CN102423685B - 一种氨基功能化mcm-48介孔材料的制备方法 - Google Patents
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Abstract
一种氨基功能化MCM-48介孔材料的制备方法，将模板剂十六烷基三甲基溴化铵和聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物溶于水，加入氢氧化钠，再加入氟化钠，最后加入正硅酸乙酯和3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷；物料的摩尔比为：正硅酸乙酯∶3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷∶十六烷基三甲基溴化铵∶聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物∶NaOH∶NaF＝1∶0.085∶0.13∶0.013∶0.5∶0.1；然后在40℃下搅拌24小时后，在100℃下晶化24小时，再洗涤、过滤、烘干，去除模板剂得氨基功能化MCM-48材料。该方法采用操作过程简单、合成时间短。
Description
技术领域
本发明属于无机功能材料以及废水处理技术领域的制备方法，特别涉及一种氨基功能化MCM-48介孔材料的制备方法。
背景技术
随着社会的发展尤其是工业的发展，重金属污染已经成为日益严重的环境问题。由于重金属具有毒性和不可降解性，进而可以通过食物链进入人体后可以累积在人体的某些器官中，造成慢性累积性中毒。为了保护和改善人类的生存环境，人们利用各种方法去除重金属离子，主要有化学沉淀法、吸咐法、离子交换、溶剂萃取法等。吸附法是一种简单易行的处理方法，常用的吸附剂有活性炭、沸石及膨润土等矿物。和这些材料相比，介孔材料具有大比表面积，高孔隙率，低密度，高透过性，可组装性，高吸附性等诸多性能，因此其吸附效果要明显优于其他材料。近年来随着介孔材料合成技术日趋成熟，越来越多的学者开始深入研究介孔材料作为一种新的吸附材料。
MCM-48具有两套螺旋三维孔道，有优良的传输性能，不易造成吸附分子移动的障碍，是一种很好的分离富集材料。介孔材料MCM-48比表面积大，孔道内表面易于有机修饰，孔径分布均匀，水热稳定性好。因此，MCM-48是一种很好的载体。
中国专利(CN 1404917A，2003)公开了一种巯基官能化MCM-48的制备方法，是将巯丙基三甲基硅烷溶于甲苯，再加入焙烧的MCM-48这种嫁接后处理方法。该方法制备的巯基官能化的MCM-48对汞离子具有较高的吸收容量。但该发明方法制备巯基官能化MCM-48过程复杂，使用甲苯对环境有污染，且用于吸附其他重金属离子未见报道。
Chunyan Liu等(Journal of Non-Crystalline Solids，2010，356，1246-1251)采用十六烷基三甲基溴化铵(CTAB)和聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物(P123)为共模板剂，制备了纯MCM-48，并对B12有高的吸附量。Hideaki Yoshitake等(Bull.Chem.Soc.Jpn.，2003，76，847-852)用嫁接法合成氨基功能化的MCM-48，对Cr(VI)和As(V)有较高的吸附量，但合成过程复杂和使用了对环境污染的甲苯，且未吸附其他重金属离子。
发明内容
本发明要解决的技术问题是提供一种工艺简单，生产周期短的氨基功能化MCM-48介孔材料的制备方法。
为解决该技术问题，本发明采用的技术方案为：
一种氨基功能化MCM-48介孔材料的制备方法，其特征在于包括以下步骤：
1)将模板剂溶于水中，而后向混合溶液中加入氢氧化钠，再加入氟化钠，搅拌溶解，最后加入硅源和氨基官能化试剂；所述模板剂为十六烷基三甲基溴化铵和聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物，氨基官能化试剂为3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷，所用的硅源为正硅酸乙酯；所用物料的摩尔比为：正硅酸乙酯∶3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷∶十六烷基三甲基溴化铵∶聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物∶NaOH∶NaF＝1∶0.085∶0.13∶0.013∶0.5∶0.1。
2)合成体系在40℃下搅拌24小时后放入高压反应釜，在100℃下晶化24小时，再洗涤、过滤、烘干，去除模板剂得氨基功能化MCM-48材料。
步骤2中去除模板剂的条件是溶剂为无水乙醇；回流温度为80～90℃；回流时间为12～24小时；真空干燥温度为40～60℃。较佳的是：回流温度为85℃；回流时间为24小时；真空干燥温度为50℃。
本发明所制备的氨基功能化MCM-48介孔材料用于废水中重金属离子的去除。本发明方法采用双模板剂共聚法合成技术，与嫁接法相比，操作过程简单、合成时间短；在合成中未使用甲苯，并且用无水乙醇作为萃取溶剂，较为环保；使用这两种模板剂合成的氨基功能化MCM-48水热稳定性好，对Mn(II)和Zn(II)吸收性能优良，具有很高的吸附量。
附图说明：
图1是本发明氨基功能化MCM-48介孔材料吸附Mn(II)的等温吸附曲线。
图2是本发明氨基功能化MCM-48介孔材料吸附Zn(II)的等温吸附曲线。
具体实施方式：
下面通过实例进一步描述本发明的特征，但本发明并不局限于下述实例。
实施例1
称取5.278g(0.00091mol)的聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物于圆底烧瓶中，加入适量去离子水，恒温40℃下搅拌至完全溶解，然后加入3.316g(0.0091mol)十六烷基三甲基溴化铵，加入1.40g(0.035mol)NaOH和0.294g(0.007mol)NaF，再逐滴加入15.5mL(0.07mol)的正硅酸乙酯和1.53mL(0.00595mol)3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷，继续搅拌一段24小时后，所得溶胶放入高压反应釜中，100℃晶化24小时。待晶化完全后，所得固体样品经二次水和无水乙醇洗涤、过滤和干燥，所得样品放在索氏提取器中，用乙醇在85℃回流24h，在真空干燥温度50℃烘干，即得氨基功能化MCM-48材料。
实施例2
在50mL具塞锥形瓶中，加入10～400mg/L Mn(II)，用缓冲溶液调节pH为7，再加入30mg氨基功能化MCM-48材料，控制温度为25℃振荡2小时，经过离心，用ICP-AES测定溶液中剩余的金属离子的浓度。根据平衡离子浓度和吸附量，绘制等温吸附曲线(见图1)，实验数据进行Langmuir拟合，经计算可得饱和吸附量为63.93mg/g。
实施例3
在50mL具塞锥形瓶中，加入10～200mg/L Zn(II)，用缓冲溶液调节pH为7，再加入30mg氨基功能化MCM-48材料，控制温度为30℃振荡2小时，经过离心，用ICP-AES测定溶液中剩余的金属离子的浓度。根据平衡离子浓度和吸附量，绘制等温吸附曲线(见图2)，实验数据进行Langmuir拟合，经计算可得饱和吸附量为83.33mg/g。
实施例4
在50mL具塞锥形瓶中，加入10～400mg/L Mn(II)，用缓冲溶液调节pH为7，再加入30mg氨基功能化MCM-48材料，控制温度为35℃振荡2小时，经过离心，用ICP-AES测定溶液中剩余的金属离子的浓度。根据平衡离子浓度和吸附量，绘制等温吸附曲线(见图1)，实验数据进行Langmuir拟合，Mn(II)的饱和吸附量为71.63mg/g。
实施例5
在50mL具塞锥形瓶中，加入10～200mg/L Zn(II)，用缓冲溶液调节pH为7，再加入30mg氨基功能化MCM-48材料，控制温度为40℃振荡2小时，经过离心，用ICP-AES测定溶液中剩余的金属离子的浓度。根据平衡离子浓度和吸附量，绘制等温吸附曲线(见图2)，实验数据进行Langmuir拟合，Zn(II)的饱和吸附量为90.91mg/g。
实施例6
在50mL具塞锥形瓶中，加入10～400mg/L Mn(II)，用缓冲溶液调节pH为7，再加入30mg氨基功能化MCM-48材料，控制温度为45℃振荡2小时，经过离心，用ICP-AES测定溶液中剩余的金属离子的浓度。根据平衡离子浓度和吸附量，绘制等温吸附曲线(见图1)，实验数据进行Langmuir拟合，Mn(II)的饱和吸附量为81.83mg/g。
实施例7
在50mL具塞锥形瓶中，加入10～200mg/L Zn(II)，用缓冲溶液调节pH为7，再加入30mg氨基功能化MCM-48材料，控制温度为50℃振荡2小时，经过离心，用ICP-AES测定溶液中剩余的金属离子的浓度。根据平衡离子浓度和吸附量，绘制等温吸附曲线(见图2)，实验数据进行Langmuir拟合，Zn(II)的饱和吸附量为100.00mg/g。
从上述实施例中，可得出氨基功能化MCM-48的吸附剂对Mn(II)和Zn(II)两种金属离子有很好的吸附效果。实施例2、4和6的结果和从实施例3、5和7的结果得出，氨基功能化MCM-48介孔材料对Mn(II)和Zn(II)的饱和吸附量随温度的增大而增大。
Claims (3)
1.一种氨基功能化MCM-48介孔材料的制备方法，其特征在于包括以下步骤：
1）将模板剂溶于水中，而后向混合溶液中加入氢氧化钠，再加入氟化钠，搅拌溶解，最后加入硅源和氨基官能化试剂；所述模板剂为十六烷基三甲基溴化铵和聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物，氨基官能化试剂为3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷，所用的硅源为正硅酸乙酯；所用物料的摩尔比为：正硅酸乙酯:3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷:十六烷基三甲基溴化铵:聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物:NaOH:NaF=1:0.085:0.13:0.013:0.5:0.1；
2）合成体系在40℃下搅拌24小时后放入高压反应釜中，在100℃下晶化24小时，再洗涤、过滤、烘干，去除模板剂得氨基功能化MCM-48介孔材料。
2.根据权利要求1所述的制备方法，其特征在于步骤2）中去除模板剂的条件是溶剂为无水乙醇；回流温度为85℃；回流时间为24小时；真空干燥温度为50℃。
3.根据权利要求1所述的方法制备得到的氨基功能化MCM-48介孔材料在吸附Mn(II)或Zn(II)中的应用。
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| CN104128161B (zh) * | 2013-05-03 | 2018-06-15 | 中国科学院生态环境研究中心 | 一种氨基改性活性焦重金属吸附剂及其制备方法 |
| CN105384181A (zh) * | 2015-11-06 | 2016-03-09 | 中国科学院山西煤炭化学研究所 | 一种共模板剂合成含铝mcm-48介孔分子筛的方法 |
| CN106925225B (zh) * | 2017-03-17 | 2020-11-03 | 北京中能环科技术发展有限公司 | 一种组氨酸功能化介孔分子筛吸附剂及其在废水处理中的应用 |
| CN107552026B (zh) * | 2017-09-06 | 2020-08-04 | 大连海洋大学 | 用于重金属脱除的改性介孔材料 |
| CN108530007A (zh) * | 2018-06-15 | 2018-09-14 | 德华兔宝宝装饰新材股份有限公司 | 一种室内甲醛分解纸面石膏板及其制备方法 |
| CN110627083B (zh) * | 2018-06-25 | 2022-01-04 | 中国石油化工股份有限公司 | 一种氨基功能化mcm分子筛的制备方法及其应用 |
| CN110354892B (zh) * | 2019-06-20 | 2022-02-22 | 山东科技大学 | 氧化物改性mcm-48分子筛的制备方法及其在脱硝协同脱汞中的应用 |
| CN113769703B (zh) * | 2021-08-20 | 2024-07-12 | 绍兴蓝竹新材料科技有限公司 | 一种氨基功能化有序介孔氧化硅吸附剂的制备方法 |
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| US6096288A (en) * | 1998-10-12 | 2000-08-01 | Mobil Oil Corporation | Synthesis of the cubic mesoporous molecular sieve MCM-48 |
| CN101214966A (zh) * | 2007-12-27 | 2008-07-09 | 中国人民解放军国防科学技术大学 | 一种高氨基含量有序介孔二氧化硅薄膜及其制备方法和应用 |
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