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CN107855109A - 一种提高含锌沸石类唑基骨架材料co2吸附性能的方法 - Google Patents

一种提高含锌沸石类唑基骨架材料co2吸附性能的方法 Download PDF

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CN107855109A
CN107855109A CN201711068415.2A CN201711068415A CN107855109A CN 107855109 A CN107855109 A CN 107855109A CN 201711068415 A CN201711068415 A CN 201711068415A CN 107855109 A CN107855109 A CN 107855109A
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oxazolyl
framework material
containing zinc
zeolites containing
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刘双
刘澜涛
周艳丽
胡春华
王涛
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Shangqiu Normal University
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Abstract

本发明属于多孔材料气体吸附技术领域,公开了一种提高含锌沸石类唑基骨架材料CO2吸附性能的方法,该方法对预合成的含锌沸石类唑基骨架材料采用后修饰负载,通过氮原子与不饱和的锌金属中心的配位作用将哌嗪引入含锌沸石类唑基骨架材料的孔道中。利用碱性的哌嗪与酸性CO2分子之间的亲和性,增加含锌沸石类唑基骨架材料孔道对CO2的吸收吸附热,使含锌沸石类唑基骨架材料对CO2的吸附量增加,在原来基础上增加30~35%。本发明方法简单,可高效吸附CO2

Description

一种提高含锌沸石类唑基骨架材料CO2吸附性能的方法
技术领域
本发明属于多孔材料气体吸附技术领域,具体涉及一种提高含锌沸石类唑基骨架材料CO2吸附性能的方法。
背景技术
沸石类唑基骨架材料是由金属离子和唑基配体连接而成的三维晶体结构,具有特殊的孔道结构,微孔发达又高度集中,且具有大的孔隙率,是一种理想的高容量气体吸附材料。沸石类唑基骨架材料对于二氧化碳捕捉及分离表现出极大的潜力[Chemsuschem,2014, 7, 3202],可用于高纯气体净化领域,主要吸附去除二氧化碳杂质气体。研究表明,沸石类唑基骨架材料的孔道表面性质是影响其二氧化碳吸附性能的主要因素。因此,对沸石类唑基骨架材料的孔道进行修饰改性,有利用提高二氧化碳吸附性能。
发明内容
基于目前沸石类唑基骨架材料CO2吸附性能不够理想,本发明的目的在于提供一种提高含锌沸石类唑基骨架材料CO2吸附性能的方法。
为实现本发明目的,本发明采用的技术方案为:
所述的提高含锌沸石类唑基骨架材料CO2吸附性能的方法通过如下步骤实现:
1)将含锌沸石类唑基骨架材料超声分散于无水正己烷中,超声使含锌沸石类唑基骨架材料均匀分散,并施加氮气保护;
2)在步骤(1)所述分散液中加入哌嗪,保持磁力搅拌,回流反应;
3)步骤(2)所述反应结束后,对反应液抽滤,将固体产物加入无水正己烷中浸渍,抽滤;
4)重复步骤(3),将固体产物常温真空干燥,得到产品;
所述的含锌沸石类唑基骨架材料为ZIF-8,ZIF-8的BET比表面积在1000~1200m2/g。
优选:按照每30~50mL无水正己烷加入1克含锌沸石类唑基骨架材料的比例进行超声分散。
优选:哌嗪与含锌沸石类唑基骨架材料中不饱和锌离子的摩尔比为5~10:1。
本发明有益效果:本发明采用后修饰负载,通过氮原子与不饱和的锌金属中心的配位作用将哌嗪引入含锌沸石类唑基骨架材料的孔道中,利用碱性的哌嗪与酸性CO2分子之间的亲和性,增加含锌沸石类唑基骨架材料孔道对CO2的吸收吸附热,进一步将含锌沸石类唑基骨架材料的CO2吸附性能提高30~35%。该方法有利于提高此类材料的二氧化碳吸附性能。
附图说明
图1为二氧化碳吸附量测试装置图;图中1-氦气电磁阀;2-二氧化碳低流量电磁阀;3-二氧化碳高流量电磁阀;4-10 Torr压力传感器;5-1000 Torr压力传感器;6-1000Torr压力传感器;7-10 torr压力传感器;8-1000 Torr压力传感器;9-样品管电磁阀;10-P0参比管电磁阀;11-样品管;12-P0参比管;13-真空电磁阀;14-超高真空电磁阀;15-高真空电磁阀;16-涡轮分子泵;17-隔膜泵;18-真空冷凝电磁阀;19-真空冷凝三向阀;20-脱气站1号;21-脱气站2号。
图2为实施例1和对比例1的X射线粉末衍射谱图,图中1为实施例1,2为对比例1。
图3为实施例1、对比例1、对比例2和对比例3在298K下二氧化碳等温吸附曲线,图中1为对比例1,2为对比例2,3为对比例3,4为实施例1。
具体实施方式
下面结合具体实施例对本发明作进一步的解释说明,但具体实施例并不对本发明作任何限定。除非特别说明,实施例中所涉及的试剂、方法均为本领域常用的试剂和方法。
实施例1
(a)含锌沸石类唑基骨架材料的制备
将5 mmol的Zn(NO3)2·6H2O和40 mmol的2-甲基咪唑溶于200mL甲醇中,室温水浴搅拌1h,静置12h;产物用100 mL 甲醇抽滤洗涤,40ºC真空干燥12h,制得含锌沸石类唑基骨架材料。
(b)含锌沸石类唑基骨架材料负载哌嗪复合材料的制备
将1g的含锌沸石类唑基骨架材料置于圆底烧瓶中,加入35ml的无水正己烷,超声分散,氮气保护。在搅拌的同时,加入哌嗪1.55g。氮气保护下,90℃回流中速搅拌24h。将产品抽滤,并用正己烷浸渍-洗涤-抽滤(50mL*2)以去除未反应的哌嗪,常温真空干燥去掉正己烷,即制得产品。
对比例1
将5 mmol的Zn(NO3)2·6H2O和40 mmol的2-甲基咪唑溶于200mL甲醇中,室温水浴搅拌1h,静置12h;产物用100 mL 甲醇抽滤洗涤,40ºC真空干燥12h,制得含锌沸石类唑基骨架材料。
对比例2
(a)含锌沸石类唑基骨架材料的制备
将5 mmol的Zn(NO3)2•6H2O和40 mmol的2-甲基咪唑溶于200mL甲醇中,室温水浴搅拌1h,静置12h;产物用100 mL 甲醇抽滤洗涤,40ºC真空干燥12h,制得含锌沸石类唑基骨架材料。
(b)含锌沸石类唑基骨架材料负载乙二胺复合材料的制备
将1g的含锌沸石类唑基骨架材料置于圆底烧瓶中,加入35ml的无水正己烷,超声分散,氮气保护。在搅拌的同时,加入乙二胺1.20mL。氮气保护下,回流中速搅拌24h。将产品抽滤,并用正己烷浸渍-洗涤-抽滤(50mL*2)以去除未反应的乙二胺,常温真空干燥去掉正己烷,即制得产品。
对比例3
(a)含锌沸石类唑基骨架材料的制备
将5 mmol的Zn(NO3)2·6H2O和40 mmol的2-甲基咪唑溶于200mL甲醇中,室温水浴搅拌1h,静置12h;产物用100 mL 甲醇抽滤洗涤,40ºC真空干燥12h,制得含锌沸石类唑基骨架材料。
(b)含锌沸石类唑基骨架材料负载N,N-二甲基乙二胺复合材料的制备
将1g的含锌沸石类唑基骨架材料置于圆底烧瓶中,加入35ml的无水正己烷,超声分散,氮气保护。在搅拌的同时,加入N,N-二甲基乙二胺1.97mL。氮气保护下,回流中速搅拌24h。将产品抽滤,并用正己烷浸渍-洗涤-抽滤(50mL*2)以去除未反应的N,N-二甲基乙二胺,常温真空干燥去掉正己烷,即制得产品。
实施例1和对比例1的X射线粉末衍射谱图如图2所示。对于对比例1,主要的衍射峰与SOD型沸石结构相符合[Science, 2008, 319, 939.]。
实施例1的X射线衍射谱图衍射峰与对比例1基本重合,这表明:1)本发明所采用的哌嗪负载实验方法并没有对复合材料中金属唑基框架材料晶体结构构成影响;2)复合材料以对比例1的含锌沸石类唑基骨架材料为基础。
根据298 K下CO2的等温吸附曲线(如图3所示),得出实施例1、对比例1、对比例2和对比例3在1 atm下的CO2吸附量分别为1.32mmol/g、0.98mmol/g、1.03mmol/g和1.05mmol/g。通过计算可知,实施例1相比于对比例1,298 K和1 atm条件下的CO2吸附性能提高了34.7%;对比例2相比于对比例1,298 K和1 atm条件下的CO2吸附性能提高了5.1%;对比例3相比于对比例1,298 K和1 atm条件下的CO2吸附性能提高了7.1%。据此可知:1)哌嗪的加入明显提高了ZIF-8在常温常压下的二氧化碳吸附性能;2)哌嗪的加入,相比于同类的碱性含氮小分子-乙二胺和N,N-二甲基乙二胺,其对ZIF-8常温常压下二氧化碳吸附性能的提升更为显著。

Claims (4)

1.一种提高含锌沸石类唑基骨架材料CO2吸附性能的方法,其特征在于,通过如下步骤实现:
1)将含锌沸石类唑基骨架材料超声分散于无水正己烷中,并施加氮气保护;
2)在步骤(1)所述分散液中加入哌嗪,保持磁力搅拌,回流反应;
3)步骤(2)所述反应结束后,对反应液抽滤,将固体产物加入无水正己烷浸渍,抽滤;
4)重复步骤(3),将固体产物常温真空干燥,得到产品;
步骤1)中所述含锌沸石类唑基骨架材料为ZIF-8。
2.如权利要求1所述的提高含锌沸石类唑基骨架材料CO2吸附性能的方法,其特征在于,ZIF-8的BET比表面积在1000~1200m2/g。
3.如权利要求1所述的提高含锌沸石类唑基骨架材料CO2吸附性能的方法,其特征在于,步骤1)中按照每30~50mL无水正己烷加入1克含锌沸石类唑基骨架材料的比例进行超声分散。
4.如权利要求1所述的提高含锌沸石类唑基骨架材料CO2吸附性能的方法,其特征在于,步骤2)中哌嗪与含锌沸石类唑基骨架材料中不饱和锌离子的摩尔比为5~10:1。
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