CN106632809B - 一种中空多孔型阿特拉津分子印迹材料的制备方法 - Google Patents

一种中空多孔型阿特拉津分子印迹材料的制备方法 Download PDF

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CN106632809B
CN106632809B CN201611121567.XA CN201611121567A CN106632809B CN 106632809 B CN106632809 B CN 106632809B CN 201611121567 A CN201611121567 A CN 201611121567A CN 106632809 B CN106632809 B CN 106632809B
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刘骏
杨明
梅运军
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Abstract

本发明涉及一种中空多孔型分子印迹材料的制备方法，包含以下步骤：a.投料；b.反应；c.洗脱，即得到本发明的中空型分子印迹材料。本发明以成本极低的碳酸钙为聚合载体，通过简单的酸洗过程即可获得具有良好通过性的分子印迹材料，该材料在用做固相萃取填充物时，可避免因通过性不好而导致较大的负压，从而大大减少萃取时间；同时，本发明制备的印迹材料因其中空多孔的特性，而具有较大比表面积，使得材料具有更多的结合点位和吸附能力。相对于现有技术，该制备方法并不增加过多的制备程序，材料成本低，并可方便的扩展应用于其他各种分子印迹材料的制备过程。

Description

一种中空多孔型阿特拉津分子印迹材料的制备方法
技术领域
本发明涉及一种中空多孔型阿特拉津分子印迹材料的制备方法。
背景技术
分子印迹技术(MolecularImprintingTechnology，MIT)是高分子化学、材料化学和生物化学的交叉学科，至今已有70年的发展历史，在色谱分离、固相萃取、生物传感器、模拟酶催化、生物医学等方面得到了日益广泛的研究和开发，展示了广阔的应用前景。利用MIT可以在聚合物中留下与模板分子大小、形状以及功能基团空间排列相匹配的空穴，从而获得对目标分子具有特异性识别能力和高亲和力的人工抗体-分子印迹聚合物(MolecularlyImprinted Polymers，MIPs)。与天然生物识别分子抗体、受体、核酸适配体相比，MIPs不但具有可与之相媲美的识别能力，还具有构效预定性、特异识别性、广泛实用性等独特的优势。其抗恶劣环境能力强、稳定性高、使用寿命长、易实现工业化，在分离富集食品和环境中目标物展现了令人瞩目的应用前景。
分子印迹材料具有良好的分子特异识别性，正是这些优异的性能，使得分子印迹材料可以用于环境吸附柱填料、环境监测设备、固相萃取、选择性电极等。中空多孔型材料较之其它形状的颗粒具有流动性好，高通过性，比表面积大等特点，通过控制制备条件，可使得中空多孔材料具备特殊的结构、高比表面积、高吸附性、可组装性、高孔隙率等特性，在催化、生物、电化学、气体吸附、色谱分离、传感器材料等领域已经显示了广泛的应用前景。
分子印迹材料的制备是传统研究热点，不同性能的材料也有合成报到，但集中于材料识别性能的研究，中空型分子印迹材料的制备方法研究鲜见报到。
发明内容
本发明要解决的技术问题是提供了一种中空多孔型阿特拉津分子印迹材料的制备方法。
本发明的技术方案是：一种中空多孔型阿特拉津分子印迹材料的制备方法，其特征在于包含以下步骤：a.投料：将一定量的模板分子、功能单体MMA充分混合2h，再加入一定量交联剂EGDMA、引发剂AIBN和研磨后的碳酸钙粉末，再加入一定体积的乙腈；b.反应：将混合溶液超声混合脱气20分钟后，通入氮气去除溶解氧，并在氮气保护下密封，在65℃、充分搅拌的条件下，聚合反应12个小时；c.洗脱：聚合物用甲醇/乙酸进行12个小时的索氏提取，洗脱去模板分子，溶解掉碳酸钙颗粒；最后在50℃条件下进行真空干燥，进行适当研磨后密封装样保存，即得到中空型分子印迹材料。
本发明一种中空多孔型阿特拉津分子印迹材料的制备方法，其特征在于所述的反应体系中加入了碳酸钙作为聚合核心。
本发明一种中空多孔型阿特拉津分子印迹材料的制备方法，其特征在于所述的碳酸钙用量与交联剂用量质量比为1∶6。
本发明的一种中空多孔型分子印迹材料经红外测定，结果表明它可完全聚合，通过TEM照片，观察到本发明的分子印迹材料形貌为中空呈多孔结构，粒径为2-5μm。
本发明的有益效果是：本发明以成本极低的碳酸钙为聚合载体，通过简单的酸洗过程即可获得具有良好通过性的分子印迹材料，该材料在用做固相萃取填充物时，可避免因通过性不好而导致较大的负压，从而大大减少萃取时间；同时，本发明制备的印迹材料因其中空多孔的特性，而具有较大比表面积，使得材料具有更多的结合点位和吸附能力。相对于现有技术，该制备方法并不增加过多的制备程序，材料成本低，并可方便的扩展应用于其他各种分子印迹材料的制备过程。
具体实施方式
下面结合实施例对本发明进一步说明。
实施例1：一种中空多孔型阿特拉津分子印迹材料的制备方法，包含以下步骤：a.投料：将一定量的模板分子、功能单体MMA充分混合2h，再加入一定量交联剂EGDMA、引发剂AIBN和研磨后的碳酸钙粉末，再加入一定体积的乙腈；b.反应：将混合溶液超声混合脱气20分钟后，通入氮气去除溶解氧，并在氮气保护下密封，在65℃、充分搅拌的条件下，聚合反应12个小时；c.洗脱：聚合物用甲醇/乙酸进行12个小时的索氏提取，洗脱去模板分子，溶解掉碳酸钙颗粒；最后在50℃条件下进行真空干燥，进行适当研磨后密封装样保存，即得到中空型分子印迹材料。所述的反应体系中加入了碳酸钙作为聚合核心。
实施例2：一种中空多孔型阿特拉津分子印迹材料的制备方法，包含以下步骤：a.投料：将一定量的模板分子、功能单体MMA充分混合2h，再加入一定量交联剂EGDMA、引发剂AIBN和研磨后的碳酸钙粉末，再加入一定体积的乙腈；b.反应：将混合溶液超声混合脱气20分钟后，通入氮气去除溶解氧，并在氮气保护下密封，在65℃、充分搅拌的条件下，聚合反应12个小时；c.洗脱：聚合物用甲醇/乙酸进行12个小时的索氏提取，洗脱去模板分子，溶解掉碳酸钙颗粒；最后在50℃条件下进行真空干燥，进行适当研磨后密封装样保存，即得到中空型分子印迹材料。所述的反应体系中加入了碳酸钙作为聚合核心。所述的碳酸钙用量与交联剂用量质量比为1∶6。
实施例3：
将0.08627g模板分子阿特拉津，0.25ml功能单体MMA，充分混合后静置反应2h，再加入3ml交联剂EGDMA，0.02g的引发剂AIBN，将0.5g的碳酸钙粉末进行充分研磨，研磨后的碳酸钙粉末加到装有50ml乙腈的250ml平底烧瓶中。加入磁子，超声混合脱气20分钟后，通入氮气去除溶解氧，并在氮气保护下密封。置于60℃的恒温集热磁力搅拌器中，调整搅拌速度使碳酸钙粉末达到悬浮状态，聚合反应12个小时。聚合物用甲醇/乙酸(70∶30，v/v)100ml进行12个小时的索氏提取，洗脱去阿特拉津模板分子，溶解掉碳酸钙颗粒。最后在50℃条件下进行真空干燥，进行适当研磨后密封装样保存。所述步骤制备产物即为中空多孔型分子印迹材料。
实施例4：将0.08627g模板分子阿特拉津，0.25ml功能单体MMA，充分混合后静置反应2h，再加入3ml交联剂EGDMA，0.02g的引发剂AIBN，将0.3g的碳酸钙粉末进行充分研磨，研磨后的碳酸钙粉末加到装有50ml乙腈的250ml平底烧瓶中。加入磁子，超声混合脱气20分钟后，通入氮气去除溶解氧，并在氮气保护下密封。置于60℃的恒温集热磁力搅拌器中，调整搅拌速度使碳酸钙粉末达到悬浮状态，聚合反应12个小时。聚合物用甲醇/乙酸(70∶30，v/v)100ml进行12个小时的索氏提取，洗脱去阿特拉津模板分子，溶解掉碳酸钙颗粒。最后在50℃条件下进行真空干燥，进行适当研磨后密封装样保存。所述步骤制备产物即为中空多孔型分子印迹材料。
实施例5：将0.08627g模板分子阿特拉津，0.25ml功能单体MMA，充分混合后静置反应2h，再加入5ml交联剂EGDMA，0.02g的引发剂AIBN，将0.5g的碳酸钙粉末进行充分研磨，研磨后的碳酸钙粉末加到装有10ml乙腈的250ml平底烧瓶中。加入磁子，超声混合脱气20分钟后，通入氮气去除溶解氧，并在氮气保护下密封。置于60℃的恒温集热磁力搅拌器中，调整搅拌速度使碳酸钙粉末达到悬浮状态，聚合反应12个小时。聚合物用甲醇/乙酸(70∶30，v/v)100ml进行12个小时的索氏提取，洗脱去阿特拉津模板分子，溶解掉碳酸钙颗粒。最后在50℃条件下进行真空干燥，进行适当研磨后密封装样保存。所述步骤制备产物即为中空多孔型分子印迹材料。本发明的一种中空多孔型分子印迹材料经红外测定，结果表明它可完全聚合，通过TEM照片，观察到本发明的分子印迹材料形貌为中空呈多孔结构，粒径为2-5μm。

Claims (3)

1.一种中空多孔型阿特拉津分子印迹材料的制备方法，其特征在于包含以下步骤：a.投料：将一定量的模板分子、功能单体MMA充分混合2h，再加入一定量交联剂EGDMA、引发剂AIBN和研磨后的碳酸钙粉末，再加入一定体积的乙腈；b.反应：将混合溶液超声混合脱气20分钟后，通入氮气去除溶解氧，并在氮气保护下密封，在65℃、充分搅拌的条件下，聚合反应12个小时；c.洗脱：聚合物用甲醇/乙酸进行12个小时的索氏提取，洗脱去模板分子，溶解掉碳酸钙颗粒；最后在50℃条件下进行真空干燥，进行适当研磨后密封装样保存，即得到中空型分子印迹材料。
2.根据权利要求1所述的一种中空多孔型阿特拉津分子印迹材料的制备方法，其特征在于所述的反应体系中加入了碳酸钙作为聚合核心。
3.根据权利要求1所述的一种中空多孔型阿特拉津分子印迹材料的制备方法，其特征在于所述的碳酸钙用量与交联剂用量质量比为1∶6。
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