CN114591477B - 亚胺连接的二苯并噻吩砜基共价有机框架材料的制备和应用 - Google Patents
亚胺连接的二苯并噻吩砜基共价有机框架材料的制备和应用 Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
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Abstract
本发明公开了一种亚胺连接的二苯并噻吩砜基共价有机框架材料及其制备方法和应用,属于材料制备领域,其通过将苯并[1,2‑b:3,4‑b′:5,6‑b′]三噻吩‑2,5,8‑三醛与3,7‑二氨基二苯并[b,d]噻吩‑5,5‑二氧化物加入到有机混合溶液中,经液氮浴中冷冻‑解冻及循环脱气3次,再真空封管后进行反应,以最终得到所述亚胺连接的二苯并噻吩砜基共价有机框架材料。本发明所得共价有机框架材料具有良好的光催化整体水分解活性,在光催化领域具有潜在的应用价值。
Description
技术领域
本发明属于材料制备及光催化领域,具体涉及一种亚胺连接的二苯并噻吩砜基COF的制备方法及其在光催化整体水分解中的应用。
背景技术
近年来,由于现代工业的快速发展,粗放式的经济发展模式,导致大量化石燃料被开发和利用,使人们面临严重的资源短缺和环境污染等问题,寻找、开发和利用新型绿色能源已成为当前科学研究的热点课题之一。太阳能作为一种绿色无污染、用之不尽的能源,被认为是最具有吸引力的替代能源。利用太阳能通过光催化剂将水分解成氢气和氧气已成为生产清洁和可再生氢能源以解决全球能源和环境问题的有前景的方法。为此,光催化剂的带隙大于1.23 eV 是一个基本要求,这是标准条件下一个水分子转化为H 2和1/2 O 2的每个电子转移的自由能变化。同时,导带最小值(CBM)位置应充分高于质子的还原电位(H +/H2),而价带最大值(VBM)位置应充分低于水的氧化电位(O2/H2O),以提供足够的动力学过电势来驱动水的还原和氧化。
传统的无机半导体、金属配合物、染料等由于其独特的氧化还原性能已经被人们广泛研究,但其存在分离困难、难以回收等缺点。金属有机骨架化合物(MOFs)虽然在非均相光催化领域表现出优异的性能,但MOFs大多是通过配位键连接而成,稳定性较弱。因此开发具有高比表面积、结构可调且具有稳定性强的高效光催化剂具有重要的现实及理论意义。
共价有机框架(COFs)是一类由有机构筑单元通过可逆共价键连接而成、具有结晶性和周期性的多孔材料,其具有高比表面积、低密度、结构精确可调等特点,其长程有序的孔道为小分子物质吸附、扩散、反应提供了理想的环境,π-π堆积的柱状芳基结构能够促进光生电子-空穴的分离、扩散、迁移,这些特点使COFs材料成为非均相光催化剂的潜在候选者。在过去的几十年中,一大类二维COF已被证明可用作光催化水分解的催化剂。然而,尽管它们中的一些具有覆盖水氧化和还原电位的带边缘,但由于驱动力不足,它们通常仅能触发光催化水分解中的半反应,即析氢反应(HER)或析氧反应(OER)由辐照诱导的电子或空穴提供。
发明内容
本发明的目的在于通过溶剂热法合成一种亚胺连接的二苯噻吩砜基共价有机框架材料,其可用于光催化整体水分解,这不仅对基于二苯并噻吩砜有机半导体的进一步研究有着推动作用,还为光催化机理的理解提供了理论基础。
为实现上述目的,本发明采用如下技术方案:
一种亚胺连接的二苯并噻吩砜基共价有机框架材料,其是将苯并[1,2-b:3,4-b′:5,6-b′]三噻吩-2,5,8-三醛和3,7-二氨基二苯并[b,d]噻吩-5,5-二氧化物加入到邻二氯苯/1,4-二氧六环的混合溶剂中,并加入醋酸溶液,在液氮浴中冷冻-解冻及循环脱气3次,再真空封管后于120 ℃反应3天制得。
其中,所用苯并[1,2-b:3,4-b′:5,6-b′]三噻吩-2,5,8-三醛和3,7-二氨基二苯并[b,d]噻吩-5,5-二氧化物的摩尔比为2:3。
所用邻二氯苯、1,4-二氧六环和醋酸溶液的体积比为5:5:1。所用醋酸溶液的浓度为6 mol/L。
所得亚胺连接的二苯并噻吩砜基共价有机框架材料可用于光催化整体水分解,其具体应用方法是以Pt离子为助催化剂,Co离子为共助催化剂,在不添加任何牺牲剂的情况下,利用所述亚胺连接的二苯并噻吩砜基共价有机框架材料在可见光条件下、纯水体系中实现光催化整体水分解。
本发明的显著优点在于:
1)本发明使用苯并[1,2-b:3,4-b′:5,6-b′]三噻吩-2,5,8-三醛和3,7-二氨基二苯并[b,d]噻吩-5,5-二氧化物为原料,通过溶剂热法得到一种亚胺连接的二苯并噻吩基共价有机框架材料,所得材料具有杂原子和较多的微孔结构以及二维共轭结构,有利于电子和空穴的传输,在光催化整体水分解反应中表现出良好的活性。
2)本发明合成方法所用到的设备和化学试剂易于获取,工艺操作简便,工艺条件简单,适用性强,工业应用价值高,易于推广利用。
附图说明
图1为本发明合成亚胺连接的二苯并噻吩砜基共价有机框架材料的反应示意图;
图2为通过实验和拟合得到的亚胺连接的二苯并噻吩砜基共价有机框架材料的X射线粉末衍射图;由图中实验与拟合结果吻合表明该共价有机框架材料的成功合成;
图3为实施例合成的亚胺连接的二苯并噻吩砜基共价有机框架材料的傅里叶变换红外光谱图;由图中C=N特征吸收峰的出现进一步表明材料的成功合成;
图4为实施例合成的亚胺连接的二苯并噻吩砜基共价有机框架材料的SEM图;
图5为实施例合成的亚胺连接的二苯并噻吩砜基共价有机框架材料的紫外可见吸收光图谱;由图中可见,该共价有机框架材料的吸光范围几乎覆盖了整个紫外可见光谱区域;
图6为实施例合成的亚胺连接的二苯并噻吩砜基共价有机框架材料在可见光条件下光催化分解水产生氢气和氧气的产量随时间变化的情况图;由图中可见,每小时生成的氢气和氧气的产量比接近2:1,其中第1小时的氢气和氧气的产量较高,之后趋于稳定。
具体实施方式
为了使本发明的目的、技术方案及优势更加清楚明白便于理解,以下结合实施例,对本发明进行进一步详细说明。可以理解,此处所描述的具体实施仅用于解释本发明,并不用于限定本发明。
实施例
将苯并[1,2-b:3,4-b′:5,6-b′]三噻吩-2,5,8-三醛(9.9 mg,0.03 mmol)、3,7-二氨基二苯并[b,d]噻吩-5,5-二氧化物(11.0 mg,0.045 mmol)和1 mL邻二氯苯/1,4-二氧六环(体积比1:1)混合溶液置于Pyrex管中,超声10分钟得到均匀的分散液后加入醋酸溶液(0.1 mL,6 mol/L),在液氮浴中冷冻-解冻及循环脱气3次,真空封管后于120 ℃反应3天,待冷却至室温,抽滤收集固体,用甲醇、N,N-二甲基甲酰胺和丙酮分别洗涤三次,得到的粉末在60 ℃真空干燥过夜,得到DW-COF的黄色粉末。
应用例
称取30 mg实施例1制备的DW-COF,加入3 mL甲醇和1wt% Pt,超声10分钟,旋蒸30min,再加入3mL冰甲醇和1mL 1.5M NaBH4,置于磁力搅拌器上搅拌6 h,抽滤收集固体,用去离子水多次洗涤,得到的粉末在60 ℃真空干燥过夜,得到样品1wt% Pt@DW-COF。
称取上述步骤获得的样品10 mg,充分研磨,加入3wt% Co(六水合氯化钴,1.2mg)及50 mL水,超声5分钟后将其投入石英玻璃反应器中。反应器抽真空后,在290~398 K下用300 W氙灯模拟可见光(λ≥420nm)照射,在光催化反应过程中,每间隔1小时用气相色谱检测光催化反应后的气体成分,并重新抽真空,继续于290~398 K下用300 W氙灯模拟可见光(λ≥420nm)照射,结果见图6。
尽管本发明的内容已经通过上述优选实施例作了详细介绍,但应当认识到上述的描述不应该被认为是对本发明的限制。在本领域技术人员阅读了上述内容后,对于本发明的多种修改和替代都是显而易见的。因此,本发明的保护范围应由所附的权利要求来限定。
Claims (4)
1.一种亚胺连接的二苯并噻吩砜基共价有机框架材料光催化整体水分解中的应用,其特征在于:所述二苯并噻吩砜基共价有机框架材料是将苯并[1,2-b:3,4-b′:5,6-b′]三噻吩-2,5,8-三醛和3,7-二氨基二苯并[b,d]噻吩-5,5-二氧化物加入到邻二氯苯/1,4-二氧六环的混合溶剂中,并加入醋酸溶液,在液氮浴中冷冻-解冻及循环脱气3次,再真空封管后进行反应而得到的;
其具体应用方法是以Pt离子为助催化剂,Co离子为共助催化剂,在不添加任何牺牲剂的情况下,利用所述亚胺连接的二苯并噻吩砜基共价有机框架材料在可见光条件下、纯水体系中实现光催化整体水分解。
2.根据权利要求1所述的应用,其特征在于:所用苯并[1,2-b:3,4-b′:5,6-b′]三噻吩-2,5,8-三醛和3,7-二氨基二苯并[b,d]噻吩-5,5-二氧化物的摩尔比为2:3。
3. 根据权利要求1所述的应用,其特征在于:所用邻二氯苯、1,4-二氧六环和醋酸溶液的体积比为5:5:1;所述醋酸溶液的浓度为6 mol/L。
4. 根据权利要求1所述的应用,其特征在于:所述反应的温度为120 ℃,时间为3天。
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