CN105664835B - 一种有机羧酸辅助批量制备多孔氮化碳材料的方法 - Google Patents
一种有机羧酸辅助批量制备多孔氮化碳材料的方法 Download PDFInfo
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Abstract
本发明涉及一种有机羧酸辅助批量制备多孔氮化碳材料的方法,是采用水热‑煅烧两步法,首先将有机羧酸和三聚氰胺均匀混合,然后在水热条件下反应得到多孔氮化碳水热前驱物,将上述水热前驱物煅烧,得到多孔氮化碳材料。通过改变有机羧酸种类和实验条件,可以实现几种不同结构形貌和比表面积多孔氮化碳材料的可控制备。本方法原料来源丰富、成本低廉、合成工艺简单、易操作、重复性好、可大批量制备。制备的多孔氮化碳材料具有高效的吸附降解有机污染物能力,在环境污染物治理、光催化产氢、药物负载等领域具有广泛的应用前景。
Description
技术领域
本发明涉及一种有机羧酸辅助批量制备多孔氮化碳材料的方法,属材料制备领域。
背景技术
石墨相氮化碳作为一种新型不含金属的半导体材料已引起人们广泛的关注。氮化碳具有类石墨层状结构,层间由范德华力结合,层内由氮和碳两种元素通过杂化形成高度离域的共轭体系,稳定性高。氮化碳作为半导体材料具有适宜的带隙宽度(约为2.7eV),能够吸收大部分可见光,又具有较强的氧化和还原能力。同时,氮化碳对环境和生物体无污染、毒性低。因此,氮化碳在光催化降解环境有机污染物、光催化制氢、荧光材料、杀菌材料等方面具有广泛的应用前景。
通过改进制备技术,控制形貌,进而有效调控氮化碳的性能是人们追求的目标。目前氮化碳的制备方法主要是三聚氰胺煅烧法。该方法主要得到块体材料,无法有效控制形貌、调控性能。多孔氮化碳材料由于具有较高的比表面积成为人们研究的热点。目前主要采用硬模板法制备。如CN103861630 A专利文献公布了一种共聚合改性的石墨相氮化碳空心球可见光催化剂,其氮化碳空心球的合成是以氰胺和有机小分子单体为前驱物、介孔二氧化硅球为模板,通过热聚合和去除模板得到的。Wang等人(J.Mater.Chem.A,2015,3,5126-5131)利用碳酸钙作为模板,制备了多孔氮化碳材料。但硬模板法实验步骤复杂、去除模板所用酸液容易造成污染等限制了其广泛应用。
发明内容
为了克服现有技术的不足,本发明提供了一种有机羧酸辅助批量制备多孔氮化碳材料的方法,是一种将有机羧酸加入三聚氰胺中,通过水热-煅烧两步法可控制备多孔氮化碳材料的方法。
一种有机羧酸辅助批量制备多孔氮化碳材料的方法,其制备步骤如下:
将三聚氰胺和有机羧酸按照质量比1:1-1:20混匀后加入水溶解,其中水与有机羧酸的质量比为1:1;或将三聚氰胺和有机羧酸按照质量比1:1-1:20混匀溶解;将溶解后的混合物于水热反应釜中80-180℃加热1-16h,得到多孔氮化碳水热前驱物;将多孔氮化碳水热前驱物于管式炉中于氮气保护下450-650℃煅烧1-6h,得到多孔氮化碳材料。
所述有机羧酸的种类为乙酸、草酸、苯甲酸或水杨酸;
优选的,所述三聚氰胺和有机羧酸的质量比为1:2-1:10;
优选的,所述溶解后的混合物于水热反应釜中100-180℃加热5-12h。
优选的,所述多孔氮化碳水热前驱物于管式炉中于氮气保护下500-600℃煅烧2-4h。
本发明采用有机羧酸辅助和水热-煅烧两步法技术,通过改变有机羧酸的种类和加入量,可控制备了多种不同形貌结构和比表面积的多孔氮化碳材料。利用有机羧酸分解产生气体的特点,形成多孔结构;通过改变有机碳链或苯环结构调控孔结构的大小。增大了氮化碳材料的比表面积,改善了多相光催化反应中的传质扩散过程,促进了光生载流子的快速分离,显著提高了对有机污染物的降解能力。
附图说明
图1是本发明实施例1中有序层状多孔氮化碳材料的X射线衍射(XRD)图;
从图1中可以发现13.7°和27.6°处出现两个明显的归属于石墨相氮化碳(100)和(002)晶面的XRD衍射峰,证明所制备材料为石墨相氮化碳材料。
图2是本发明实施例1,2,6中不同形貌多孔氮化碳材料的扫描电镜照片(SEM);
其中a图为实施例1中乙酸和三聚氰胺在水溶剂中水热然后煅烧制备的有序层状多孔氮化碳材料;b图为实施例2中乙酸和三聚氰胺在无水条件下水热然后煅烧制备的多孔氮化碳材料;c图为实施例6中苯甲酸和三聚氰胺在水溶剂中水热然后煅烧制备的管状多孔氮化碳材料;
从图2a中可以观察到明显的层状多孔结构;图2b中可以观察到均匀的多孔结构;图2c中可以观察到明显的管状多孔结构。
图3是本发明实施例1中有序层状多孔氮化碳材料的N2吸附脱附曲线与单纯三聚氰胺制备的氮化碳材料的对比图;
图3看出,有序层状多孔氮化碳材料的吸附脱附性能明显优于三聚氰胺制备的氮化碳材料,BET方法计算有序层状多孔氮化碳材料的比表面积为138m2/g,远高于单纯三聚氰胺制备的氮化碳材料的比表面积31m2/g。
图4是本发明实施例1中有序层状多孔氮化碳材料和单纯三聚氰胺制备的氮化碳材料对罗丹明B在太阳光下的催化活性对比图;
图4可以看到,有序层状多孔氮化碳材料对罗丹明B的光催化降解效果远优于纯三聚氰胺制备的氮化碳材料。
具体实施方式:
下面结合附图和具体实施例对本发明的具体内容作进一步详细说明。
本发明中所述有机羧酸的种类可以为乙酸、草酸、苯甲酸或水杨酸,但不限于这几种有机羧酸;本实施例所用有机羧酸均为分析纯。本实施例所使用惰性气体可使用氮气。
实施例1.
将三聚氰胺和分析纯乙酸按照质量比1:10混匀,分散于溶剂水中,其中,水与乙酸的体积比为1:1,将上述溶液于水热反应釜中160℃加热10h,得到多孔氮化碳水热前驱物;将上述水热前驱物于管式炉中氮气保护下550℃煅烧2h,得到有序层状多孔氮化碳材料,如图1,图2a所示。有序层状多孔氮化碳材料的比表面积为138m2g-1,远高于单纯三聚氰胺制备的氮化碳材料的比表面积31m2/g,如图3所示。
实施例2.
将三聚氰胺和乙酸按照质量比1:10混匀,无水条件下,将上述溶液于水热反应釜中180℃加热16h,得到多孔氮化碳水热前驱物;将上述水热前驱物于管式炉中惰性气体保护下500℃煅烧6h,得到多孔氮化碳材料,如图2b所示。均匀多孔氮化碳材料的比表面积为76m2/g。
实施例3.
将三聚氰胺和草酸按照质量比1:5混匀,分散于溶剂水中,其中,水与草酸的质量比为1:1,将上述溶液于水热反应釜中180℃加热5h,得到多孔氮化碳水热前驱物;将上述水热前驱物于管式炉中惰性气体保护下600℃煅烧2h,得到多孔氮化碳材料。多孔氮化碳材料的比表面积为106m2/g。
实施例4.
将三聚氰胺和草酸按照质量比1:20混匀,分散于溶剂水中,其中,水与草酸的质量比为1:1,将上述溶液于水热反应釜中150℃加热10h,得到多孔氮化碳水热前驱物;将上述水热前驱物于管式炉中惰性气体保护下500℃煅烧4h,得到多孔氮化碳材料。多孔氮化碳材料的比表面积为112m2/g。
实施例5.
将三聚氰胺和丁酸按照质量比1:1混匀,分散于溶剂水中,其中,水与丁酸的质量比为1:1,将上述溶液于水热反应釜中80℃加热16h,得到多孔氮化碳水热前驱物;将上述水热前驱物于管式炉中惰性气体保护下450℃煅烧6h,得到多孔氮化碳材料。多孔氮化碳材料的比表面积为86m2/g。
实施例6.
将三聚氰胺和苯甲酸按照质量比1:1混匀,分散于溶剂水中,其中,水与苯甲酸的质量比为1:1,将上述溶液于水热反应釜中180℃加热16h,得到多孔氮化碳水热前驱物;将上述水热前驱物于管式炉中惰性气体保护下550℃煅烧6h,得到管状多孔氮化碳材料,如图2c所示。管状多孔氮化碳材料的比表面积为68m2/g。
实施例7.
将三聚氰胺和水杨酸按照质量比1:5混匀,分散于溶剂水中,其中,水与水杨酸的质量比为1:1,将上述溶液于水热反应釜中180℃加热16h,得到多孔氮化碳水热前驱物;将上述水热前驱物于管式炉中惰性气体保护下550℃煅烧6h,得到管状多孔氮化碳材料。管状多孔氮化碳材料的比表面积为66m2/g。
验证例:
将本发明实施例1中所制备的有序层状多孔氮化碳材料用于有机染料罗丹明B的光催化降解实验,具体过程和步骤如下:
将50mg有序层状多孔氮化碳材料分散于50mL 50mg/L的罗丹明B溶液中,于黑暗条件下搅拌30min使其达到吸附平衡,然后将溶液置于太阳光下,每隔5min用移液枪吸取1mL溶液至离心管中,离心收集上清液,利用紫外-可见分光光度计测定吸光度,根据最大吸收波长553nm波长下罗丹明B溶液的吸光度绘制出不同光照时间下对50mg/L罗丹明B溶液的光催化降解曲线图。
图4是本发明实施例1中有序层状多孔氮化碳材料和单纯三聚氰胺制备的氮化碳材料对罗丹明B在太阳光下的催化活性对比图,可以看到,有序层状多孔氮化碳材料在太阳光照射20min后对罗丹明B降解率基本达到100%,而单纯三聚氰胺制备的氮化碳材料在太阳光照射20min后对罗丹明B的降解率仅为4.1%,表明所制备的有序层状多孔氮化碳材料优异的光催化性能。
以上实施案例的说明可用来帮助理解本发明的原理及方法。但是以上实施案例并不唯一,不应理解为对本发明的限制。与本发明构思无实质性差异的各种工艺方案均在本发明的保护范围之内。
Claims (4)
1.一种有机羧酸辅助批量制备多孔氮化碳材料的方法,其特征在于其制备步骤如下:
将三聚氰胺和有机羧酸按照质量比1:1-1:20混匀后加入水溶解,其中水与有机羧酸的质量比为1:1;或将三聚氰胺和有机羧酸按照质量比1:1-1:20混匀溶解;将溶解后的混合物于水热反应釜中80-180℃加热1-16h,得到多孔氮化碳水热前驱物;将多孔氮化碳水热前驱物于管式炉中于氮气保护下450-650℃煅烧1-6h,得到多孔氮化碳材料;
所述有机羧酸为乙酸、草酸、苯甲酸或水杨酸。
2.如权利要求1所述的一种有机羧酸辅助批量制备多孔氮化碳材料的方法,其特征在于所述三聚氰胺和有机羧酸的质量比为1:2-1:10。
3.如权利要求1所述的一种有机羧酸辅助批量制备多孔氮化碳材料的方法,其特征在于所述溶解后的混合物于水热反应釜中100-180℃加热5-12h。
4.如权利要求1所述的一种有机羧酸辅助批量制备多孔氮化碳材料的方法,其特征在于所述多孔氮化碳水热前驱物于管式炉中于氮气保护下500-600℃煅烧2-4h。
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