CN112480132A - 一种基于Salen结构共价有机骨架材料的制备与用途 - Google Patents
一种基于Salen结构共价有机骨架材料的制备与用途 Download PDFInfo
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Abstract
Description
技术领域
本发明属于共价有机骨架材料领域,具体涉及一种基于Salen结构共价有机骨架材料的制备以及其在光催化气固二氧化碳还原中的应用。
背景技术
近年来,化石燃料作为主要能源被迅速消耗的同时也释放出大量的二氧化碳,不断地消耗不可再生能源造成的环境污染和温室效应已成为全球性问题。可见光驱动将二氧化碳转化为燃料前体(一氧化碳,甲酸等),而可行的燃料(甲烷,乙醇等)代替化石能源可能是未来重要的绿色环保措施和可持续发展手段。因此,开发稳定环保的光催化剂已成为近些年的热点研究方向。
二维共价有机骨架材料是典型的多孔晶体材料,它是具有强π-π堆积特性并通过强共价键连接的刚性骨架。由于其稳定的化学结构,强大的可见光吸收能力和出色的电子传输能力,它在许多领域(例如储能,催化反应和电化学)中发挥着重要作用。合理设计共价有机框架材料的结构可以对特定反应起到关键作用。最有特色的孔隙率和可见光吸收能力将共价有机框架材料的应用扩展到了光催化二氧化碳还原方向。最近,一些二维共价有机骨架材料已被应用于将金属离子安装到框架上以进行二氧化碳的光还原,例如具有卟啉和联吡啶单元的共价有机框架结构。迄今为止的光催化二氧化碳还原多为气液两相的催化反应,而气固两项的催化反应更接近于实际应用。但是目前气固光催化二氧化碳还原仍然处于初级阶段。
发明内容
本发明的目的在于提供一种基于Salen结构共价有机骨架材料的制备方法和在光催化气固二氧化碳还原中的应用。
本发明采用的技术方案为:
上面所述的基于Salen结构共价有机骨架材料的制备方法,其特征为包括以下步骤:(1)将1,3,5-三嗪-2,4,6-三(4’-羟基-5’-甲酰基)苯、乙二胺、二甲基亚砜和乙醇依次加入到一根Pyrex管中,超声1小时后加入乙酸水溶液,并进行三次液氮冷冻脱气操作以实现反应体系的真空无氧条件;将经过脱气操作的Pyrex管自然解冻后放入的烘箱中120~150℃加热进行反应,72~120小时后关闭烘箱,使其自然冷却至室温。
(2)过滤步骤(1)中得到的粗产物,并用N,N-二甲基甲酰胺和乙醇多次洗涤至滤液为无色。分别使用甲醇和丙酮进行溶剂交换,在100~150℃真空干燥箱中保持24~48小时蒸发溶剂后,得到黄色粉末状的基于Salen结构的共价有机框架材料。
步骤(1)中称取物质的量比为2:3~3:2的1,3,5-三嗪-2,4,6-三(4’-羟基-5’-甲酰基)苯与乙二胺至真空管中。
步骤(1)中取摩尔比为1:2~2:1的二甲基亚砜和乙醇于管中。
步骤(1)中所述的乙酸的物质的量的浓度为5-6mol L-1,加入的乙酸的体积为0.3~0.5mL。
本发明的有益效果为:
基于Salen结构共价有机骨架材料,由于材料结构的独特性导致其可作为光催化剂进行气固光催化反应,将二氧化碳还原为一氧化碳。
附图说明:
图1本发明具体实施例1的合成路线图;
图2本发明具体实施例1的X射线粉末衍射图;
图3本发明具体实施例1的红外光谱图;
图4本发明具体实施例1的光催化气固二氧化碳还原性能图。
具体实施方式:
下面结合结合实施例对本发明作进一步详细阐述:
上面所述的基于Salen结构共价有机骨架材料的制备方法,其特征为包括以下步骤:(1)将1,3,5-三嗪-2,4,6-三(4’-羟基-5’-甲酰基)苯、乙二胺、二甲基亚砜和乙醇依次加入到一根Pyrex管中,超声1小时后加入乙酸水溶液,并进行三次液氮冷冻脱气操作以实现反应体系的真空无氧条件;将经过脱气操作的Pyrex管自然解冻后放入的烘箱中120~150℃加热进行反应,72~120小时后关闭烘箱,使其自然冷却至室温。
(2)过滤步骤(1)中得到的粗产物,并用N,N-二甲基甲酰胺和乙醇多次洗涤至滤液为无色。分别使用甲醇和丙酮进行溶剂交换,在100~150℃真空干燥箱中保持24~48小时蒸发溶剂后,得到黄色粉末状的基于Salen结构的共价有机框架材料。
步骤(1)中称取物质的量比为2:3~3:2的1,3,5-三嗪-2,4,6-三(4’-羟基-5’-甲酰基)苯与乙二胺至真空管中。
步骤(1)中取摩尔比为1:2~2:1的二甲基亚砜和乙醇于管中。
步骤(1)中所述的乙酸的物质的量的浓度为5-6mol L-1,加入的乙酸的体积为0.3~0.5mL。
本发明在如下实施例中更详细地叙述,但实施例不构成对本发明的限制。
具体实施例:
将0.02205g的1,3,5-三嗪-2,4,6-三(4’-羟基-5’-甲酰基)苯,0.0045g的乙二胺,1.5ml二甲基亚砜和1.5ml乙醇依次加入到Pyrex管中,常温超声一小时后使用移液枪加入0.5ml物质的量浓度为5M的乙酸水溶液,并进行三次液氮冷冻脱气操作以实现反应体系的真空无氧条件。将经过脱气操作的Pyrex管自然解冻后放入的烘箱中120℃加热进行反应,72小时后关闭烘箱,使其自然冷却至室温。过滤固体产物用N,N-二甲基甲酰胺和乙醇多次洗涤至滤液为无色。使用丙酮溶剂交换后将固体粉末置于100℃真空干燥箱中保持48小时蒸发溶剂,得到0.021g基于Salen结构共价有机骨架材料。
其产物XRD及按AA堆积模拟的产物粉末XRD衍射图谱如图2。在3.2°、5.7°、6.8°、9°和26°处的峰分别对应100晶面、120晶面、220晶面、130晶面和001晶面。从图可见,实验图谱与模拟图谱的峰型完全吻合,说明得到的产物即为基于Salen结构共价有机骨架材料。其红外图谱如图3所示,从图可见所得产物在1630cm-1附近处有很强大吸收,对应于C=N,说明两种单体发生了缩合反应。
其产物的光催化气固二氧化碳还原性能测试图如图4,将0.010g基于Salen结构共价有机骨架材料制成均匀的膜置于反应器底部,持续通入纯二氧化碳一段时间后开启光源进行光催化反应,其还原产物一氧化碳5小时的产量高达1036.9μmol g-1,平均每小时207.38μmol g-1。
Claims (6)
2.权利要求1中的基于Salen结构共价有机骨架材料制备方法,其特征为包括以下步骤:
(1) 将1,3,5-三嗪-2,4,6-三(4’-羟基-5’-甲酰基)苯、乙二胺、二甲基亚砜和乙醇依次加入到一根Pyrex管中,超声1小时后加入乙酸水溶液,并进行三次液氮冷冻脱气操作以实现反应体系的真空无氧条件;将经过脱气操作的Pyrex管自然解冻后放入的烘箱中120~150℃加热进行反应,72~120小时后关闭烘箱,使其自然冷却至室温;
(2) 过滤步骤(1)中得到的粗产物,并用N,N-二甲基甲酰胺和乙醇多次洗涤至滤液为无色,分别使用甲醇和丙酮进行溶剂交换,在100~150℃真空干燥箱中保持24~48小时蒸发溶剂后,得到黄色粉末状的基于Salen结构的共价有机框架材料。
3.根据权利要求2所述的基于Salen结构共价有机骨架材料的制备方法,其特征在于,步骤(1)中称取物质的量比为2:3~3:2的1,3,5-三嗪-2,4,6-三(4’-羟基-5’-甲酰基)苯与乙二胺至真空管中。
4.根据权利要求2所述的基于Salen结构共价有机骨架材料的制备方法,其特征在于,步骤(1)中取摩尔比为1:2~2:1的二甲基亚砜和乙醇于管中。
5.根据权利要求2所述的基于Salen结构共价有机骨架材料的制备方法,其特征在于,步骤(1)中所述的乙酸的物质的量的浓度为5-6 mol L-1,加入的乙酸的体积为0.3~0.5mL。
6.根据权利要求(1)所述的基于Salen结构共价有机骨架材料,由于材料结构的独特性导致其可作为光催化剂进行气固光催化反应,将二氧化碳还原为一氧化碳。
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CN115028789A (zh) * | 2022-06-10 | 2022-09-09 | 哈尔滨理工大学 | 一种含有Salen基团共价有机框架材料的制备与用途 |
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CN115028789A (zh) * | 2022-06-10 | 2022-09-09 | 哈尔滨理工大学 | 一种含有Salen基团共价有机框架材料的制备与用途 |
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