CN107383262A - 一种基于多功能单体及交联剂的多孔吸附剂的制备方法 - Google Patents

一种基于多功能单体及交联剂的多孔吸附剂的制备方法 Download PDF

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CN107383262A
CN107383262A CN201710628763.4A CN201710628763A CN107383262A CN 107383262 A CN107383262 A CN 107383262A CN 201710628763 A CN201710628763 A CN 201710628763A CN 107383262 A CN107383262 A CN 107383262A
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crosslinking agent
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黄晓佳
裴苗
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Xiamen University
Shenzhen Research Institute of Xiamen University
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Abstract

一种基于多功能单体及交联剂的多孔吸附剂的制备方法，涉及多孔吸附剂。将多功能单体、混合交联剂、引发剂和致孔剂混合，超声成溶液，再倒入容器中，密封后聚合反应，所得萃取材料后处理，即得基于多功能单体及交联剂的多孔吸附剂。制备简单、重复性好、低成本和富含功能基团，在对实际样品进行实际萃取时，具有萃取效率高、操作简便、可重复使用和使用寿命长等优点。利用两种功能单体及两种交联剂，制备了含多功能单体及交联剂的多孔吸附剂。由于该吸附剂含有多种官能团，因此具有理想的萃取性能。制备以3‑丙烯酰胺苯硼酸/1‑乙烯基咪唑为多功能单体，二乙烯基苯/乙二醇二甲基丙烯酸酯为混合交联剂，利用原位聚合制备含多功能基团的吸附剂。

Description

一种基于多功能单体及交联剂的多孔吸附剂的制备方法
技术领域
本发明涉及多孔吸附剂，尤其是涉及一种基于多功能单体及交联剂的多孔吸附剂的制备方法。
背景技术
整体材料首先由Hjerten等(Hjerten S,Liao J L,Zhang R.Journal ofChromatography A,1989,473:1)提出，其具有原料丰富、制备简单、通透性好、传质速度快和易改性等优点，目前已被广泛用作高效液相色谱(Zhong J,Hao M B,Li R,etal.Journal of Chromatography A,2014,1333:79)、毛细管液相色谱(MoravcováD,Carrasco-Correa E J,Planeta J,et al.Journal of Chromatography A,2015,1402:27)和毛细管电色谱(Zhao H Y,Wang Y C,Cheng H Y,Journal of Chromatography A,2016,1452:27)等分离模式的固定相。近几年，多孔整体材料也用于复杂样品前处理过程中的分离介质(梅萌，黄晓佳，色谱，2016，12：1168)及蛋白质组学(Zhao C,Yin R C,Yin J F,etal.Analytical Chemistry,2012,84:1157)研究中。
为了有效萃取目标物，根据“相似相溶”原理，吸附剂需能与目标物产生多重作用力。基于整体材料的多孔吸附剂，一般由单体、交联剂、引发剂及致孔剂聚合而成，其中单体种类及组成对吸附剂的萃取性能有很大影响。
发明内容
本发明旨在提供利用两种功能单体及两种交联剂，吸附剂含有多种官能团，具有理想萃取性能的一种基于多功能单体及交联剂的多孔吸附剂的制备方法。
本发明的具体步骤如下：
将多功能单体、混合交联剂、引发剂和致孔剂混合，超声成溶液，再倒入容器中，密封后聚合反应，所得萃取材料后处理，即得基于多功能单体及交联剂的多孔吸附剂；所述多功能单体为3-丙烯酰胺苯硼酸/1-乙烯基咪唑，混合交联剂为二乙烯基苯/乙二醇二甲基丙烯酸酯，引发剂为偶氮二异丁腈或过氧化苯甲酰，致孔剂为二甲基亚砜；所述多功能单体、混合交联剂、引发剂组成反应单体混合剂，所述反应单体混合剂的组成按质量百分比为多功能单体20％～60％，引发剂为0.5％～2％，余为混合交联剂；所述反应单体混合剂∶致孔剂按质量比为1︰(0.5～4)；所述3-丙烯酰胺苯硼酸/1-乙烯基咪唑的质量比可为1/4～4/1，所述二乙烯基苯与乙二醇二甲基丙烯酸酯的质量比可为3/1～1/3。
所述聚合反应的条件可为50～80℃下聚合反应6～24h；所述聚合反应的过程可为：
所述萃取材料后处理的具体方法可为：将萃取材料置于索氏提取器中，以溶剂提取4～24h，或将萃取材料置于溶剂中，浸泡至液体中无杂质检出，使用时，用超纯水分别浸泡活化0.5～24h。所述溶剂可选自甲醇、乙腈、乙醇等中的一种。
本发明以3-丙烯酰胺苯硼酸/1-乙烯基咪唑为多功能单体，二乙烯基苯/乙二醇二甲基丙烯酸酯为混合交联剂，偶氮二异丁腈或过氧化苯甲酰为引发剂，二甲基亚砜为致孔剂；将上述化合物按一定比例混匀后，利用原位聚合技术，在一定温度下引发聚合一定时间，经过后处理即可得到含多功能基团的吸附剂。
本发明所述的吸附剂制备简单、重复性好、低成本和富含功能基团，在对实际样品进行实际萃取时，具有萃取效率高、操作简便、可重复使用和使用寿命长等优点。
本发明利用两种功能单体及两种交联剂，制备了含多功能单体及交联剂的多孔吸附剂。由于该吸附剂含有多种官能团，因此具有理想的萃取性能。
本发明首次制备以3-丙烯酰胺苯硼酸/1-乙烯基咪唑为多功能单体，二乙烯基苯/乙二醇二甲基丙烯酸酯为混合交联剂，利用原位聚合技术制备含多功能基团的吸附剂。该吸附剂具有制备简单、通透性好、富含官能基团、高性价比等优点，因此本发明所制备的吸附剂具有广阔的实际应用价值。
附图说明
图1为本发明实施例2中萃取材料的红外光谱图。在图1中，从左到右的主要吸收峰的波数分别为2950cm-1、1730cm-1、1348cm-1、1278cm-1、1166cm-1、1112cm-1、712cm-1、664cm-1。
图2为本发明实施例2中萃取材料的扫描电镜图。
图3为本发明实施例4中加标6种磺酰脲类除草剂的液相色谱分离谱图。在图3中，曲线a为实际水样萃取前，曲线b为解析液；标记：TRM为氟胺磺隆，THM为噻吩磺隆，MEM为甲磺隆，CHS为氯磺隆，PRS为氟磺隆，HAM为氯吡啶磺隆。
具体实施方式
下面通过实施例对本发明作进一步的说明。
实施例1
1)反应混合试剂的配制：所述反应单体混合剂的组成按质量百分比为3-丙烯酰胺苯硼酸/1-乙烯基咪唑(两种功能单体质量比为1/4)20％，引发剂偶氮二异丁腈0.5％，交联剂二乙烯基苯/乙二醇二甲基丙烯酸酯79.5％(两种交联剂质量比为3/1)；按质量比，反应单体混合剂∶致孔剂为1∶0.5。
2)按上述比例称取反应单体和致孔剂混和后，超声成均一溶液，将上述溶液倒入一定内径的容器中，密封后置于80℃温度下聚合反应6h。
3)萃取材料的后处理：将步骤二获取的萃取材料置于索氏提取器中，以甲醇为溶剂，提取4h，或将萃取材料置于上述溶剂中，浸泡至液体中无杂质检出。在使用前，用超纯水浸泡活化0.5h。
实施例2
1)反应混合试剂的配制：所述反应单体混合剂的组成按质量百分比为3-丙烯酰胺苯硼酸/1-乙烯基咪唑(两种功能单体质量比为1/1)40％，引发剂偶氮二异丁腈1％，交联剂二乙烯基苯/乙二醇二甲基丙烯酸酯59％(两种交联剂质量比为1/2)；按质量比，反应单体混合剂∶致孔剂为1∶1.5。
2)按上述比例称取反应单体和致孔剂混和后，超声成均一溶液，将上述溶液倒入一定内径的容器中，密封后置于70℃温度下聚合反应12h。
3)萃取材料的后处理：将步骤二获取的萃取材料置于索氏提取器中乙腈为溶剂，提取12h，或将萃取材料置于上述溶剂中，浸泡至液体中无杂质检出。在使用前，用超纯水浸泡活化12h。
附图1为萃取材料的红外光谱图，附图2为该材料的扫描电镜图。
实施例3
1)反应混合试剂的配制：所述反应单体混合剂的组成按质量百分比为3-丙烯酰胺苯硼酸/1-乙烯基咪唑(两种功能单体的质量比为4/1)60％，引发剂过氧化苯甲酰2％，余为交联剂二乙烯基苯/乙二醇二甲基丙烯酸酯38％(两种交联剂质量比为1/3)；按质量比，反应单体混合剂∶致孔剂为1∶4。
2)按上述比例称取反应单体和致孔剂混和后，超声成均一溶液，将上述溶液倒入一定内径的容器中，密封后置于50℃温度下聚合反应24h。
3)萃取材料的后处理：将步骤二获取的萃取材料置于索氏提取器中，以乙醇为溶剂，提取24h，或将萃取材料置于上述溶剂中，浸泡至液体中无杂质检出。在使用前，用超纯水浸泡活化24h。
实施例4
按实施例2配制反应溶液，然后将反应溶液注射入细的玻璃毛细纤维(直径0.5mm)中，纤维两端密封后于70℃聚合12h，即可得纤维状萃取材料。合成后去掉每根玻璃纤维两端的密封头，用刀片将玻璃纤维一端的外层纤维涂层和玻璃割除，露出约2cm的纤维状聚合材料。然后，将数根细纤维绑在一起组成固相萃取纤维束。以上即为制得的纤维束固相萃取装置。
实施例5
取实际河湖水样20mL，加入磺酰脲类除草剂(加标浓度均为100μg/L)，将按实施例4制备的固相萃取纤维束中的整体材料部分插入液面，室温在600r/min搅拌萃取吸附50min，然后将纤维束取出，用400μL乙腈/甲酸(99/1，v/v)在同样的转速下解吸20min，色谱条件：Kromasil C18色谱柱(250mm×4.6mm i.d.，5μm)，流速1.0mL/min，进样量20μL。流动相为0.4％磷酸水溶液(A)和乙腈(B)组成，采用梯度洗脱程序，程序如下：0～5min，30％B；5～10min，30％B～55％B；10～13min，55％B～60％B；13～15min，60％B；15～18min，60％B～85％B；18～20min，85％B～30％B；20～21min，30％B。图3为加标水样萃取前(a)和萃取液(b)的液相色谱分离谱图。

Claims (7)

1.一种基于多功能单体及交联剂的多孔吸附剂的制备方法，其特征在于其具体步骤如下：
将多功能单体、混合交联剂、引发剂和致孔剂混合，超声成溶液，再倒入容器中，密封后聚合反应，所得萃取材料后处理，即得基于多功能单体及交联剂的多孔吸附剂；所述多功能单体为3-丙烯酰胺苯硼酸/1-乙烯基咪唑，混合交联剂为二乙烯基苯/乙二醇二甲基丙烯酸酯，引发剂为偶氮二异丁腈或过氧化苯甲酰，致孔剂为二甲基亚砜；所述多功能单体、混合交联剂、引发剂组成反应单体混合剂，所述反应单体混合剂的组成按质量百分比为多功能单体20％～60％，引发剂为0.5％～2％，余为混合交联剂；所述反应单体混合剂∶致孔剂按质量比为1︰(0.5～4)。
2.如权利要求1所述一种基于多功能单体及交联剂的多孔吸附剂的制备方法，其特征在于所述3-丙烯酰胺苯硼酸/1-乙烯基咪唑的质量比为1/4～4/1。
3.如权利要求1所述一种基于多功能单体及交联剂的多孔吸附剂的制备方法，其特征在于所述二乙烯基苯与乙二醇二甲基丙烯酸酯的质量比为3/1～1/3。
4.如权利要求1所述一种基于多功能单体及交联剂的多孔吸附剂的制备方法，其特征在于所述聚合反应的条件为50～80℃下聚合反应6～24h。
5.如权利要求1所述一种基于多功能单体及交联剂的多孔吸附剂的制备方法，其特征在于所述聚合反应的过程为：
6.如权利要求1所述一种基于多功能单体及交联剂的多孔吸附剂的制备方法，其特征在于所述萃取材料后处理的具体方法为：将萃取材料置于索氏提取器中，以溶剂提取4～24h，或将萃取材料置于溶剂中，浸泡至液体中无杂质检出。
7.如权利要求1所述一种基于多功能单体及交联剂的多孔吸附剂的制备方法，其特征在于所述溶剂选自甲醇、乙腈、乙醇中的一种。
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