CN106804587A - 一种兼具防治果树腐烂病的温敏型缓释农药及其制备方法 - Google Patents
一种兼具防治果树腐烂病的温敏型缓释农药及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种兼具防治果树腐烂病的温敏型缓释农药,由以下重量份的原料组成:阿魏酸2‑7,淀粉10‑18,二甲基亚砜适量,对甲基苯磺酸1‑4,碳酸氢钠4‑13,无水乙醚适量,N‑哌啶丙烯酰胺15‑27,去离子水适量,十二烷基硫酸钠2‑5,农药活性成分21‑30,偶氮二异丁腈2‑6,四甲基乙二胺1‑2,花椒籽油4‑10,硫酸铜1‑3,硫酸亚铁1‑3。本发明以阿魏酸和淀粉为原料合成了阿魏酸淀粉酯,与N‑哌啶丙烯酰胺发生自由基聚合反应,制得温敏型水凝胶,利用其能随环境温度的变化发生可逆性的膨胀和收缩,从而实现对农药活性成分的持续稳定的释放,可达到长效、降低污染、经济的控制梨小食心虫的目的。
Description
技术领域
本发明属于农药生产技术领域,具体涉及一种兼具防治果树腐烂病的温敏型缓释农药及其制备方法。
背景技术
果树食心虫是钻蛀果实进行危害的蛾类幼虫的统称,常见有梨小食心虫、桃小食心虫、桃蛀螟、梨大食心虫等 10 余种类,是果树生产中一类常发性害虫。其中,梨小食心虫又名梨小蛀果蛾、东方果蠹蛾、桃折梢虫等,简称“梨小”,可危害仁果类和核果类多种果树,如梨、苹果、桃、李等果树的果实及嫩梢。在我国中部地区一年发生5代,以老熟幼虫主要在枝干粗皮颖内结茧越冬。翌年3月份开始化蛹,4月份成虫羽化,一般五六月份,第一、二代幼虫主要危害桃梢,7月份以后逐渐向梨上转移,7月下旬至9月主要危害梨果。其发生时间长,且发生与温度关系密切。
药物释放体系对于药物的作用至关重要,尤其是控制农药、杀虫剂释放的体系,由于农药、杀虫剂具有很强的毒性,如何能够降低其毒性,提高药物的利用率和杀虫效果,需要制备合适的药物载体,开发合适的药物释放体系。在需要药物释放时能够很快释放出来,产生功效,不需要释放时能够包覆于载体之内,长时间保存。
石萌、权静等人在其《N-乙烯基己内酰胺温敏含糖共聚物纳米纤维的制备及其载药释放研究》一文中选择阿魏酸衍生物前药为药物模型,发展了一种简单便捷的制备含有温敏性共聚单体NVCL的纳米载药纤维。温度响应性材料N-乙烯基己内酰胺,其均聚物的相转变温度范围在30-40℃,具有较强的配位能力和适宜的成膜性,良好的生物相容性。
发明内容
针对现有技术的不足,本发明提供一种兼具防治果树腐烂病的温敏型缓释农药及其制备方法。
一种兼具防治果树腐烂病的温敏型缓释农药,其特征在于,由以下重量份的原料组成:阿魏酸2-7份,淀粉10-18份,二甲基亚砜适量,对甲基苯磺酸1-4份,碳酸氢钠4-13份,无水乙醚适量,N- 哌啶丙烯酰胺15-27份,去离子水适量,十二烷基硫酸钠2-5份,农药活性成分21-30份,偶氮二异丁腈2-6份,四甲基乙二胺1-2份,花椒籽油4-10份,硫酸铜1-3份,硫酸亚铁1-3份。
具体步骤如下:
(1)阿魏酸淀粉酯的合成:
将阿魏酸和二甲基亚砜加入带有搅拌的三颈烧瓶中加热溶解,之后加入淀粉搅拌混合均匀,滴入对甲基苯磺酸的二甲基亚砜溶液,控温110-130℃,反应3-5小时,反应完成后冷却至室温,用15%的碳酸氢钠水溶液洗涤2-3次,有机相蒸馏、浓缩得到黏稠膏状物,经无水乙醚洗涤处理,得到阿魏酸淀粉酯;
(2)将N- 哌啶丙烯酰胺与步骤(1)制备的阿魏酸淀粉酯加入去离子水中,配成均匀溶液,转移至聚合管中,用油泵抽真空后通氮气5-13分钟,反复多次使反应瓶处于无氧状态,生成混合水溶液;
(3)配制活性成分分散液:
①、将硫酸铜、硫酸亚铁粉碎,过60-200目筛,备用;
②、将十二烷基硫酸钠溶解于去离子水中,然后在转速为1500-3000rpm的条件下,加入农药活性成分、花椒籽油及上述粉碎后的硫酸铜、硫酸亚铁混合均匀,得到农药活性成分分散液;
(4)向步骤(2)混合水溶液中缓慢加入上述活性成分分散液,搅拌分散均匀,加入偶氮二异丁腈作为引发剂,继续通氮气5-10分钟,之后加入四甲基乙二胺,将反应体系置于50-70℃条件下,在氮气保护下交联聚合反应4-7小时,然后冷却,过滤,用去离子水冲洗两次固相物,过滤沥干后,真空干燥至恒重,即得。
其中,所述的农药活性成分为高效氯氰菊酯与甲氨基阿维菌素苯甲酸盐的混合物,二者的重量比为10:1-1:3,优选为2:1。
与现有技术相比,本发明具有以下优点:
(1)本发明以 N- 哌啶丙烯酰胺为单体材料,与阿魏酸淀粉酯发生自由基聚合反应,制得温敏型水凝胶包覆农药活性成分,利用水凝胶的温度敏感性,能随环境温度的变化发生可逆性的膨胀和收缩,从而实现对农药活性成分的持续稳定的释放,可达到长效、降低污染、经济的控制梨小食心虫的目的。
(2)本发明以阿魏酸和淀粉为原料,在对甲基苯磺酸的催化作用下合成了阿魏酸淀粉酯,既含有阿魏酸基,又具有亲水性的低聚糖基团,兼具了阿魏酸和低聚糖的双重活性,具有调节植物生长发育和抑菌作用,其抗氧化性能对果蔬具有一定的保鲜作用,另外本发明凝胶载体生物相容性高,可完全生物降解,对人畜安全无毒,不污染环境,无残留。
(3)本发明中添加的花椒籽油具有抗菌、驱虫、防腐及透皮吸收等多方面作用,同时具有诱导植物抗病性和刺激植物生长的双重作用,还具有促进树体伤口愈合的作用,与能促进伤口愈合的硫酸铜、硫酸亚铁复配作用可促使伤口愈合,促进新皮生长,对果树腐烂病具有显著的治疗效果。
具体实施方式
一种兼具防治果树腐烂病的温敏型缓释农药,其特征在于,由以下重量份的原料组成:阿魏酸5份,淀粉15份,二甲基亚砜适量,对甲基苯磺酸2份,碳酸氢钠9份,无水乙醚适量,N- 哌啶丙烯酰胺25份,去离子水适量,十二烷基硫酸钠2-5份,农药活性成分23份,偶氮二异丁腈4份,四甲基乙二胺2份,花椒籽油8份,硫酸铜2份,硫酸亚铁2份。
具体步骤如下:
(1)阿魏酸淀粉酯的合成:
将阿魏酸和二甲基亚砜加入带有搅拌的三颈烧瓶中加热溶解,之后加入淀粉搅拌混合均匀,滴入对甲基苯磺酸的二甲基亚砜溶液,控温120℃,反应4小时,反应完成后冷却至室温,用15%的碳酸氢钠水溶液洗涤3次,有机相蒸馏、浓缩得到黏稠膏状物,经无水乙醚洗涤处理,得到阿魏酸淀粉酯;
(2)将N- 哌啶丙烯酰胺与步骤(1)制备的阿魏酸淀粉酯加入去离子水中,配成均匀溶液,转移至聚合管中,用油泵抽真空后通氮气10分钟,反复多次使反应瓶处于无氧状态,生成混合水溶液;
(3)配制活性成分分散液:
①、将硫酸铜、硫酸亚铁粉碎,过100目筛,备用;
②、将十二烷基硫酸钠溶解于去离子水中,然后在转速为2000rpm的条件下,加入农药活性成分、花椒籽油及上述粉碎后的硫酸铜、硫酸亚铁混合均匀,得到农药活性成分分散液;
(4)向步骤(2)混合水溶液中缓慢加入上述活性成分分散液,搅拌分散均匀,加入偶氮二异丁腈作为引发剂,继续通氮气8分钟,之后加入四甲基乙二胺,将反应体系置于60℃条件下,在氮气保护下交联聚合反应6小时,然后冷却,过滤,用去离子水冲洗两次固相物,过滤沥干后,真空干燥至恒重,即得。
其中,所述的农药活性成分为高效氯氰菊酯与甲氨基阿维菌素苯甲酸盐的混合物,二者的重量比为10:1-1:3,优选为2:1。
Claims (3)
1.一种兼具防治果树腐烂病的温敏型缓释农药,其特征在于,由以下重量份的原料组成:阿魏酸2-7份,淀粉10-18份,二甲基亚砜适量,对甲基苯磺酸1-4份,碳酸氢钠4-13份,无水乙醚适量,N- 哌啶丙烯酰胺15-27份,去离子水适量,十二烷基硫酸钠2-5份,农药活性成分21-30份,偶氮二异丁腈2-6份,四甲基乙二胺1-2份,花椒籽油4-10份,硫酸铜1-3份,硫酸亚铁1-3份。
2.根据权利要求书1所述的一种兼具防治果树腐烂病的温敏型缓释农药的制备方法,其特征在于,具体步骤如下:
(1)阿魏酸淀粉酯的合成:
将阿魏酸和二甲基亚砜加入带有搅拌的三颈烧瓶中加热溶解,之后加入淀粉搅拌混合均匀,滴入对甲基苯磺酸的二甲基亚砜溶液,控温110-130℃,反应3-5小时,反应完成后冷却至室温,用15%的碳酸氢钠水溶液洗涤2-3次,有机相蒸馏、浓缩得到黏稠膏状物,经无水乙醚洗涤处理,得到阿魏酸淀粉酯;
(2)将N- 哌啶丙烯酰胺与步骤(1)制备的阿魏酸淀粉酯加入去离子水中,配成均匀溶液,转移至聚合管中,用油泵抽真空后通氮气5-13分钟,反复多次使反应瓶处于无氧状态,生成混合水溶液;
(3)配制活性成分分散液:
①、将硫酸铜、硫酸亚铁粉碎,过60-200目筛,备用;
②、将十二烷基硫酸钠溶解于去离子水中,然后在转速为1500-3000rpm的条件下,加入农药活性成分、花椒籽油及上述粉碎后的硫酸铜、硫酸亚铁混合均匀,得到农药活性成分分散液;
(4)向步骤(2)混合水溶液中缓慢加入上述活性成分分散液,搅拌分散均匀,加入偶氮二异丁腈作为引发剂,继续通氮气5-10分钟,之后加入四甲基乙二胺,将反应体系置于50-70℃条件下,在氮气保护下交联聚合反应4-7小时,然后冷却,过滤,用去离子水冲洗两次固相物,过滤沥干后,真空干燥至恒重,即得。
3.根据权利要求书1、2所述的一种兼具防治果树腐烂病的温敏型缓释农药的制备方法,其特征在于,所述的农药活性成分为高效氯氰菊酯与甲氨基阿维菌素苯甲酸盐的混合物,二者的重量比为10:1-1:3,优选为2:1。
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