CN106818731A - 一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊及其制备方法 - Google Patents

一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊及其制备方法 Download PDF

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CN106818731A
CN106818731A CN201611153586.0A CN201611153586A CN106818731A CN 106818731 A CN106818731 A CN 106818731A CN 201611153586 A CN201611153586 A CN 201611153586A CN 106818731 A CN106818731 A CN 106818731A
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Abstract

本发明公开了一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊及其制备方法，其特征在于，是由以下重量份的原料制成：吡唑醚菌酯2‑5，毒死蜱原药15‑25，膨润土30‑50，二氧化硅3‑5，艾蒿精油3‑8，尿素30‑40，十二烷基三甲基氯化铵1‑2，甲醛60‑70，盐酸适量，甲醇10‑20，氢氧化钠适量，苯乙烯‑马来酸酐共聚钠盐2‑5，聚丙烯酸钠2‑3，蒸馏水250‑800；本发明将有机膨润土作为载体引入微胶囊中，不仅可以达到延缓药物释放的目的，同时增加了微胶囊悬浮剂的稳定性，延长农药的使用寿命；配合添加的吡唑醚菌酯具有杀菌的功效。

Description

一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊及其制 备方法
技术领域
本发明涉及一种农药制剂，具体涉及一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊及其制备方法。
背景技术
微囊悬浮剂可谓是当前农药新剂型中技术含量最高的一种。它是以高分子材料作为囊壁，通过化学、物理或物理化学的方法，将作为囊心的农药活性物质包裹起来，形成一种具有半透膜的微型胶囊。并将它们以一定的浓度稳定地分散悬浮在作为连续相的水中。微胶囊化的农药制剂与常规剂型农药相比具有如下一些优点：1.引入了控制释放技术，延长了农药的持效期，减少施药数量和频率，提高农药的利用率，节约农药用量。2.提高农药的稳定性（尤其对生物源农药），避免因环境因素如光照、空气、雨水、土壤、微生物及其它化学物质造成有效成分的分解、氧化、流失等。3.将油相与水相分离，对某些水不稳定而难以加工成微乳剂及水乳剂的农药（如部分有机磷农药），则适宜加工为微胶囊，扩大农药的使用范围，提高与其它农药的复配能力。4.抑制农药的挥发性，掩蔽不愉快的气味，降低农药对人、畜、鱼及其它动物的接触毒性、吸入毒性和对作物的药害，减轻了农药对环境的压力。
赵德在《脲醛树脂制备毒死蜱微胶囊及性能表征》中，以脲醛树脂为壁材制备了毒死蜱微胶囊，但是还存在着分散性、稳定性不够理想，缓释性欠佳，环保、健康、持续发展理念欠缺。
发明内容
基于以上的思考，本发明旨在提供一种稳定的、缓释效果好、杀虫效果好，同时符合环保、可持续发展理念。
本发明所要解决的技术问题采取以下的技术方案实现：
一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊，其特征在于，是由以下重量份的原料制成：
吡唑醚菌酯2-5，毒死蜱原药15-25，膨润土30-50，二氧化硅3-5，艾蒿精油3-8，尿素30-40，十二烷基三甲基氯化铵1-2，甲醛60-70，盐酸适量，甲醇10-20，氢氧化钠适量，苯乙烯-马来酸酐共聚钠盐2-5，聚丙烯酸钠2-3，蒸馏水250-800；
所述甲醛的质量分数为30～40％，盐酸的质量分数为20-30％，氢氧化钠质量分数为20-40。
根据权利要求1所述的一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊的制备方法，其特征在于，是由以下步骤制成：
a. 将膨润土、二氧化硅、充分分散到100-200份蒸馏水中，制成膨润土悬浮液,加入十二烷基三甲基氯化铵，在温度为60-80℃的恒温水浴振荡器上以120-150r/min的速度振荡3-5h，之后离心、过滤、烘干，得有机膨润土、二氧化硅混合物；
b. 将步骤a所得混合物重新分散在50-100份蒸馏水中制成悬浮液，将毒死蜱原药、吡唑醚菌酯、艾蒿精油溶解在甲醇中，加入到上述悬浮液中，在20-40℃的恒温水浴振荡器上以130-160r/min的速度振荡3-5h，真空抽滤后用蒸馏水洗涤2-3次，烘干，即得载药有机膨润土、二氧化硅混合物；
c. 将尿素、甲醛和100-150份蒸馏水混合，用氢氧化钠调节体系 pH值为8-9，升温至65～70℃，搅拌反应 40-80min，得脲醛树脂预聚物水溶液；
d. 向步骤c所得预聚物水溶液中加入步骤b所得混合物，再加入苯乙烯-马来酸酐共聚钠盐和聚丙烯酸钠作为乳化剂和分散剂，1300-1600 r/min的转速搅拌10-30min后，降低转速至700-900 r/min，40-80min 内分批次加入盐酸调节体系 pH 值为 1.5-2.5；转速逐步降至 100-300 r/min，逐步升温至 50-80℃固化囊壁，反应30-60min后，加入氢氧化钠调节体系 pH 值为中性，即得毒死蜱微囊悬浮剂。
本发明的有益效果是：采用原位聚合法，利用脲醛树脂对毒死蜱进行微胶囊化，可以在很大程度上克服毒死蜱通常使用的乳油剂型所带来的有机溶剂污染环境、浪费资源的问题，同时延长了持效期，提高了农药的有效利用率、避免了农药的分解流失，减轻毒性和药害；用十二烷基三甲基氯化铵对膨润土进行改性，降低膨润土的亲水性，从而提高了其对疏水性毒死蜱分子和艾蒿精油的吸附量；将有机膨润土作为载体引入微胶囊中，不仅可以达到延缓药物释放的目的，同时增加了微胶囊悬浮剂的稳定性，延长农药的使用寿命；另一方面，艾蒿精油可以在毒死蜱中发挥重要增效作用，减少农药使用量，达到环保、可持续发展的目的；配合添加的吡唑醚菌酯具有杀菌的功效。
具体实施方式
下面结合实施例对本发明的具体实施方式作进一步描述。
实施例
一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊，其特征在于，是由以下重量份的原料制成：
吡唑醚菌酯5，毒死蜱原药25，膨润土50，二氧化硅5，艾蒿精油8，尿素40，十二烷基三甲基氯化铵2，甲醛70，盐酸适量，甲醇20，氢氧化钠适量，苯乙烯-马来酸酐共聚钠盐5，聚丙烯酸钠3，蒸馏水800；
所述甲醛的质量分数为30～40％，盐酸的质量分数为20-30％，氢氧化钠质量分数为20-40。
根据权利要求1所述的一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊的制备方法，其特征在于，是由以下步骤制成：
a. 将膨润土、二氧化硅、充分分散到100-200份蒸馏水中，制成膨润土悬浮液,加入十二烷基三甲基氯化铵，在温度为60-80℃的恒温水浴振荡器上以120-150r/min的速度振荡3-5h，之后离心、过滤、烘干，得有机膨润土、二氧化硅混合物；
b. 将步骤a所得混合物重新分散在50-100份蒸馏水中制成悬浮液，将毒死蜱原药、吡唑醚菌酯、艾蒿精油溶解在甲醇中，加入到上述悬浮液中，在20-40℃的恒温水浴振荡器上以130-160r/min的速度振荡3-5h，真空抽滤后用蒸馏水洗涤2-3次，烘干，即得载药有机膨润土、二氧化硅混合物；
c. 将尿素、甲醛和100-150份蒸馏水混合，用氢氧化钠调节体系 pH值为8-9，升温至65～70℃，搅拌反应 40-80min，得脲醛树脂预聚物水溶液；
d. 向步骤c所得预聚物水溶液中加入步骤b所得混合物，再加入苯乙烯-马来酸酐共聚钠盐和聚丙烯酸钠作为乳化剂和分散剂，1300-1600 r/min的转速搅拌10-30min后，降低转速至700-900 r/min，40-80min 内分批次加入盐酸调节体系 pH 值为 1.5-2.5；转速逐步降至 100-300 r/min，逐步升温至 50-80℃固化囊壁，反应30-60min后，加入氢氧化钠调节体系 pH 值为中性，即得毒死蜱微囊悬浮剂。
本发明的性能测试数据为：微胶囊前 5d 释放量≤ 37.32％。

Claims (2)

1.一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊，其特征在于，是由以下重量份的原料制成：
吡唑醚菌酯2-5，毒死蜱原药15-25，膨润土30-50，二氧化硅3-5，艾蒿精油3-8，尿素30-40，十二烷基三甲基氯化铵1-2，甲醛60-70，盐酸适量，甲醇10-20，氢氧化钠适量，苯乙烯-马来酸酐共聚钠盐2-5，聚丙烯酸钠2-3，蒸馏水250-800；
所述甲醛的质量分数为30～40％，盐酸的质量分数为20-30％，氢氧化钠质量分数为20-40。
2.根据权利要求1所述的一种艾蒿精油增效的吡唑醚菌酯、毒死蜱复配微胶囊的制备方法，其特征在于，是由以下步骤制成：
a. 将膨润土、二氧化硅、充分分散到100-200份蒸馏水中，制成膨润土悬浮液,加入十二烷基三甲基氯化铵，在温度为60-80℃的恒温水浴振荡器上以120-150r/min的速度振荡3-5h，之后离心、过滤、烘干，得有机膨润土、二氧化硅混合物；
b. 将步骤a所得混合物重新分散在50-100份蒸馏水中制成悬浮液，将毒死蜱原药、吡唑醚菌酯、艾蒿精油溶解在甲醇中，加入到上述悬浮液中，在20-40℃的恒温水浴振荡器上以130-160r/min的速度振荡3-5h，真空抽滤后用蒸馏水洗涤2-3次，烘干，即得载药有机膨润土、二氧化硅混合物；
c. 将尿素、甲醛和100-150份蒸馏水混合，用氢氧化钠调节体系 pH值为8-9，升温至65～70℃，搅拌反应 40-80min，得脲醛树脂预聚物水溶液；
d. 向步骤c所得预聚物水溶液中加入步骤b所得混合物，再加入苯乙烯-马来酸酐共聚钠盐和聚丙烯酸钠作为乳化剂和分散剂，1300-1600 r/min的转速搅拌10-30min后，降低转速至700-900 r/min，40-80min 内分批次加入盐酸调节体系 pH 值为 1.5-2.5；转速逐步降至 100-300 r/min，逐步升温至 50-80℃固化囊壁，反应30-60min后，加入氢氧化钠调节体系 pH 值为中性，即得毒死蜱微囊悬浮剂。
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CN102362590A (zh) * 2011-11-11 2012-02-29 中国农业科学院植物保护研究所 一种微囊化农药制剂
CN105284871A (zh) * 2014-07-18 2016-02-03 青岛瀚生生物科技股份有限公司 吡唑醚菌酯与毒死蜱复配的微胶囊悬浮剂及其制备方法

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