CN105597695B - 一种功能化β环糊精改性氧化石墨烯复合材料的制备方法 - Google Patents
一种功能化β环糊精改性氧化石墨烯复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,将预先干燥的β‑环糊精用DMF溶解,在氮气保护下,依次加入GPTMS和氢氧化钠反应得到改性环糊精;取改性环糊精用去离子水溶解得到水解产物,加入氧化石墨烯超声反应,得到环糊精改性氧化石墨烯超分子杂化材料。本发明方法具有成本低廉、工艺简单、吸附性能高且易分离、环境友好等优点。
Description
技术领域
本发明属于吸附材料技术领域,具体涉及一种功能化β环糊精改性氧化石墨烯复合材料的制备方法。
背景技术
环糊精,分子形如一个圆筒,外部含有大量的羟基,内部为一疏水空腔,可与许多无机、有机分子结合成主客体包合物,并且能够改变被包合物的物理和化学性质,具有保护、稳定客体分子和选择性定向分子的特性;此外,环糊精具有来源广泛、价格低廉、易降解、无污染等优点,因此,其作为吸附材料在环保等领域中具有重要的研究和应用价值。但在实际应用中,环糊精仍面临着一些问题,如:(1)化学性质不稳定,易溶解而流失;(2)吸附时间长,耗时;(3)对金属离子以及有机污染物的吸附量低;(4)难分离;(5)机械性能差。如何解决好这些问题决定了环糊精在水处理中的应用前景,对其进行改性是一个很好的解决方法。
以石墨烯为载体材料,将环糊精嫁接到其表面,制备环糊精/石墨烯复合纳米材料。此复合材料具有良好的机械性能,具有很大的比表面积,增加了环糊精分子的包络位点,获得具有吸附量大、易于分离、重复使用效果好和无二次污染的-吸附剂。该复合材料可用于废水中重金属的分离富集和有机物废水的处理中。为环境污染的处理和废物回收利用提供了简单易行的方法和手段。
发明内容
本发明的目的在于提供一种新的功能化β环糊精改性氧化石墨烯复合材料的制备方法,致使制备的复合材料能充分发挥各自的性能,增加各自材料在其他方面的应用。
本发明具体通过以下技术方案实现:
一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,包括以下步骤:
1)在圆底烧瓶中加入预先干燥的β-环糊精,然后向其中加入溶剂DMF(N,N-二甲基甲酰胺)溶解环糊精;
2)在氮气保护下加入GPTMS(γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷);
3)继续加入氢氧化钠,在氮气保护下连续搅拌48h,将反应后的溶液冷却到室温并向其中加入丙酮沉淀出产物;
4)在真空烘箱中烘干得到泛黄的白色水溶性粉末即为改性环糊精(β-CD/GPTMS);
5)取改性环糊精(β-CD/GPTMS)用去离子水溶解直到溶解完全,用冰乙酸调节溶液的pH值到4~6,持续搅拌1小时得到水解产物;
6)取氧化石墨烯(GO)并加入到上述水解产物中反应,超声分散处理40分钟后连续搅拌反应10小时,反应完全后的悬浮液用去离子水去洗涤除去未反应的β-CD/GPTMS,抽滤,得到环糊精改性GO超分子杂化材料记为β-CD/GPTMS/GO。
本发明所述的β-环糊精与GPTMS的摩尔比为1:6。
本发明步骤(3)中氢氧化钠在55℃条件下搅拌反应。
本发明步骤(4)中真空烘箱的温度条件为40℃。
本发明所述的改性环糊精与氧化石墨烯的质量比为10:1。
本发明所述的改性环糊精与氧化石墨烯在90℃温度下反应。
本发明的有益效果为:(1)β-CD上含有大量的羟基,通过对其进行功能化改性,能大幅地提高其β-CD在其他方面的反应,拓宽了β-CD的应用方向,充分利用β-CD材料的性能;(2)由于GO表面含有羟基、羧基和环氧基,对阳离子的吸附性能不是很优越,通过β-CD功能化GO,不仅能够增加GO的吸附性能,而且也能增强GO在废水中的分散性,以充分发挥其吸附性能。
通过功能化改性,β-环糊精的利用方向得到拓展,且与GO相结合在一起,不仅能充分利用β-环糊精的结构特点,而且也能提高GO在除去金属离子的能力。β-环糊精功能化GO能够进一步提高GO的分散性,而且使GO的结构更加快速高效的除去金属离子,充分利用两种材料的特点来除去废水中的金属离子来达到净化废水目的。
附图说明
图1是实施例1制备所得β-CD/GPTMS/GO复合物的电镜图。
具体实施方式
下面结合实施例对本发明做进一步的说明,以下所述,仅是对本发明的较佳实施例而已,并非对本发明做其他形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更为同等变化的等效实施例。凡是未脱离本发明方案内容,依据本发明的技术实质对以下实施例所做的任何简单修改或等同变化,均落在本发明的保护范围内。
实施例1
本实施例提供了一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,具体通过以下过程完成。
(1)功能化β-CD的制备
在圆底烧瓶中加入5g预先干燥的β-环糊精,然后向其中加入溶剂40mL DMF(N,N-二甲基甲酰胺)溶解环糊精并进行氮气保护,紧接着在氮气保护下加入5.9mL的GPTMS(β-CD与GPTMS的摩尔比为1:6)。随后,向溶解有环糊精的溶剂中加入0.1g氢氧化钠,在氮气保护和55℃下连续搅拌48h。将反应后的溶液冷却到室温并向其中加入的丙酮沉淀出产物,得到的产物用大量的丙酮洗涤,然后在40℃真空烘箱中烘干得到泛黄的白色水溶性粉末即为改性环糊精即β-CD/GPTMS。
(2)β-CD/GPTMS/GO的制备
取一定量的改性环糊精(β-CD/GPTMS)并用30mL的去离子水溶解直到溶解完全,然后用冰乙酸来调节溶液的pH值到4~6,持续搅拌1小时得到水解产物。紧接着,取一定量的GO并加入到上述水解液中反应,超声分散处理大约40分钟后在90℃温度下连续搅拌反应10小时。反应完全后的悬浮液用大量的去离子水去洗涤除去未反应的β-CD/GPTMS,抽滤,得到环糊精改性GO超分子杂化材料记为β-CD/GPTMS/GO。
将上述制得的β-CD/GPTMS/GO复合物置于扫描电镜下观察,其结构如图1所示,从图中可以看出基地为片层的氧化石墨烯,而图中圆圈区域则为β-CD,说明通过上述方法制备成功制备了β-CD/GPTMS/GO复合物。
实施例2
将实施例1制备的β-CD/GPTMS/GO复合物应用于六价铬离子废水的处理,包括以下步骤:取三个初始浓度分别为10、20和40mg/L的六价铬溶液,调节溶液的pH值为3.0,加入实施例1制得的β-CD/GPTMS/GO复合物,该复合物的用量为0.17g/L,在30℃空气浴恒温振荡器进行振荡吸附反应,转速为180rpm,用紫外分光光度法测定废水中未被吸附的六价铬的含量,计算的吸附量结果见表1。
表1 不同铬初始浓度条件下β-CD/GPTMS/GO复合物对铬的吸附量数据
初始浓度(mg/L) | 10 | 20 | 40 |
吸附量(mg/L) | 45.63 | 56.78 | 70.82 |
由表1可知,在初始浓度为10mg/L的条件下该该复合物对六价铬的吸附量为45.63mg/g,并随初始浓度增加而增加,初始浓度为40mg/L时吸附量达到70.82mg/g。
实施例3
将实施例1制备的β-CD/GPTMS/GO复合物应用于六价铬离子废水的处理,包括以下步骤:取初始浓度为10mg/L的六价铬溶液,调节溶液的pH值为3.0,加入实施例1制得的β-CD/GPTMS/GO复合物,该复合物的用量为0.17g/L,分别在10、30和50℃的空气浴恒温振荡器进行吸附反应,转速为180rpm,用紫外分光光度法测定废水中未被吸附的六价铬的含量,计算的吸附量结果见表2。
表2 不同温度条件下β环糊精与磁性氧化石墨烯复合物对铬的吸附量数据
反应温度(℃) | 10 | 30 | 50 |
吸附量(mg/L) | 35.42 | 38.45 | 44.53 |
由表2可知,在反应温度为10℃的条件下该复合物对铬离子的吸附量为35.42mg/g,并随初始温度的增加而增加,在温度为50℃时吸附量达到44.53mg/g。
实施例4
将实施例1制备的β-CD/GPTMS/GO复合物应用于六价铬离子废水的处理,包括以下步骤:取初始浓度为10mg/L的六价铬溶液,调节溶液的pH值为3.0,加入实施例1制得的β-CD/GPTMS/GO复合物,该吸附剂的用量为0.17g/L,在30℃空气浴恒温振荡器进行振荡吸附反应,转速为180rpm,吸附反应开始10、30、60、360、720、1080和1440分钟后,用紫外分光光度法测定各样品中未被吸附的六价铬的含量,计算的吸附量结果见表3。
表3 不同反应时间下β环糊精与磁性氧化石墨烯复合物对铬的吸附量数据
反应时间(min) | 10 | 30 | 60 | 360 | 720 | 1080 | 1440 |
吸附量(mg/L) | 27.13 | 29.89 | 31.24 | 40.25 | 44.83 | 46.71 | 47.75 |
由表3可知,随着时间的增长,该复合物对金属铬的吸附量逐渐增大,在24小时后增长缓慢,基本达到吸附平衡。
Claims (5)
1.一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,其特征在于,包括以下步骤:
1)在圆底烧瓶中加入预先干燥的β-环糊精,然后向其中加入溶剂DMF溶解环糊精;
2)在氮气保护下加入GPTMS;所述的β-环糊精与GPTMS的摩尔比为1:6;
3)继续加入氢氧化钠,在氮气保护下连续搅拌48h,将反应后的溶液冷却到室温并向其中加入丙酮沉淀出产物;
4)在真空烘箱中烘干得到泛黄的白色水溶性粉末即为改性环糊精;
5)取改性环糊精用去离子水溶解直到溶解完全,用冰乙酸调节溶液的pH值到4~6,持续搅拌1小时得到水解产物;
6)取氧化石墨烯并加入到上述水解产物中反应,超声分散处理40分钟后连续搅拌反应10小时,反应完全后的悬浮液用去离子水去洗涤除去未反应的改性环糊精,抽滤,得到所述的功能化β环糊精改性氧化石墨烯复合材料。
2.根据权利要求1所述的一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,其特征在于,步骤(3)中氢氧化钠在55℃条件下搅拌反应。
3.根据权利要求1所述的一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,其特征在于,步骤(4)中真空烘箱的温度条件为40℃。
4.根据权利要求1所述的一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,其特征在于,所述的改性环糊精与氧化石墨烯的质量比为10:1。
5.根据权利要求4所述的一种功能化β环糊精改性氧化石墨烯复合材料的制备方法,其特征在于,所述的改性环糊精与氧化石墨烯在90℃温度下反应。
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