CN110720454A - 一种抗光解纳米农药及其制备方法 - Google Patents

一种抗光解纳米农药及其制备方法 Download PDF

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CN110720454A
CN110720454A CN201911059543.XA CN201911059543A CN110720454A CN 110720454 A CN110720454 A CN 110720454A CN 201911059543 A CN201911059543 A CN 201911059543A CN 110720454 A CN110720454 A CN 110720454A
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photolysis
nano
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肖清波
张晞
孟丽
奚永兰
叶小梅
朱艳
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Jiangsu Academy of Agricultural Sciences
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Abstract

本发明属于纳米农药制剂技术领域，具体涉及一种抗光解纳米农药及其制备方法。本发明以多孔性纳米沸石、纳米凹凸棒土、纳米二氧化硅等为载体，吸附一定量的聚苯乙烯、聚丙烯腈等高分子材料后，在惰性气氛下碳化处理、自然冷却、重新分散后，负载对太阳光敏感的农药分子，如咯菌腈、咪鲜胺等，即得到具有抗光降解效果的纳米农药。本发明制备的纳米农药具有有效屏蔽可见光、紫外光等能力，同时还具有良好的分散性与农药分子负载能力，是一种低成本、环境友好的理想抗光解纳米农药。

Description

一种抗光解纳米农药及其制备方法
技术领域
本发明涉及纳米农药领域，具体涉及一种具有抗光解效果的纳米农药及其制备方法。
背景技术
对农药进行纳米化加工与改性具有增加对生物组织穿透性、赋予药物分子靶向性传输等优点。纳米技术与农药领域的结合有助于迅速创制传统方法难以获得的高效农药新剂型。当前，通过纳米载体包裹在太阳光照下易光解的农药分子，提高易光解农药的稳定性是一个重要的研究方向。通过构建具有紫外线阻隔功能的纳米载体，将农药活性成分吸附或包裹在载体中，能有效降低到达药物分子的太阳光强度，从而减少农药分子的光降解，提高药效。然而，
当前大部分抗光解纳米载体由吸收太阳光的高分子材料组成，具有价格昂贵、材料种类少、不易修饰、易污染环境等缺点。
为了克服上述高分子材料的缺陷，选择环境友好、价格低廉的无机纳米载体材料，通过简易改性方法使其具备吸收太阳光功能，是一个重要的研究方向。
因此，有必要提供一种抗光解纳米农药及其制备方法，该制备方法简单、易操作，且制备的纳米农药组合物具有较好的抗光解性能，并减少农药用量。
发明内容
有鉴于此，本发明提供一种抗光解纳米农药及其制备方法，能够解决现有的抗光解纳米载体成本高昂、高分子残留易污染环境的问题。本发明根据多孔性无机纳米材料的负载特性，吸附高分子材料，经过高温降解形成具有光屏蔽功能的炭材料，进一步负载农药，获得一类具有抗光解功能的纳米农药。
为此目的，本发明采用如下技术方案：
一种抗光解纳米农药，所述农药由抗光解纳米载体和易光解性农药分子组成。
抗光解纳米载体由多孔无机纳米材料与高分子材料按质量比100:1-100:10混合。
所述多孔无机纳米材料为纳米沸石、纳米凹凸棒土、纳米二氧化硅中的一种或几种。
所述高分子材料为十六烷基三甲基氯化铵、聚苯乙烯、聚丙烯腈、酚醛树脂、植物油中的一种或几种。
所述易光解农药分子包括阿维菌素、咯菌腈、咪鲜胺、敌克松、辛硫磷、鱼藤酮、氟乐灵中的一种或几种。
本发明的另一目的是提供上述抗光解纳米农药的制备方法，包括以下步骤：
（1）按质量比称取多孔无机纳米材料、高分子材料、高分子材料的溶剂，充分搅拌后离心得到混合物A；
（2）将混合物A在烘箱中干燥去除溶剂分子后，在惰性气氛下400-800 oC高温碳化，自然冷却后超声或研磨分散，得到抗光解纳米载体；
（3）按质量比称取抗光解纳米载体、易光解农药、农药的溶剂，充分搅拌后离心得到混合物B；
（4）将混合物B在烘箱中干燥去除溶剂分子后，得到抗光解纳米农药。
所述高分子材料的溶剂为乙醇，所述农药的溶剂为丙酮。
本发明的制备方法简单易行，解决了抗光解纳米农药制备方法复杂、高分子残留等问题，通过本发明方法制得的纳米农药通过室内毒力测定，显示出良好的抗光解效果。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种抗光解纳米农药，包括易光解农药咪鲜胺，中空介孔SiO2、碳化植物油，制备方法包括以下步骤，
1. 将100mg粒径为30nm的中空介孔SiO2与1mL废弃植物油、1mL乙醇充分搅拌混合，离心干燥，得到混合物A。
2.将混合物A在氮气气氛下500 oC碳化1小时，自然冷却后研磨分散，得到抗光解纳米载体。
3.将50mg抗光解纳米载体、180mg咪鲜胺加入到5mL丙酮溶液中，充分搅拌后离心得到混合物B。
4.将混合物B常温下避光真空干燥除丙酮分子，得到抗光解纳米农药。
5.纳米农药光照射分解试验：称取20mg抗光解纳米农药与咪鲜胺原药，分别置于氙灯(300W)下照射8小时，然后取样通过液相色谱分析咪鲜胺的降解率，抗光解纳米农药的降解率为5%，而咪鲜胺原药的降解率达到72%。
实施例2
一种抗光解纳米农药，包括易光解农药咯菌腈，中空介孔SiO2、碳化植物油，制备方法包括以下步骤，
1.将100mg粒径为30nm的中空介孔SiO2与1mL废弃植物油、1mL乙醇充分搅拌混合，离心干燥，得到混合物A。
2.将混合物A在氮气气氛下500 oC碳化1小时，自然冷却后研磨分散，得到抗光解纳米载体。
3.将50mg抗光解纳米载体、100mg咯菌腈加入到5mL丙酮溶液中，充分搅拌后离心得到混合物B。
4.将混合物B常温下避光真空干燥除丙酮分子，得到抗光解纳米农药。
5. 纳米农药光照射分解试验：称取20mg抗光解纳米农药与咯菌腈原药，分别置于氙灯(300W)下照射8小时，然后取样通过液相色谱分析咪鲜胺的降解率，抗光解纳米农药的降解率为7%，而咪鲜胺原药的降解率达到67%。
实施例3
一种抗光解纳米农药，包括易光解农药阿维菌素，纳米凹凸棒土、碳化植物油，制备方法包括以下步骤，
1.将50mg商业纳米凹凸棒土与1mL废弃植物油、1mL乙醇充分搅拌混合，离心干燥，得到混合物A。
2.将混合物A在氮气气氛下500 oC碳化1小时，自然冷却后研磨分散，得到抗光解纳米载体。
3.将50mg抗光解纳米载体、100mg阿维菌素加入到5mL丙酮溶液中，充分搅拌后离心得到混合物B。
4.将混合物B常温下避光真空干燥除丙酮分子，得到抗光解纳米农药。
5.纳米农药光照射分解试验：称取20mg抗光解纳米农药与阿维菌素原药，分别置于氙灯(300W)下照射8小时，然后取样通过液相色谱分析咪鲜胺的降解率，抗光解纳米农药的降解率为12%，而阿维菌素原药的降解率达到87%。
实施例4
一种抗光解纳米农药，包括易光解农药敌克松，中空介孔SiO2、碳化树脂，制备方法包括以下步骤，
1.将100mg粒径为30nm的中空介孔SiO2与1mL聚苯乙烯、1mL乙醇充分搅拌混合，离心干燥，得到混合物A。
2.将混合物A在氮气气氛下800 oC碳化1小时，自然冷却后研磨分散，得到抗光解纳米载体。
3. 将50mg抗光解纳米载体、100mg敌克松加入到5mL丙酮溶液中，充分搅拌后离心得到混合物B。
4.将混合物B常温下避光真空干燥除丙酮分子，得到抗光解纳米农药。
5.纳米农药光照射分解试验：称取20mg抗光解纳米农药与敌克松原药，分别置于氙灯(300W)下照射8小时，然后取样通过液相色谱分析咪鲜胺的降解率，抗光解纳米农药的降解率为4%，而敌克松原药的降解率达到74%。
实施例5
一种抗光解纳米农药，包括易光解农药辛硫磷，纳米凹凸棒土、碳化树脂，制备方法包括以下步骤，
1.将50mg商业纳米凹凸棒土与1mL十六烷基三甲基氯化铵、1mL乙醇充分搅拌混合，离心干燥，得到混合物A。
2.将混合物A在氮气气氛下800 oC碳化1小时，自然冷却后研磨分散，得到抗光解纳米载体。
3.将50mg抗光解纳米载体、100mg辛硫磷加入到5mL丙酮溶液中，充分搅拌后离心得到混合物B。
4.将混合物B常温下避光真空干燥除丙酮分子，得到抗光解纳米农药。
5.纳米农药光照射分解试验：称取20mg抗光解纳米农药与辛硫磷原药，分别置于氙灯(300W)下照射8小时，然后取样通过液相色谱分析咪鲜胺的降解率，抗光解纳米农药的降解率为8%，而敌克松原药的降解率达到59%。
实施例6
一种抗光解纳米农药，包括易光解农药氟乐灵，纳米沸石、碳化树脂，制备方法包括以下步骤，
1.将100mg纳米沸石与10mL酚醛树脂、1mL乙醇充分搅拌混合，离心干燥，得到混合物A。
2.将混合物A在氮气气氛下800 oC碳化1小时，自然冷却后研磨分散，得到抗光解纳米载体。
3.将50mg抗光解纳米载体、100mg氟乐灵加入到5mL丙酮溶液中，充分搅拌后离心得到混合物B。
4.将混合物B常温下避光真空干燥除丙酮分子，得到抗光解纳米农药。
5.纳米农药光照射分解试验：称取20mg抗光解纳米农药与氟乐灵原药，分别置于氙灯(300W)下照射8小时，然后取样通过液相色谱分析咪鲜胺的降解率，抗光解纳米农药的降解率为10%，而氟乐灵原药的降解率达到74%。
以上所述，仅为本发明的具体实施方式，本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求所界定的保护范围为准。

Claims (7)

1.一种抗光解纳米农药，其特征在于，所述农药由抗光解纳米载体和易光解性农药分子组成。
2.根据权利要求1所述的抗光解纳米农药，其特征在于，抗光解纳米载体由多孔无机纳米材料与高分子材料按质量比100:1-100:10混合。
3.根据权利要求1所述的抗光解纳米农药，其特征在于，农药分子重量占纳米农药总质量的5%-50%。
4.根据权利要求2所述的抗光解纳米农药，其特征在于，所述多孔无机纳米材料为纳米沸石、纳米凹凸棒土、纳米二氧化硅中的一种或几种。
5.根据权利要求2所述的抗光解纳米农药，其特征在于，所述高分子材料为十六烷基三甲基氯化铵、聚苯乙烯、聚丙烯腈、酚醛树脂、植物油中的一种或几种。
6.根据权利要求1所述的抗光解纳米农药，所述易光解农药分子包括阿维菌素、咯菌腈、咪鲜胺、敌克松、辛硫磷、鱼藤酮、氟乐灵中的一种或几种。
7.权利要求1-6所述的抗光解纳米农药的制备方法，其特征在于，包括以下步骤：
（1）按质量比称取多孔无机纳米材料、高分子材料、高分子材料的溶剂，充分搅拌后离心得到混合物A；
（2）将混合物A在烘箱中干燥去除溶剂分子后，在惰性气氛下400-800 oC高温碳化，自然冷却后超声或研磨分散，得到抗光解纳米载体；
（3）按质量比称取抗光解纳米载体、易光解农药、农药的溶剂，充分搅拌后离心得到混合物B；
（4）将混合物B在烘箱中干燥去除溶剂分子后，得到抗光解纳米农药。
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