a、b中所得物料混合，调pH为6-7，在70-80℃下反应4h，产物经过滤、水洗醇洗3次，在烘箱中于80-90℃干燥3h；
d. 将丙环唑和液体石蜡混合，加热至50-60℃搅拌溶解成油相，将乳化剂 OP-10 1:5:15与丙二醇、蒸馏水混合，升温至60-70℃搅拌溶解成水相，把油相加入水相中，搅拌均匀得水乳剂；
e. 将聚碳酸亚丙酯1:10溶于二氯甲烷中，加入毒死蜱，60-70℃振荡摇匀，与c、d中所得物料混合乳化分散10min，使之形成稳定的O/W型乳液，恒温水浴搅拌3h，即得到一种微囊悬浮剂。
上述实施例制备的一种含丙环唑的杀菌型毒死蜱微囊悬浮剂的性能检测结果如下所示：
对农田中的害虫杀灭效果好，10h害虫死亡率为100%；缓释效果好，自然条件下50d的累积释药率≥80%；持效性好，用药后100d的杀灭率≥98%。

Claims (2)

1.一种含丙环唑的杀菌型毒死蜱微囊悬浮剂，其特征在于，由下述重量份的原料制得：
毒死蜱5-8，聚碳酸亚丙酯27-38，聚乙烯醇16-23，聚乳酸8-15，明胶6-11，乳化硅油0.2-0.3，海藻酸钠5-9，有机膨润土3-7，MCM-41分子筛4-9，KH550 1-3，聚丙烯酸4-8，水滑石3-7，丙环唑3-6，液体石蜡4-10，乳化剂OP-10 2-4，丙二醇、二氯甲烷、乙醇、甲苯、蒸馏水适量。
2.根据权利要求1所述的一种含丙环唑的杀菌型毒死蜱微囊悬浮剂的制备方法，其特征在于，按以下步骤进行：
a. 将聚乳酸1:5-10溶于二氯甲烷，聚乙烯醇、明胶1:1:50-100溶于蒸馏水，两者混合高速分散乳化30-50s，加入乳化硅油，磁力搅拌2-3h，得A液；向海藻酸钠中1:20-30加入蒸馏水，搅拌溶解，1:10-15加入有机膨润土、乙醇，超声分散1-2h，得B液；将A、B液均匀混合待用；
b. 向MCM-41分子筛中1:20-30加入甲苯，搅拌下滴加KH550，在氮气保护下，加热回流、搅拌反应2-4h，冷却至室温后，1:30-40加入聚丙烯酸、蒸馏水，磁力搅拌2-3h，过滤，醇洗水洗3-5次，干燥；
c. 在氮气保护下，将水滑石1:20-30溶于乙醇中形成透明溶液，与a、b中所得物料混合，调pH为6-7，在60-80℃下反应4-8h，产物经过滤、水洗醇洗3-5次，在烘箱中于80-90℃干燥2-3h；
d. 将丙环唑和液体石蜡混合，加热至50-70℃搅拌溶解成油相，将乳化剂 OP-10 1:3-5:10-20与丙二醇、蒸馏水混合，升温至60-80℃搅拌溶解成水相，把油相加入水相中，搅拌均匀得水乳剂；
e. 将聚碳酸亚丙酯1:5-10溶于二氯甲烷中，加入毒死蜱，60-70℃振荡摇匀，与c、d中所得物料混合乳化分散5-10min，使之形成稳定的O/W型乳液，恒温水浴搅拌2-4h，即得到一种微囊悬浮剂。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109329277A (zh) * 2018-12-03 2019-02-15 黄美红 一种除草剂用吸附载体
CN109575144A (zh) * 2018-12-03 2019-04-05 黄美红 一种季铵-磺酸化微晶纤维素稳定剂及其在细胞元除草剂中的应用

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109329277A (zh) * 2018-12-03 2019-02-15 黄美红 一种除草剂用吸附载体
CN109575144A (zh) * 2018-12-03 2019-04-05 黄美红 一种季铵-磺酸化微晶纤维素稳定剂及其在细胞元除草剂中的应用
CN109329277B (zh) * 2018-12-03 2022-06-17 山东碧奥生物科技有限公司 一种除草剂用吸附载体

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