CN110090655A - 一种蒙脱石/石墨相氮化碳复合光催化材料的制备方法 - Google Patents
一种蒙脱石/石墨相氮化碳复合光催化材料的制备方法 Download PDFInfo
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Abstract
本发明属于环境保护技术领域，涉及一种光催化材料的制备方法。特指一种以尿素和蒙脱石为原料，利用湿法共混共焙烧制备蒙脱石/石墨相氮化碳复合光催化剂的方法。本方法通过优化湿法共混的尿素和蒙脱石的比例、调控煅烧的气氛和升温速率等，增大复合材料比表面积的同时，抑制光生电子和空穴的复合，促进活性物种的传质效率，增强复合材料的可见光利用效率，从而提高光催化速率，达到高效分解矿化有机污染物的目的。本发明中的原料价格低廉、来源广泛，合成工艺简单易操作，研发过程绿色无污染，合成的蒙脱石/石墨相氮化碳复合光催化剂无毒无污染，适合大规模应用。
Description
技术领域
本发明属于环境保护技术领域，涉及一种蒙脱石/石墨相氮化碳复合光催化材料的制备方法。
技术背景
以太阳能为驱动力的光催化降解技术具有充分利用清洁的可再生能源的特点，在环境污染防治领域具有独特的优势和良好的应用前景。石墨相氮化碳(g-C3N4)作为一种非金属有机聚合物半导体材料，其带隙约为2.7eV并且具有合适的能带位置，能吸收可见光。此外，g-C3N4具有良好的物理化学稳定性，在光催化降解污染物方面具有潜在的应用前景。g-C3N4可由一些富含氮元素的有机物质如双氰胺、三聚氰胺等通过热缩聚过程形成。然而，部分前驱体对人类和环境具有潜在毒性，还具有不稳定、合成困难以及不能大规模应用等缺陷。尿素作为一种常见和廉价的化合物在化工行业广泛使用。同时，尿素无毒、稳定、易保存，可作为合成g-C3N4的理想前驱体。
g-C3N4在光照下价带电子能够激发至导带形成电子–空穴对，电子与溶解氧结合，也可与水分子反应。上述过程促使三种活性物质的生成，即空穴(h+)、超氧自由基(·O2 -)和羟基自由基(·OH)。这些活性物质可分解某些有机污染物，即g-C3N4可光催化降解有机污染物。然而，g-C3N4的光生电子和空穴易复合，量子产率低。近些年来引发了针对g-C3N4改性来提高其量子效率的研究热潮，改性方法包括带隙调控、缺陷调控、优化孔结构、表面敏化、构造异质结、负载纳米碳材料等。但大多方法合成工艺复杂，原料成本高。本方法利用粘土矿物—蒙脱石(Mt)掺杂改性g-C3N4，提高其光催化效率。
蒙脱石由两层硅氧四面体晶片夹一层铝氧八面体晶片组成，属于2:1型层状硅酸盐矿物，具有二维层状纳米结构。蒙脱石具有较高的比表面积，且层间的水合阳离子易发生离子交换，使其有很强的吸附能力。采用蒙脱石掺杂氮化碳可增大复合催化剂的比表面积，提高其吸附能力。另外，蒙脱石层间只存在松弛的范德华力，硅、铝易与水中阳离子发生晶格置换，使得蒙脱石层间存在过剩的负电荷，可抑制催化剂光生电子和空穴的复合，从而可以更高效地产生活性物种，促进传质效率，提高光催化降解污染物的速率，进而增强催化效率。蒙脱石/石墨相氮化碳(Mt/g-C3N4)复合光催化剂同时具有环境友好、低成本和稳定高效的特性。
发明内容
本发明针对现有技术中的问题，提供一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，得到一种合成工艺简单、研发过程绿色无污染、成本低、催化活性高的光催化剂。
为达到上述目的，采用技术方案如下：
本发明提供了一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于由一定比例的尿素和蒙脱石湿法共混共焙烧制备而成。
在本发明中所述的Mt为提纯后的钠基蒙脱石，g-C3N4由尿素为前驱体制备而成。
一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，具体包括以下步骤：
1)称取一系列不同质量的蒙脱石加入超纯水中，搅拌并超声得到一定固液比的蒙脱石悬浊液；
2)将尿素加入上述蒙脱石悬浊液中，水浴搅拌过夜；
3)将尿素/蒙脱石混合物冷冻干燥后研磨成粉末，转移至加盖的坩埚中，在马弗炉中以一定的升温速率高温煅烧，产物为灰黄色固体,记为Mt/g-C3N4，研磨待用。
所述尿素添加量为10～20g，以尿素为前驱体制备g-C3N4，产率以2％计算；
所述Mt添加量为g-C3N4质量分数的0.25％～2.5％，优选的所述Mt添加量为1％，超声时间为30～60min；
所述尿素和超纯水的固液比为1:2～1:3，优选为1:2，所述水浴温度为50～60℃，优选为50℃，搅拌时间为10～14h，优选为12h；
所述煅烧气氛为半密闭的空气气氛(坩埚加盖)；所述升温程序为：以3～10℃/min的升温速率升至500～600℃，恒温时间2～3h，优选的，升温速率为5℃/min，恒温时间2h。冷却至室温后取出。
本发明还提供了一种复合光催化剂在光催化降解有机污染物中的应用，所述复合光催化剂选自上述复合光催化剂或者由上述方法制备得到的复合光催化剂，该催化剂具有良好的光催化降解金霉素污染的效果。
本发明制备的Mt/g-C3N4复合光催化剂无毒无污染，在水中难降解有机物处理方面具有高活性，具有很好的应用前景和市场价值。此外，本发明提供的复合光催化剂制备方法简单易行，原料成本低，适合大规模应用。
附图说明
附图1：石墨相氮化碳(g-C3N4)场发射扫描电镜形貌图；
附图2：蒙脱石(Mt)场发射扫描电镜形貌图；
附图3：蒙脱石/石墨相氮化碳复合材料(1.0％Mt/g-C3N4)场发射扫描电镜形貌图。
具体实施方式
以下实施例进一步阐释本发明的技术方案，下面结合实例对本发明提供的复合光催化剂及其制备方法进行说明，但本发明的保护范围不受以下实例的限制。
实施例1：
石墨相氮化碳光催化剂，它是由如下步骤制备得到的：
(1)称取10g尿素加入坩埚中，加盖放入马弗炉中；
(2)以速率5℃/min升温至550℃，恒温2h，产物研磨，即得石墨相氮化碳光催化剂。
实施例2：
一种蒙脱石/石墨相氮化碳复合光催化剂，它是由如下步骤制备得到的：
(1)将2mg蒙脱石加入30mL超纯水中，搅拌均匀后超声30min得到蒙脱石悬浊液；
(2)将10g尿素加入到上述蒙脱石悬浊液中，水浴50℃搅拌过夜；
(3)将步骤(2)中混合物冷冻干燥，所得固体混合物研磨并转移至加盖的坩埚中，以
速率5℃/min升温至550℃，恒温2h，产物研磨，即得1.0％Mt/g-C3N4复合光催化剂。
参照图1和2所示，图1为实施例1所得原始的石墨相氮化碳片层结构、多孔结构的场发射扫描电镜形貌图；图2为实施例2所得蒙脱石/石墨相氮化碳复合材料场发射扫描电镜形貌图，电镜图片中可观察到g-C3N4及蒙脱石的片层结构，且部分为g-C3N4包覆蒙脱石片层，这种结构可增强光催化效果。
实施例3：
重复实施例2，有以下不同点，蒙脱石的添加量为0.5mg、1.0mg、5mg。将得到不同配比Mt的复合材料分别记为0.25％Mt/g-C3N4、0.5％Mt/g-C3N4、2.5％Mt/g-C3N4。
实施例4：
Mt/g-C3N4复合光催化剂可见光条件下光催化降解金霉素速率评价：
将实施例2与实施例3制得的四种不同配比Mt/g-C3N4进行光催化降解金霉素(CTC)实验。实验条件为：室温25℃条件下，将10mg催化剂与100mL浓度为20mg/L的金霉素溶液混合于光催化反应器中，避光磁力搅拌30min使体系达到吸附-解吸平衡。以300W氙灯作为光源(加装420nm滤光片)，间隔一定时间取样，过0.22um水系针式滤头，使用超高效液相色谱-二极管阵列检测器联用检测CTC浓度(CTC最大吸收波长369nm)，使用拟一级动力学方程计算降解速率：
ln(C0/Ct)＝kt
其中C0为体系中金霉素初始浓度(20mg/L)，Ct为反应t min时体系中金霉素浓度，k为反应速率常数。
表1光催化降解CTC拟一级动力学拟合参数对比
不难发现，同样的实验条件下，本发明蒙脱石/石墨相氮化碳光催化剂的降解速率相对较快，效果增益显著。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的研究人员来说，在不脱离本发明原理的前提下，可做出改进和修饰，这些改进和修饰也应视作本发明的保护范围。
Claims (9)
1.一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于由尿素和蒙脱石(Mt)湿法共混共焙烧制备而成。
2.根据权利要求1所述的Mt为提纯后的钠基蒙脱石，石墨相氮化碳(g-C3N4)由尿素为前驱体制备而成。
3.一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，具体包括以下步骤：
1)称取不同质量的蒙脱石加入超纯水中，搅拌并超声得到蒙脱石悬浊液；
2)将尿素加入上述蒙脱石悬浊液中，水浴搅拌过夜；
3)将尿素/蒙脱石混合液冷冻干燥，所得固体研磨后转移至加盖的坩埚中，在马弗炉中煅烧得到灰黄色固体,即得Mt/g-C3N4，研磨待用。
4.根据权利要求3所述的一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于步骤2)，以尿素为前驱体制备g-C3N4，所述尿素添加量为10～20g，g-C3N4产率以2％计算。
5.根据权利要求3所述的一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于步骤1)中Mt添加量为g-C3N4质量分数的0.25％～2.5％，超声时间为30～60min。
6.根据权利要求3所述的一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于步骤2)所述尿素和超纯水的固液比为1:2～1:3，所示水浴温度为50～60℃，搅拌时间为10～14h。
7.根据权利要求3所述的一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于步骤3)所述煅烧气氛为半密闭的空气气氛(坩埚加盖)。
8.根据权利要求3所述的一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于步骤3)所述煅烧过程以速率3～10℃/min升温至500～600℃，恒温2～3h，冷却至室温后取出，研磨得到Mt/g-C3N4复合光催化剂。
9.一种蒙脱石/石墨相氮化碳复合光催化剂的制备方法，其特征在于，所述复合光催化剂选自权利要求1～2任意一项所述的复合光催化剂，或者由权利要求3～7任意一项所述的制备方法得到的复合光催化剂。
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