CN108554452B - 一种由尿素可控制备二维有机碳氮的方法 - Google Patents
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Abstract
本发明属于二维有机材料制备技术领域,提供了一种由尿素可控制备二维有机碳氮的方法,包括以下步骤:(1)前驱体制备;(2)有机碳氮材料制备;(3)产物后处理,此外还可以进一步地对得到的有机碳氮材料进行不同形貌的制备。本发明具有简单直接,对环境无毒无害的特点,制备出的二维有机碳氮材料具有极好的光催化性能。
Description
技术领域
本发明涉及一种由尿素可控制备二维有机碳氮的方法,属于二维有机材料制备技术领域。
背景技术
二维材料,可分为无机二维材料和有机二维材料。如无机二维材料有石墨烯,六方氮化硼纳米片和二硫化钼纳米片等,由于它们具有优良的物理和化学性质而引起研究者的广泛关注,研究表明它们在电子、激光、生物、催化、机械等方面具有广阔的应用前景。而有机二维材料,如有机MOF等,它们既有二维材料的物理特性(如导电),也包含有机材料的柔性,具有应用于新型能源材料(如柔性超电)的潜力。近年来,研究者对有机二维材料的研究越来越多,各种新型的二维有机材料被陆续发现,研究表明它们在能源、环保、催化等方面具有很广的应用前景。
提到二维碳氮材料,大家通常想到是二维无机碳氮材料,它已经被应用于了高效光解水制氢、超级电容和锂离子电池等领域。但是,有机的二维碳氮材料目前还没有其他人研究,如果制备出有机的二维碳氮材料,它能够很好地调控下一步无机碳氮材料的形貌。从目前的研究成果可以看出,各种维度的无机碳氮材料具有非常好的光催化解水制氢性能。(见参考文献S.Cao,J.Low,J. Yu,M.Jaroniec,Adv.Mater.2015,27,2150;X.H.Li,J.S.Zhang,X. F.Chen,A.Fischer,A.Thomas,M.Antonietti,and X.C.Wang,Chem.Mater.2011,23,4344;G.G.Liu,T.Wang,H.B.Zhang,X.G.Meng,D.Hao,K. Chang,P.Li,T.Kako andJ.H.Ye,Angew.Chem.Int.Ed.2015,54,13561; Q.H.Liang,Z.Li,X.L.Yu,Z.H.Huang,F.Y.Kang and Q.H.Yang, Adv.Mater.2015,27,4634.)
此外,工业生产的尿素严重过剩,农耕土地用不了大量的尿素,放置过久尿素就会失效,还会污染环境。为了更好的解决这个问题,本发明将会以尿素为研究对象,通过化学反应由尿素制备出一种二维有机碳氮材料,其不仅在研究领域具有较高的研究价值,而且在应用领域也具有较高的研究价值。
发明内容
针对上述问题,本发明提出一种简单、有效地由尿素可控制备二维有机碳氮材料的方法,该方法得到的有机碳氮材料具有高附加值。
本发明提供的一种由尿素可控制备二维有机碳氮的方法包括以下步骤:
(1)前驱体制备:将尿素粉末和蒸馏水按1:50~1:200的比例均匀混合,形成分散溶液,在室温下进行超声磁力搅拌2~60min;
(2)有机碳氮材料制备:将步骤(1)获得的前驱体溶液于高压反应釜中在 100~220℃下,反应6~36小时,然后自然冷却,其中高压反应釜衬里为聚四氟乙烯,外壁为不锈钢;
(3)产物后处理:将步骤(2)所得到产物过滤后,取沉淀依次用无水酒精和蒸馏水冲洗2~5次,直至无杂质泡沫,最后放在50℃~80℃真空干燥中干燥24小时。上述尿素可以替换为三聚氰胺或者双氰胺,或者三者中任意两者的混合物,或者三者的混合物。
另外,上述方法还可以包括步骤(4)有机碳氮材料不同形貌的制备:将步骤(3)所得的有机碳氮材料于真空管式炉中,在氮气保护气氛下,加热到300℃以上,保温0~2.5h。
上述步骤(4)中不同形貌与加热温度和保温时间的对应关系见下表:
表1有机碳氮材料热处理所得形貌与加热温度、保温时间对应表:
本发明所获得的有益效果:
(1)本发明所提供的层状有机碳氮材料的制备方法具有简单直接,对环境无毒无害的特点。
(2)本发明能够通过层状有机碳氮材料的后续热处理工艺可控调节层状有机碳氮材料的形貌。
(3)本发明获得的层状有机碳氮材料的光催化性能优异,其光催化水解制氢产率为1325.1μmol h-1g-1。
附图说明
图1为实施例1所得层状有机碳氮材料的结构示意图。
图2为实施例1所得层状有机碳氮材料与尿素原料的扫描电镜对比图,其中a为尿素原料,b为层状有机碳氮材料。
图3为实施例1所得层状有机碳氮材料的原子力显微镜扫描图。
图4为光催化性能检测。
具体实施方式
实施例1
本实施例由尿素可控制备二维有机碳氮材料,具体步骤如下:
(1)将0.5克尿素粉末分散在30毫升蒸馏水中,超声磁力搅拌60min,形成分散溶液;
(2)将步骤(1)获得的前驱体转移到50毫升的聚四氟乙烯衬里内衬中,然后置于不锈钢高压釜内;
(3)然后将高压釜密封,并保持在100℃的高温下6小时,然后自然冷却到室温;
(4)将产品过滤掉,取沉淀用蒸馏水冲洗几次,最后在80℃真空干燥箱中干燥24小时;
(5)将步骤(4)所得的粉末于真空管式炉中,在氮气保护气氛下,加热到300℃,保温1.5h即得二维有机碳氮材料;该二维有机碳氮材料的分子结构示意图见图1,图2是所得有机碳氮材料与尿素原料的扫描电镜对比图,可以看出颗粒状的尿素反应后得到了堆积层状的二维有机碳氮材料,这种层状结构得到了原子力显微镜(图3)的验证。
实施例2-6
本组实施例与实施例1的不同之处在于:步骤(5)中保温时间如下表所示
表2实施例2-6步骤(5)中保温时间
其中实施例2保温时间为0h,也即实施例2没有步骤(5),实施例1-6所得有机碳氮材料的光催化性能对比见图4,可以看出本组实施例所得有机碳氮材料的光催化能力均比目前使用的C3N4要高,且实施例的光催化性能最高,其制氢产率为1325.1μmol h-1g-1,且从图4d中可以看出实施例1的循环催化能力很好,证明本发明所得的有机碳氮材料具有良好的稳定性。
实施例7
本实施例与实施例1的不同之处在于:步骤(1)中将尿素粉末与蒸馏水的用量分别改为尿素0.3克,蒸馏水30毫升。
实施例8
本实施例与实施例1的不同之处在于:步骤(1)中将蒸馏水改为乙醇溶液,尿素的用量0.5克,蒸馏水25毫升。
实施例9
本实施例与实施例1的不同之处在于:步骤(3)中的超声时间改为0.5小时。
实施例10
本实施例与实施例1的不同之处在于:步骤(4)中高压釜密封并分别保持在150℃,200℃,220℃的高温下反应。
实施例11
本实施例与实施例1的不同之处在于:步骤(4)中高温下反应时间分别为 8h、10h、20h、36h。
Claims (1)
1.一种由尿素可控制备二维有机碳氮的方法,其特征是,包括以下步骤:
(1)将0.5克尿素粉末分散在30毫升蒸馏水中,超声磁力搅拌60min,形成分散溶液;
(2)将步骤(1)获得的前驱体转移到50毫升的聚四氟乙烯衬里内衬中,然后置于不锈钢高压釜内;
(3)然后将高压釜密封,并保持在100℃的高温下6小时,然后自然冷却到室温;
(4)将产品过滤掉,取沉淀用蒸馏水冲洗几次,最后在80℃真空干燥箱中干燥24小时;
(5)将步骤(4)所得的粉末于真空管式炉中,在氮气保护气氛下,加热到300℃,保温1.5h。
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