CN115428790A - 一种凹土与表面活性剂司盘80协同稳定的农药微乳剂及其制备方法 - Google Patents
一种凹土与表面活性剂司盘80协同稳定的农药微乳剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及天然矿物资源利用技术领域,公开了一种凹土与表面活性剂司盘80协同稳定的农药微乳剂及其制备方法,该微乳剂由油相、水相及司盘80组成,所述油相为高氯氰菊酯‑甲苯有机相,所述水相为凹土‑水分散液,其中,所述高氯氰菊酯在所述微乳剂中的质量浓度为3‑17%,所述凹土在所述微乳剂中的质量浓度为1‑2%,所述司盘80在所述微乳剂中的摩尔浓度为10‑30mM。该微乳剂是一种由纤维状的黏土颗粒‑凹土部分代替了有机表面活性剂的新型乳液体系,以凹土部分取代液体有机表面活性剂,乳液体系粘度提高,乳液液滴在植物叶面的粘着力增加,更耐雨水冲刷,提高吸收效率,在降低了有机表面活性剂用量的同时达到了更好的应用效果,从而降低生产成本,绿色环保。
Description
技术领域
本发明涉及天然矿物资源利用技术领域,特别涉及一种凹土与表面活性剂司盘80协同稳定的农药微乳剂及其制备方法。
背景技术
微乳剂(ME)是一种由两种类似于乳液的液体组成的分散体系,它通常由三种不同的物质(通常是水[W]和油[O]和表面活性剂)组成,并且在某些情况下它可能含有助剂,这取决于其组分和组成。微乳剂所形成的微乳液分散体系,胶束直径小至约100 nm或更小,热力学稳定,易于形成。这种小液滴尺寸和整个系统的表面张力降低可以产生更高的农药效率,并且可以减少任何聚结倾向。由于表面活性剂浓度高,微乳液体系可有效降低表面张力,改善液滴与目标之间的相互作用,使液滴在到达植物叶面后不会反弹,使其在植物表面更粘稠附着,润湿和扩散大大提高了液体的吸收效率。此外,许多微乳液农药液滴在蒸发和浓缩过程中形成高粘度的液晶相,可以将农药牢固地粘附在植物表面,不易被雨水冲走。
尽管与乳油相比,微乳剂已大大降低了有机溶剂的用量,但欲制备稳定的微乳剂,目前仍需使用一定量的价格不菲的表面活性剂,成本较高,且传统的液体表面活性剂大多为有机表面活性剂,与目前绿色环保的理念尚有一定的距离。
发明内容
发明目的:针对现有技术中存在的问题,本发明提供一种凹土与表面活性剂司盘80协同稳定的农药微乳剂及其制备方法,以凹凸棒石粘土与表面活性剂协同作用的方式代替一贯的单一表面活性剂,用以配制高氯氰菊酯微乳剂配方,达到降低成本、绿色环保的目的。
技术方案:本发明提供了一种凹土与表面活性剂司盘80协同稳定的油包水型(W/O)农药微乳剂,由油相、水相及司盘80组成,所述油相为高氯氰菊酯-甲苯有机相,所述水相为凹土-水分散液;其中,所述高氯氰菊酯在所述微乳剂中的质量浓度为3-17%,所述凹土在所述微乳剂中的质量浓度为1-2%,所述司盘80在所述微乳剂中的摩尔浓度为10-30mM。
优选地,所述油相与水相的体积比为1:1;
优选地,所述凹土为蒙脱石型凹土,其中的凹凸棒石与蒙脱石的总质量含量>85%,且凹凸棒石的质量含量≮30%、粒度<13μm。
本发明还提供了一种凹土与表面活性剂司盘80协同稳定的油包水型(W/O)农药微乳剂的制备方法,包括以下步骤:
S1:将凹土过325目筛后,加入到去离子水中,超声形成凹土-水分散液,即为水相;同时,将高氯氰菊酯溶于甲苯中形成油相;
S2:将所述油相与所述水相混合后加入司盘80,打浆得所述农药微乳剂。
有益效果:本发明中凹土与表面活性剂司盘80协同稳定的农药微乳剂是一种由纤维状的黏土颗粒——凹土部分代替了传统的有机表面活性剂的新型乳液体系。由于黏土是天然的矿物,环保,大规模应用性价比更高;以凹土部分取代液体有机表面活性剂,使整个乳液体系的粘度大大提高,乳液液滴在植物叶面的粘着力大大增加,使得药效时间更长,更耐雨水冲刷,吸收效率得到大幅度提高,液体有机表面活性剂的用量得到大幅度降低,节约成本的同时进一步达到绿色环保的目的。本制备工艺简单易行,充分发挥无机黏土的分散稳定效能,以凹土部分代替有机表面活性剂作为乳化剂,在大大降低了有机表面活性剂用量的同时达到了更好的应用效果,从而大大降低了生产成本,拓展了凹土的应用领域,达到绿色环保的目的。
具体实施方式
下面结合具体实施方式对本发明进行详细的介绍。
以下各实施方式均选用杂质主要为蒙脱石的凹土,过325目筛,其中凹凸棒石与蒙脱石的总质量含量>85%,且凹凸棒石的质量含量≮30%、粒度<13μm。
实施例1:
称取0.15 g凹土分散于5.0mL去离子水中,超声5分钟,形成水相;同时称取2.0g的高氯氰菊酯,溶于5.0mL甲苯中形成油相,将水相与油相以等体积相混合,加入0.043g司盘80,并在8000rpm的转速下打浆5分钟,即得微乳剂。所得微乳剂中凹土占微乳剂质量浓度为1.2%,司盘80在乳液中的摩尔浓度为10 mM,高氯氰菊酯占微乳剂质量浓度为17%。
所制得的微乳液(W/O)液滴直径均小于100nm,将所制得的微乳液分别在0℃和54℃下储存7天后,微乳液的外观保持均匀,没有任何沉淀或相分离,并且没有析出水相和油相,表明微乳液的稳定性没有显著变化。
实施例2:
称取0.15 g凹土分散于7.0mL去离子水中,超声5分钟,形成水相;同时称取0.5g的高氯氰菊酯,溶于7.0mL甲苯中形成油相,将水相与油相以等体积相混合,加入0.060g司盘80,并在8000rpm的转速下打浆5分钟,即得微乳剂。所得微乳剂中凹土占微乳剂质量浓度为1.0%,司盘80在乳液中的摩尔浓度为10 mM,高氯氰菊酯占微乳剂质量浓度为3%。
所制得的微乳液(W/O)液滴直径均小于100nm,将所制得的微乳液分别在0℃和54℃下储存7天后,微乳液的外观保持均匀,没有任何沉淀或相分离,并且没有析出水相和油相,表明微乳液的稳定性没有显著变化。
实施例3:
称取0.20 g凹土分散于5.0mL去离子水中,超声5分钟,形成水相;同时称取1.0g的高氯氰菊酯,溶于5.0mL甲苯中形成油相,将水相与油相以等体积相混合,加入0.129g司盘80,并在8000rpm的转速下打浆5分钟,即得微乳剂。所得微乳剂中凹土占微乳剂质量浓度为1.8%,司盘80在乳液中的摩尔浓度为30 mM,高氯氰菊酯占微乳剂质量浓度为9%。
所制得的微乳液(W/O)液滴直径均小于100nm,将所制得的微乳液分别在0℃和54℃下储存7天后,微乳液的外观保持均匀,没有任何沉淀或相分离,并且没有析出水相和油相,表明微乳液的稳定性没有显著变化。
实施例4:
称取0.22 g凹土分散于5.0mL去离子水中,超声5分钟,形成水相;同时称取0.5g的高氯氰菊酯,溶于5.0mL甲苯中形成油相,将水相与油相以等体积相混合,加入0.086g司盘80,并在8000rpm的转速下打浆5分钟,即得微乳剂。所得微乳剂中凹土占微乳剂质量浓度为2.0%,司盘80在乳液中的摩尔浓度为20 mM,高氯氰菊酯占微乳剂质量浓度为5%。
所制得的微乳液(W/O)液滴直径均小于100nm,将所制得的微乳液分别在0℃和54℃下储存7天后,微乳液的外观保持均匀,没有任何沉淀或相分离,并且没有析出水相和油相,表明微乳液的稳定性没有显著变化。
实施例5:
称取0.20 g凹土分散于6.0mL去离子水中,超声5分钟,形成水相;同时称取1.5g的高氯氰菊酯,溶于6.0mL甲苯中形成油相,将水相与油相以等体积相混合,加入0.077g司盘80,并在8000rpm的转速下打浆5分钟,即得微乳剂。所得微乳剂中凹土占微乳剂质量浓度为1.5%,司盘80在乳液中的摩尔浓度为15 mM,高氯氰菊酯占微乳剂质量浓度为11%。
所制得的微乳液(W/O)液滴直径均小于100nm,将所制得的微乳液分别在0℃和54℃下储存7天后,微乳液的外观保持均匀,没有任何沉淀或相分离,并且没有析出水相和油相,表明微乳液的稳定性没有显著变化。
对比例:
取7.0mL去离子水中,作为水相;同时称取0.5g的高氯氰菊酯,溶于7.0mL甲苯中形成油相,将水相与油相以等体积相混合,加入0.060g司盘80,并在8000rpm的转速下打浆5分钟,即得乳液。所得乳液中凹土占乳液质量浓度为0%,司盘80在乳液中的摩尔浓度为10 mM,高氯氰菊酯占乳液质量浓度为3%。
所制得的乳液在室温(25℃)下半小时内即有4.2mL油相析出,12小时后油相基本完全析出。
对比实施例1-5与对比例可以发现,当不加入凹土时,少量的司盘80即使在室温(25℃)下也不能形成稳定的微乳液;而加入少量的凹土后(1%-2%),只需少量的司盘80(10-30mM)就可以形成在低温(0℃)、高温(54℃)下均能稳定放置一星期的微乳剂。
上述实施方式只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所做的等效变换或修饰,都应涵盖在本发明的保护范围之内。
Claims (4)
1.一种凹土与表面活性剂司盘80协同稳定的农药微乳剂,其特征在于,由油相、水相及司盘80组成,所述油相为高氯氰菊酯-甲苯有机相,所述水相为凹土-水分散液;
所述高氯氰菊酯在所述微乳剂中的质量浓度为3-17%,所述凹土在所述微乳剂中的质量浓度为1-2%,所述司盘80在所述微乳剂中的摩尔浓度为10-30mM。
2.根据权利要求1所述的凹土与表面活性剂司盘80协同稳定的农药微乳剂,其特征在于,所述油相与水相的体积比为1:1。
3.根据权利要求1所述的凹土与表面活性剂司盘80协同稳定的农药微乳剂,其特征在于,所述凹土为蒙脱石型凹土,其中的凹凸棒石与蒙脱石的总质量含量>85%,且凹凸棒石的质量含量≮30%、粒度<13μm。
4.一种如权利要求1至3中任一项所述的凹土与司盘80协同稳定的农药微乳剂的制备方法,其特征在于,包括以下步骤:
S1:将凹土过325目筛后,加入到去离子水中,超声形成凹土-水分散液,即为水相;同时,将高氯氰菊酯溶于甲苯中形成油相;
S2:将所述油相与所述水相混合后加入司盘80,打浆得所述农药微乳剂。
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