CN109289888B - 一种硼掺杂多孔氮化碳材料的制备方法 - Google Patents
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Abstract
本发明公开了一种硼掺杂多孔氮化碳材料的制备方法,属于光催化材料的合成技术领域。本发明的技术方案要点为:加热三聚氰胺获得石墨相氮化碳,将其与氯化钠、氯化钾和氨硼烷混合研磨后置于空气气氛下加热反应,利用融盐和空气的造孔作用和氨硼烷的热解得到硼掺杂多孔氮化碳材料。本发明制得的硼掺杂多孔氮化碳材料制备方案工序简单,易于扩大生产,具有较大的比表面积和表面特异性吸附作用,表现出良好的光催化性能。
Description
技术领域
本发明属于光催化材料的合成技术领域,具体涉及一种硼掺杂多孔氮化碳材料的制备方法。
背景技术
太阳能具有廉价、无污染等特点,且取之不尽用之不竭,因此成为最具开发潜力的新能源之一。石墨相氮化碳作为经典的非金属半导体,具有可调的带隙、良好的热稳定性和化学稳定性、成本低廉及制作方法简单等优点,成为目前光催化材料领域关注的热点。公开号为CN108404960A的专利公开了一种硫铟锌金氮化碳二维层状复合光催化剂的制备方法,该工艺通过将金胶体溶液等试剂与石墨相氮化碳混合后进行吸附,经水热反应后获得硫铟锌金氮化碳二维层状复合光催化剂,该方法虽然操作简便,但是由于试剂成本高,不宜商业化推广应用。公开号为CN108380237A的专利公开了氮缺陷石墨相氮化碳纳米片光催化剂及其制备方法与应用,该工艺通过对三种富氮有机物分段高温煅烧,并在惰性气体环境下获得氮缺陷石墨相氮化碳的纳米材料,该过程复杂,环保性较低,不宜规模化生产。公开号为CN108246339A的专利公开了一种共价有机骨架/氮化碳复合材料的制备方法及其应用,该工艺通过苯二胺和三甲酰基间苯三酚合成共价有机骨架材料,进而与氮化碳反应获得目标产物,该方法获得的材料虽然拥有高氮掺杂量和丰富的孔隙结构,但是由于使用的有机试剂具有较高毒性,故不具有绿色环保等特性。
石墨相氮化碳因具有独特的结构而表现出优异的物理特性和化学特性,在光催化领域具有广泛的应用前景。对石墨相氮化碳进行表面修饰,可以在保证其自身特性的同时,提高待降解分子在其表面的吸附和活化过程,有效降低其催化电位。对石墨相氮化碳进行硼掺杂,利用硼杂原子的缺电子特性,实现待降解分子在其表面的吸附和活化,进而提高光催化活性。
发明内容
本发明解决的技术问题是提供了一种成本低廉且合成过程简单的硼掺杂多孔氮化碳材料的制备方法,该方法制得的硼掺杂多孔氮化碳材料因造孔而使其获得较大的比表面积并且提供了良好的电子传输孔道,另外该方法制得的硼掺杂多孔氮化碳材料因掺入了硼元素而获得了合适的带隙,从而提高了对太阳光的利用率。
本发明为解决上述技术问题采用如下技术方案,一种硼掺杂多孔氮化碳材料的制备方法,其特征在于具体步骤为:
步骤S1:将三聚氰胺充分研磨后装入瓷坩埚中,密封后放入马弗炉中,以5℃/min的升温速率升温至550℃并保持2小时,冷却至室温后用沸水反复冲洗得到纯净的石墨相氮化碳;
步骤S2:将步骤S1得到的石墨相氮化碳与氯化钠、氯化钾和氨硼烷研磨混合后置于瓷舟内,再将瓷舟置于空气气氛的管式炉内,于750℃反应1-5分钟后将产物取出,用热水清洗干净后置于真空干燥箱内干燥得到硼掺杂多孔氮化碳材料。
进一步优选,步骤S2中所述石墨相氮化碳、氯化钠、氯化钾和氨硼烷的投料质量比为2:1:1:1-2。
进一步优选,步骤S2中在空气气氛下一步完成对石墨相氮化碳的造孔与掺硼。
本发明制备步骤简单且反应条件温和,制得的硼掺杂多孔氮化碳材料具有较大的比表面积和吸附活化作用,因而表现出良好的光催化性能,能够用于对待降解染料、二氧化碳等分子进行选择性吸附,在光催化材料领域具有广阔的应用前景。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明,但不应该将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
步骤S1:将三聚氰胺充分研磨后装入瓷坩埚中,密封后放入马弗炉中,以5℃/min的升温速率升温至550℃并保持2小时,冷却至室温后用沸水反复冲洗得到纯净的石墨相氮化碳;
步骤S2:取步骤S1得到的石墨相氮化碳与氯化钠、氯化钾和氨硼烷按2:1:1:1的质量比混合均匀后平铺于瓷舟内,再将该瓷舟置于空气气氛下的管式炉内,于750℃反应1分钟后取出,用热水清洗干净后置于真空干燥箱内干燥得到硼掺杂多孔氮化碳材料。
实施例2
步骤S1:将三聚氰胺充分研磨后装入瓷坩埚中,密封后放入马弗炉中,以5℃/min的升温速率升温至550℃并保持2小时,冷却至室温后用沸水反复冲洗得到纯净的石墨相氮化碳;
步骤S2:取步骤S1得到的石墨相氮化碳与氯化钠、氯化钾和氨硼烷按2:1:1:1.5的质量比混合均匀后平铺于瓷舟内,再将该瓷舟置于空气气氛下的管式炉内,于750℃反应2.5分钟后取出,用热水清洗干净后置于真空干燥箱内干燥得到硼掺杂多孔氮化碳材料。
实施例3
步骤S1:将三聚氰胺充分研磨后装入瓷坩埚中,密封后放入马弗炉中,以5℃/min的升温速率升温至550℃并保持2小时,冷却至室温后用沸水反复冲洗得到纯净的石墨相氮化碳;
步骤S2:取步骤S1得到的石墨相氮化碳与氯化钠、氯化钾和氨硼烷按2:1:1:2的质量比混合均匀后平铺于瓷舟内,再将该瓷舟置于空气气氛下的管式炉内,在750℃反应2.5分钟后取出,用热水清洗干净后置于真空干燥箱内干燥得到硼掺杂多孔氮化碳材料。
实施例4
步骤S1:将三聚氰胺充分研磨后装入瓷坩埚中,密封后放入马弗炉中,以5℃/min的升温速率升温至550℃并保持2小时,冷却至室温后用沸水反复冲洗得到纯净的石墨相氮化碳;
步骤S2:取步骤S1得到的石墨相氮化碳与氯化钠、氯化钾和氨硼烷按2:1:1:1.5的质量比混合均匀后平铺于瓷舟内,再将该瓷舟置于空气气氛下的管式炉内,于750℃反应2.5分钟后取出,用热水清洗干净后置于真空干燥箱内干燥得到硼掺杂多孔氮化碳材料。
实施例5
步骤S1:将三聚氰胺充分研磨后装入瓷坩埚中,密封后放入马弗炉中,以5℃/min的升温速率升温至550℃并保持2小时,冷却至室温后用沸水反复冲洗得到纯净的石墨相氮化碳;
步骤S2:取步骤S1得到的石墨相氮化碳与氯化钠、氯化钾和氨硼烷按2:1:1:1.5的质量比混合均匀后平铺于瓷舟内,再将该瓷舟置于空气气氛下的管式炉内,于750℃反应5分钟后取出,用热水清洗干净后置于真空干燥箱内干燥得到硼掺杂多孔氮化碳材料。
以上实施例描述了本发明的基本原理、主要特征及优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明原理的范围下,本发明还会有各种变化和改进,这些变化和改进均落入本发明保护的范围内。
Claims (3)
1.一种硼掺杂多孔氮化碳材料的制备方法,其特征在于具体步骤为:
步骤S1:将三聚氰胺充分研磨后装入瓷坩埚中,密封后放入马弗炉中,以5℃/min的升温速率升温至550℃并保持2小时,冷却至室温后用沸水反复冲洗得到纯净的石墨相氮化碳;
步骤S2:将步骤S1得到的石墨相氮化碳与氯化钠、氯化钾和氨硼烷研磨混合后置于瓷舟内,再将瓷舟置于空气气氛的管式炉内,于750℃反应1-5分钟后将产物取出,用热水清洗干净后置于真空干燥箱内干燥得到硼掺杂多孔氮化碳材料。
2.根据权利要求1所述的硼掺杂多孔氮化碳材料的制备方法,其特征在于:步骤S2中所述石墨相氮化碳、氯化钠、氯化钾和氨硼烷的投料质量比为2:1:1:1-2。
3.根据权利要求1所述的硼掺杂多孔氮化碳材料的制备方法,其特征在于:步骤S2中在空气气氛下一步完成对石墨相氮化碳的造孔与掺硼。
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