CN112756013B - 一种可用于光催化水净化的共价有机骨架/杨柳絮复合催化剂的制备方法 - Google Patents
一种可用于光催化水净化的共价有机骨架/杨柳絮复合催化剂的制备方法 Download PDFInfo
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Abstract
一种可用于光催化水净化的共价有机骨架/杨柳絮复合催化剂的制备方法,属于功能材料领域。以自然界的杨/柳絮为基底,在不使用任何催化剂的条件下,利用三聚氰胺与三甲酰间苯三酚单体,经溶剂热偶联处理,即可在杨/柳絮表面负载含有三嗪的多孔共价有机骨架(COF),所得的复合结构在光催化水净化领域具有较好的应用前景。
Description
技术领域
本发明涉及一种可用于光催化水净化的共价有机骨架(COF)负载于杨(柳) 絮的制备方法,属于功能材料领域。
技术背景
当前,寻找新型高效的污水处理材料尤为迫切。共价有机骨架(COF)是一类新兴的多孔晶体材料,基于可逆化学反应将功能单元以共价键的形式连接成高度有序的二维层叠层结构或特定的三维拓扑结构,由设计分子构件构筑而成,这些构件通过共价键周期性地连接和扩展。它们具有高稳定性,有序开孔结构和易于功能化设计的特点。COF的合成通常在溶剂热体系中进行,采用单一或混合溶剂以溶解部分单体,通过高温及低压条件下长时间反应获得COF微晶聚集体,其间贯穿了包括聚合、结晶、组装等多个过程。开发均一可调的COF 纳米材料,不仅是多孔有机高分子领域中一个较难解决的课题,而且也会推动 COF在更多领域的应用探索。由于其内置的光活性和纳米级规整性,COF已成为吸收自然光进行催化作用的可行的平台。之前的研究集中在于COF孔中的物理吸附,而通过COF与大尺寸、易分离的载体构建复合材料,一方面保证COF 材料的光活性,另一方面也便于回收,避免COF在反应过程中的聚集行为。
杨/柳絮呈纤维管状,柔软质轻,易收集,具有较大的比表面积,表面富含有机功能基团,易于与优选的光催化材料表面键合而形成复合材料,因此可探索出新型高效的污水处理净水材料。
通过此种方法合成的COF/杨(柳)絮复合纳米结构形貌均一,分散性好,便于回收,在室温下能够稳定存在,经有机半导体复合,开发出了可吸收太阳光的吸附-催化复合材料,Cr(VI)等进行吸附-太阳光降解,经协同作用提高了净化效率,在水处理领域有较好的应用前景。
发明内容
本发明的目的是提供一种可用于光催化水净化的共价有机骨架(COF)负载于杨絮或/和柳絮的催化剂的制备方法,利于批量制备在水处理领域和催化领域具有广泛应用前景的有机复合纳米材料,可将杨(柳)絮变废为宝,大大降低成本,提高净水效率,实际应用价值重大。
本发明的目的通过以下技术方案予以实现:
(1)首先将杨絮或/和柳絮分散于稀硫酸水溶液中酸化处理,磁力搅拌,实现表面酸化功能化,而后固液分离,烘干;其中所述稀硫酸的体积百分比浓度为5%-20%;
(2)将表面酸化处理后的杨絮或/和柳絮分散于有机溶剂二甲基亚砜(DMSO) 中,然后往前述悬浮液中加入三聚氰胺和三甲酰间苯三酚单体,与杨絮或/和柳絮发生反应,杨絮或/和柳絮表面被反应制得的三嗪COF覆盖,而后固液分离,回收的粉末用蒸馏水洗涤,干燥,收集,即可得到三嗪COF改性的杨絮或/和柳絮复合材料;其中反应温度为120-200℃,反应时间为18-28小时;杨絮或/和柳絮、三聚氰胺与三甲酰间苯三酚的质量关系为(0.05-0.1):(0.03-0.06): (0.05-0.10);
复合催化剂的应用,用于光催化还原Cr(VI)为Cr(III);以Cr(VI)光催化还原为探针反应验证复合结构的光催化效果:取20mg复合结构分散于60 mL 120mg/L的重铬酸钾溶液中,添加20mg柠檬酸为空穴捕获剂,在300W 氙灯(模太阳光拟)下光照15分钟,即可完全将Cr(VI)光催化还原为Cr(III)。
本发明以杨(柳)絮为原料,经三聚氰胺和三甲酰间苯三酚的二甲基亚砜 (DMSO)溶剂热处理,能够可控制备三嗪COF负载的杨柳絮复合结构,该方法证实通过此方法改性杨(柳)絮的可操作性。
本发明的有益效果是:本发明的制备方法所得的产品可重复性好,操作简单,成本低,能够变废为宝。所得的三嗪COF负载的杨(柳)絮纳米结构在光催化领域具有较好的应用前景。
附图说明
图1:改性后的COF/杨(柳)絮照片;
图2:原始杨(柳)絮以及改性后的COF/杨(柳)絮的扫描电镜图片;
图3:实施例1改性后模拟太阳光下Cr(VI)的光催化还原图片(Cr(VI)浓度随时间变化图);
具体实施方式
下面结合实施例对本发明作进一步说明,但本发明并不限于以下实施例。
实施例1
1、首先将杨(柳)絮分散于稀硫酸水溶液中酸化处理,磁力搅拌,实现表面酸化功能化,而后固液分离,60℃烘干;其中所述稀硫酸的浓度为5%(体积百分比)。
2、将表面酸化处理后的杨(柳)絮分散于有机溶剂二甲基亚砜(DMSO)中,然后往前述悬浮液中加入三聚氰胺和三甲酰间苯三酚单体,与杨(柳)絮发生反应,杨(柳)絮表面被反应制得的三嗪COF覆盖,而后固液分离,回收的粉末用蒸馏水洗涤,干燥,收集,即可得到三嗪COF改性的杨(柳)絮复合材料。其中溶剂热温度为120℃,水热处理时间为18小时;杨(柳)絮、三聚氰胺与三甲酰间苯三酚的质量关系为0.05g:0.03g:0.05g;添加二甲基亚砜10mL。
实施例2
1、首先将杨(柳)絮分散于稀硫酸水溶液中酸化处理,磁力搅拌,实现表面酸化功能化,而后固液分离,60℃烘干;其中所述稀硫酸的浓度为20%(体积百分比)。
2、将表面酸化处理后的杨(柳)絮分散于有机溶剂二甲基亚砜(DMSO)中,然后往前述悬浮液中加入三聚氰胺和三甲酰间苯三酚单体,与杨(柳)絮发生反应,杨(柳)絮表面被反应制得的三嗪COF覆盖,而后固液分离,回收的粉末用蒸馏水洗涤,干燥,收集,即可得到三嗪COF改性的杨(柳)絮复合材料。其中溶剂热温度为200℃,水热处理时间为28小时;杨(柳)絮、三聚氰胺与三甲酰间苯三酚的质量关系为0.1g:0.06g:0.10g;添加二甲基亚砜15mL。
实施例3
1、首先将杨(柳)絮分散于稀硫酸水溶液中酸化处理,磁力搅拌,实现表面酸化功能化,而后固液分离,60℃烘干;其中所述稀硫酸的浓度为15%(体积百分比)。
2、将表面酸化处理后的杨(柳)絮分散于有机溶剂二甲基亚砜(DMSO)中,然后往前述悬浮液中加入三聚氰胺和三甲酰间苯三酚单体,与杨(柳)絮发生反应,杨(柳)絮表面被反应制得的三嗪COF覆盖,而后固液分离,回收的粉末用蒸馏水洗涤,干燥,收集,即可得到三嗪COF改性的杨(柳)絮复合材料。其中溶剂热温度为180℃,水热处理时间为20小时;杨(柳)絮、三聚氰胺与三甲酰间苯三酚的质量关系为0.07g:0.04g:0.067g;添加二甲基亚砜12mL。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所做的任何修改,等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (1)
1.一种用于光催化水净化的共价有机骨架/杨柳絮复合催化剂的应用,用于光催化还原Cr VI为Cr III,其中共价有机骨架/杨柳絮复合催化剂的制备方法包括以下步骤:
(1)首先将杨絮或/和柳絮分散于稀硫酸水溶液中酸化处理,磁力搅拌,实现表面酸化功能化,而后固液分离,烘干;其中所述稀硫酸的体积百分比浓度为5%-20%;(2)将表面酸化处理后的杨絮或/和柳絮分散于有机溶剂二甲基亚砜DMSO中,然后往前述悬浮液中加入三聚氰胺和三甲酰间苯三酚单体,与杨絮或/和柳絮发生溶剂热反应,杨絮或/和柳絮表面被反应制得的三嗪COF覆盖,而后固液分离,回收的粉末用蒸馏水洗涤,干燥,收集,即得到三嗪COF改性的杨絮或/和柳絮复合材料;其中反应温度为120-200 ℃,反应时间为18-28小时;杨絮或/和柳絮、三聚氰胺与三甲酰间苯三酚的质量关系为(0.05-0.1): (0.03-0.06):(0.05-0.10)。
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