CN106084282B - 一种快速阳离子聚合制备疏水亲油复合材料的方法及应用 - Google Patents

一种快速阳离子聚合制备疏水亲油复合材料的方法及应用 Download PDF

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CN106084282B
CN106084282B CN201610392638.3A CN201610392638A CN106084282B CN 106084282 B CN106084282 B CN 106084282B CN 201610392638 A CN201610392638 A CN 201610392638A CN 106084282 B CN106084282 B CN 106084282B
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朱小彪
刘亚鹏
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Abstract

本发明公开了一种快速阳离子聚合制备疏水亲油复合材料的方法，包括以下步骤：S1：聚氨酯海绵或无纺布改性，在适量正己烷溶剂中加入聚氨酯海绵或无纺布，并且滴加十八烷基三氯硅烷，室温水浴搅拌，取出吹干；S2：超声处理，取适量改性后的聚氨酯海绵或无纺布放入圆底烧瓶中，之后加入正己烷有机溶剂，再加入三氟化硼乙醚引发剂，超声片刻之后加入二乙烯基苯单体继续超声反应；S3：烘干，将S2中的产物用镊子取出后，用无水乙醇冲洗三遍后放入烘箱烘干，得到疏水亲油复合材料。本发明提出的疏水亲油复合材料能吸附等同于自身重量的四十倍油类；并且油类回收简单快速，能够多次重复使用，该方法也可以在无纺布、脱脂棉以及其他纺织物上实现。

Description

一种快速阳离子聚合制备疏水亲油复合材料的方法及应用
技术领域
本发明涉及一种适用于原油泄漏，油田排放污水回收以及处理的环境友好型吸附剂及其制备方法，属于环境材料，高分子化学及聚合物和环境保护技术领域，具体为一种快速阳离子聚合制备疏水亲油复合材料的方法及应用。
背景技术
随着科技的快速发展和能源的日益匮乏，人类对石油及其副产物的需求越来越高，加剧了能源危机和含油废水的污染。含油废水来源广泛，石油产业中原油等油品的开发、加工和运输等，冶金制造业产生的乳化油废水等。高浓度的含油废水流入江河湖海中就会形成大片的油膜，这不仅仅造成了油品的浪费，而且这层油膜使阳光穿透不了水面，从而使水下藻类的光合作用下降，导致水中的溶解氧急剧下降，严重的会导致水中生物的死亡，破坏水中生态平衡。同时，含油废水成分复杂且难生物降解，一般的生物方法很难做到去除水中的油类，这些有害成分会通过生物链最终在人体内积累，危害人类的身体安全。
含油废水的处理方法主要有气浮法、化学絮聚法、电解法、电磁法、膜分离法、物理吸附法以及生物法等。吸附法是利用吸附剂表面的活性,将分子态的污染物浓集于表面而达到去除目的。人们床用的传统的吸附剂主要有活性炭、木丝绵、聚丙烯纤维以及吸附树脂等，但是传统的吸油材料普遍存在以下问题，1：吸附量比较小，只能吸附等同于自身重量几倍或者十几倍的油品；2：传统吸油材料在吸油的同时也会吸附水，影响油品的吸收；3：解吸困难，不能够有效的回收油品。
发明内容
本发明的目的在于提供一种快速阳离子聚合制备疏水亲油复合材料的方法及应用，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：
一种快速阳离子聚合制备疏水亲油复合材料的方法，包括以下步骤：
S1：聚氨酯海绵或无纺布改性，在适量正己烷溶剂中加入聚氨酯海绵或无纺布，并且滴加十八烷基三氯硅烷，室温水浴搅拌，取出吹干；
S2：超声处理，取适量改性后的聚氨酯海绵或无纺布放入圆底烧瓶中，之后加入正己烷有机溶剂，再加入三氟化硼乙醚引发剂，超声片刻之后加入二乙烯基苯单体继续超声反应；
S3：烘干，将S2中的产物用镊子取出后，用无水乙醇冲洗三遍后放入烘箱烘干，得到疏水亲油复合材料。
优选的，步骤S1中加入聚氨酯海绵或无纺布1g，正己烷溶剂为60ml，十八烷基三氯硅烷2mL，室温水浴搅拌24h，用N2吹干。
更进一步的，步骤S2中改性后的聚氨酯海绵或无纺布0.5g，正己烷有机溶剂100mL，三氟化硼乙醚100uL，超声片刻的时间为1-2min，继续超声反应的时间为30min。
一种由上述的制备方法得到的疏水亲油复合材料。
本发明另一方面还提供一种快速阳离子聚合反应制备PDVB的方法，以正己烷为有机溶剂，三氟化硼乙醚为引发剂，超声片刻之后加入二乙烯基苯单体，再继续超声反应30℃即可得到大量的一维纳米材料PDVB。
优选的，所述二乙烯基苯单体需要过碱性Al2O3的柱子以去除单体中存在的叔丁基邻苯二酚阻聚剂。
本发明还提供一种上述疏水亲油复合材料的应用，该应用包括以下步骤：
将疏水亲油复合材料放到盛有实验模拟含油废水的玻璃容器内，吸附废水表面的柴油；
进一步的，还提供另一种疏水亲油复合材料的应用，该应用包括以下步骤：
将疏水亲油复合材料填充到反应器中，用蠕动泵控制适量的流速下往反应器中循环注入模拟废水运行2h后观察废水中含油量的变化。
与现有技术相比，本发明的有益效果是：本发明提出的疏水亲油复合材料能吸附等同于自身重量的四十倍油类；使油类通过，而水会被阻隔在上面，吸油的同时不吸水，并且重复使用10次后，该疏水亲油复合材料的吸附量依然保持在40g/g左右，而且通过扫描电镜观察到该复合材料的表面特征几乎没变化，表现出良好的再生性能，该方法也可以在无纺布、脱脂棉以及其他纺织物上实现。
附图说明
图1为一维纳米纤维材料聚二乙烯基苯电镜图；
图2中(A)空白无纺布的电镜照片，(B)为改性无纺布制得的疏水亲油复合材料的电镜照片，可以看出改性后的无纺布表面基本上都成功负载上了聚二乙烯基苯；
图3中(A)空白聚氨酯海绵的电镜照片，(B)为改性聚氨酯海绵制得的疏水亲油复合材料的电镜照片，可以看出改性后的聚氨酯海绵表面也基本上都成功负载上了聚二乙烯基苯；
图4为疏水亲油复合材料吸附表面油的效果图。
具体实施方式
下面将结合本发明实施例中的附图1-4，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅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
一种快速阳离子聚合制备疏水亲油复合材料的方法，包括以下步骤：
S1：聚氨酯海绵改性，在60ml正己烷溶剂中加入聚氨酯海绵1g，并且滴加2ml十八烷基三氯硅烷，室温水浴并用磁子搅拌24h，水浴后取出用N2吹干待用；
S2：超声处理，取0.5g改性后的聚氨酯海绵放入200ml圆底烧瓶中，之后加入100ml正己烷有机溶剂，再加入100ul三氟化硼乙醚引发剂，超声1～2min之后加入二乙烯基苯单体继续超声反应30min左右；
S3：烘干，将S2中的产物用镊子取出后，用无水乙醇冲洗三遍后放入烘箱烘20min后取出，得到疏水亲油复合材料。
实施例2
实施例1中步骤S2所涉及的快速阳离子聚合反应制备PDVB的方法，包括以下步骤，以正己烷为有机溶剂，三氟化硼乙醚为引发剂，超声片刻之后加入二乙烯基苯单体，再继续超声反应30℃即可得到大量的一维纳米材料PDVB。二乙烯基苯单体是经过碱性Al2O3的柱子以去除单体中存在的叔丁基邻苯二酚阻聚剂。
实施例3
实施例1制备的疏水亲油复合材料的吸油性能测试，该疏水亲油复合材料作为含油废水的吸附剂，通过接触角测量仪测得其中聚氨酯海绵的接触角由原来的90°增为127°。取0.05g的疏水亲油复合材料放入盛有10mL柴油的小烧杯中，吸附1min后取出直接称取吸满油的疏水亲油复合材料的重量，最后计算出该疏水亲油复合材料能吸附等同于自身重量40倍的柴油。
实施例4
实施例1制备的疏水亲油复合材料的再生性能测试，取0.05g的疏水亲油复合材料放入50mL的纯油体系中，吸附1min待吸满油后取出称其质量的变化，称量质量后挤压疏水亲油复合材料使其体积缩小70％左右时大部分的油都已挤压出来，再用无水乙醇冲洗三次后放入烘箱烘干，重复以上过程。实验发现：重复使用10次后，该疏水亲油复合材料的吸附量依然保持在40g/g左右，而且通过扫描电镜观察到该复合材料的表面特征几乎没变化，表现出良好的再生性能。
实施例5
疏水亲油复合材料的应用，在盛有100mL去离子水的锥形瓶中放入1g的柴油，在30℃下放入震荡箱中以200r/min震荡2h，配置成模拟含油废水，放入玻璃容器内，将疏水亲油复合材料放到该玻璃容器内，吸附废水表面的柴油。
实施例6
疏水亲油复合材料的应用，取适量的疏水亲油复合材料填充到反应器中，通过蠕动泵以恒定流速往反应器中循环注入模拟废水，接触2h后测其COD。数值与空白作对比，可以观察到模拟含油废水的COD降低了16.35％，说明疏水亲油复合材料对乳化油也有一定的处理效果。
实施例7
第二种疏水亲油复合材料的制备方法，其与实施例1的区别在于，用无纺布替换聚氨酯海绵
取适量改性后烘干的无纺布放入200mL的圆底烧瓶中，加入100mL的正己烷有机溶剂，再滴加100uL的三氟化硼乙醚引发剂，超声1～2min后加入去除过阻聚剂的二乙烯基苯单体继续超声反应30min左右；将上一过程中的产物用镊子取出后，用无水乙醇冲洗三遍后放入烘箱烘20min后取出，得到改性无纺布复合材料。
通过接触角测量仪测得无纺布的接触角由原来的99°增为123.5°。研究发现该材料具有很好的疏水亲油性，其能使油类通过，而水会被阻隔在上面。实验用偶氮染料将柴油或者四氯化碳等有机溶剂染成红色后，按照有机溶剂和去离子水1:1的比例配好溶液通过该复合材料，发现有机溶剂会全部渗透出来，而复合材料上面则是澄清的水。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (6)

1.一种快速阳离子聚合制备疏水亲油复合材料的方法，其特征在于，包括以下步骤：
S1：聚氨酯海绵或无纺布改性，在适量正己烷溶剂中加入聚氨酯海绵或无纺布，并且滴加十八烷基三氯硅烷，室温水浴搅拌，取出吹干；
S2：超声处理，取适量改性后的聚氨酯海绵或无纺布放入圆底烧瓶中，之后加入正己烷有机溶剂，再加入三氟化硼乙醚引发剂，超声片刻之后加入二乙烯基苯单体继续超声反应；
S3：烘干，将S2中的产物用镊子取出后，用无水乙醇冲洗三遍后放入烘箱烘干，得到疏水亲油复合材料。
2.如权利要求1所述的方法，其特征在于，步骤S1中加入聚氨酯海绵或无纺布1g，正己烷溶剂为60ml，十八烷基三氯硅烷2mL，室温水浴搅拌24h，用N2吹干。
3.如权利要求1或2所述的方法，其特征在于，步骤S2中改性后的聚氨酯海绵或无纺布0.5g，正己烷有机溶剂100mL，三氟化硼乙醚100μ L ，超声片刻的时间为1-2min，继续超声反应的时间为30min。
4.一种由权利要求1或2或3所述的方法得到的疏水亲油复合材料。
5.一种如权利要求4所述的疏水亲油复合材料的应用，其特征在于，该应用包括以下步骤：
将疏水亲油复合材料放到盛有实验模拟含油废水的玻璃容器内，吸附废水表面的柴油。
6.一种如权利要求4所述的疏水亲油复合材料的应用，其特征在于，该应用包括以下步骤：
将疏水亲油复合材料填充到反应器中，用蠕动泵控制适量的流速下往反应器中循环注入模拟废水运行2h。
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