CN106975511A - 一种MoS2/C60/g‑C3N4复合光催化剂及其制备方法 - Google Patents
一种MoS2/C60/g‑C3N4复合光催化剂及其制备方法 Download PDFInfo
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- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01J35/39—
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
本发明公开了一种MoS2/C60/g‑C3N4复合光催化材料及其制备方法,属于纳米光催化材料技术领域;本发明以水热法制备的MoS2与C60和g‑C3N4以共沉淀法进行复合,形成了具有片状形貌的纳米复合物,该复合物中中MoS2所占质量比为3%~9%,C60与g‑C3N4质量比为1:1,经过测试,其在可见光照射下相比MoS2、C60和g‑C3N4的催化效率得到了显著提高,6%MoS2/C60/g‑C3N4经可见光照射70min罗丹明B降解率可达100%。本发明中所采用的制备方法过程简单易控、操作方便、成本低、产物的可见光催化活性高。
Description
技术领域
本发明属于纳米光催化材料技术领域。
背景技术
石墨相氮化碳(g-C3N4)作为一种碳基材料,具有制备原料来源广,价格便宜,制备方法简单且易于工业化等特点。作为可见光催化剂其具有可调的电子结构和良好的物理和化学稳定性。由于它的禁带宽度为2.70eV,能够被可见光激发,可以吸收可见光分解水制氢;然而,g-C3N4也有很多缺点影响了其光催化性能的提高,特别是较高的电子空穴复合率,严重降低了其光催化效率,对于改善g-C3N4光催化性能,提高其电子空穴分离率一直是该领域研究的重点。
MoS2片状结构在电化学方面有较广泛的应用,作为知名的产氢催化剂,二硫化钼被视为理想的催化剂,被广泛应用于光催化、传感等领域。
虽然两种材料都可以作为光催化材料使用但是如何进一步提高其光催化效率是目前亟待解决的重要课题。
发明内容
针对上述问题,本发明提出了一种MoS2/C60/g-C3N4复合光催化剂,利用了闭壳结构的C60所具有的独特的电子性能。已知C60的闭壳结构由30个键合分子轨道与60个π电子,这种结构利于有效的电子转移。C60的独特结构使其可以作为一个优秀的电子受体,有效地引起快速光诱导电荷分离和相对较慢的电荷重组,则可以提高g-C3N4电子空穴分离率,该复合结构中由于MoS2的植入使g-C3N4层间距变大,有效增大催化剂的比表面。并且由于MoS2、C60和g-C3N4之间所形成异质结,提高了光电荷的分离效率,有效地提高了光催化效率。
MoS2/C60/g-C3N4复合光催化剂,中MoS2所占质量比为3%~9%,C60与g-C3N4质量比为1:1;该复合催化剂为片状形貌,复合结构中以尺寸为1μm、厚度为50~70nm的g-C3N4为基底,依次在其表面复合C60和尺寸为200~500nm,厚度为50~80nm的片状MoS2得到。
该复合光催化剂的制备方法具体如下:
1)水热法制备MoS2;
2)制备g-C3N4;
3)C60/g-C3N4复合物的制备:按照质量比1:1称取g-C3N4与C60,将二者按照5mg/mL的比例分散于无水乙醇中,分散均匀后在外加搅拌条件下持续12h,然后置于80~100℃条件下干燥,得到C60/g-C3N4复合物;
4)MoS2/C60/g-C3N4复合物的制备:0.9~2.7:30比例称取水热法制备的MoS2和C60/g-C3N4复合物,将二者按照1.5~5mg/mL的比例分散于无水乙醇中,分散均匀后在外加搅拌条件下持续3h,然后置于80~100℃条件下干燥,得到MoS2/C60/g-C3N4复合物;
步骤1)中水热法制备MoS2的具体步骤如下:
按照质量比为0.37~0.38:1的比例称取钼酸钠和硫脲溶于去离子水中,完全溶解后再超声分散30min以上,得到混合溶液,混合溶液中钼酸钠浓度为0.19~0.20mol/L;将混合溶液转移至反应釜中,充填度为65%,在240℃条件下反应24h后自然冷却至室温;用去离子水和乙醇分别洗涤后,在60℃条件下干燥,得到片状MoS2。
步骤2)制备g-C3N4的具体步骤如下:将三聚氰胺以2.0~2.3℃/min的升温速率为从室温加热到550℃,并于550℃保温4h,然后以相同的速率降温至室温后得到淡黄色粉末状的g-C3N4。
本发明的有益效果:
本发明的制备过程简单易控、操作方便、成本低、产物的可见光催化活性高,其中,6%MoS2/C60/g-C3N4经可见光照射70min罗丹明B降解率可达100%。在复合纳米材料的制备和应用领域有着广阔的发展前景。
附图说明
图1 C60和所制备的MoS2、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4以及MoS2/C60/g-C3N4复合光催化剂的X射线衍射(XRD)谱图;
图2所制备的C60、MoS2、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4以及MoS2/C60/g-C3N4复合光催化剂的傅立叶红外光谱(FT-IR)图;
图3所制备的MoS2/C60/g-C3N4复合光催化剂的X射线光电子能谱(XPS)图;
图4所制备复合催化剂MoS2/C60/g-C3N4的透射电镜(TEM)照片;
图5所制备复合催化剂MoS2/C60/g-C3N4的高分辨透射电镜(HRTEM)照片;
图6所制备的C60、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4以及MoS2/C60/g-C3N4复合光催化剂在可见光条件下降解罗丹明B的光催化降解率曲线图。
具体实施方式
下面以具体实施例的方式对本发明技术方案作进一步解释和说明。
实施例1
1.MoS2的制备:采用水热合成法,将0.15g钼酸钠和0.4g硫脲共溶于32.5mL去离子水中,在磁力搅拌器上搅拌30min。搅拌结束后再超声分散30min。将超声后的溶液装入内衬聚四氟乙烯不锈钢反应釜中,充填度为65%,加热到240℃并保持24h后自然冷却至室温。用去离子水和乙醇分别洗涤3次后,在60℃条件下将产物进行干燥。
2.g-C3N4的制备:采用三聚氰胺为原料,取24mmol三聚氰胺于坩埚中,将坩埚放入马弗炉中,以升温速率为2.0-2.3℃/min加热到550℃,于550℃保温4h,然后以相同的速率降至初始温度后将坩埚取出,得到淡黄色粉末状的g-C3N4。
3.C60/g-C3N4的制备:将50mg C60和50mg g-C3N4超声30min分散于20mL无水乙醇中,在磁力搅拌器上搅拌12h后,于干燥箱内80℃烘干,即得C60/g-C3N4。
4.MoS2/C60/g-C3N4的制备:将0.9mg MoS2和30mg C60/g-C3N4超声1h分散于20mL无水乙醇中,在磁力搅拌器上搅拌3h后,于干燥箱内80℃烘干,即得MoS2/C60/g-C3N4。
结构与形貌表征
如图1所示,为C60和所制备的MoS2、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4以及MoS2/C60/g-C3N4复合光催化剂的XRD图,从图1可知MoS2/C60/g-C3N4复合光催化剂的XRD图谱中含有硫化钼、g-C3N4和C60特征峰,且未出现其他杂峰,证明复合物中仅包含有以上三种物质。
如图2所示,所有C60的特征峰(1427cm-1、1180cm-1、575cm-1、528cm-1)以及g-C3N4的特征峰(3168cm-1、1635cm-1、1574cm-1、1420cm-1、1328cm-1、1253cm-1、812cm-1)都可以从MoS2/C60/g-C3N4图谱中可以观察到。
如图3所示,C 1s的两个峰分别在283.9eV(C-C)和287.6eV(N-C=N)。287.6eV与288.0eV相接近可知C60对g-C3N4的N-C=N几乎没有影响。N 1s的峰出现在398.2eV(C=N-C)。Mo 3d的峰分别在228.2eV和231.4eV可知钼的存在形式为Mo4+,S 2p的峰出现在161.5eV可知的存在形式为S2 2-。
图4为所制备的MoS2/C60/g-C3N4样品的TEM照片,其形貌为片状。图5中可以测量出晶体条纹距离分别为0.366nm和0.63nm,分别对应g-C3N4(002)和MoS2(002)的晶面间距,由此可以看出g-C3N4和MoS2成功复合到了一起,根据图4可以看到透明的C60与片状的复合物复合在一起。
光催化活性验证试验:
使用Rh B作为模型化合物对所制备样品的光催化性能进行评价。在实验中,在100mL 0.01mmolL-1的Rh B溶液中加入0.01g催化剂并放入玻璃反应器中。采用500W氙灯(λ>420nm)照射。将420nn滤波器***灯和样品之间以除去紫外光(λ<420nm)。在可见光照明之前将悬浮液在黑暗中强烈搅拌30分钟。然后将溶液在磁力搅拌下暴露于可见光照射。在给定的时间间隔,定期收集和分析4mL的悬浮液。通过UV-2550紫外光谱仪对Rh B浓度进行分析,在紫外可见光的最大波段为552nm时记录吸收光谱强度。
结果如图6所示,所制备的MoS2/C60/g-C3N4催化剂较纯相C60、g-C3N4、C60/g-C3N4、MoS2/C60及MoS2/g-C3N4光催化效率有大幅度提高,其中6%MoS2/C60/g-C3N4Rh B光催化效率最高,经可见光照射70min Rh B降解率可达100%。
Claims (4)
1.一种MoS2/C60/g-C3N4复合光催化剂,其特征在于,该复合光催化剂中MoS2所占质量比为3%~9%,C60与g-C3N4质量比为1:1;该复合催化剂为片状形貌,复合结构以尺寸为1μm、厚度为50~70nm的g-C3N4为基底,依次在其表面复合C60和尺寸为200~500nm,厚度为50~80nm的片状MoS2得到。
2.如权利要求1所述MoS2/C60/g-C3N4复合光催化剂的制备方法,具体步骤如下:
1)水热法制备MoS2;
2)制备g-C3N4;
3)C60/g-C3N4复合物的制备:按照质量比1:1称取g-C3N4与C60,将二者按照5mg/mL的比例分散于无水乙醇中,分散均匀后在外加搅拌条件下持续12h,然后置于80~100℃条件下干燥,得到C60/g-C3N4复合物;
4)MoS2/C60/g-C3N4复合物的制备:0.9~2.7:30比例称取水热法制备的MoS2和C60/g-C3N4复合物,将二者按照1.5~5mg/mL的比例分散于无水乙醇中,分散均匀后在外加搅拌条件下持续3h,然后置于80~100℃条件下干燥,得到MoS2/C60/g-C3N4复合物。
3.根据权利要求2所述的MoS2/C60/g-C3N4复合光催化剂的制备方法,其特征在于,步骤1)中水热法制备MoS2的具体步骤如下:
按照质量比为0.37~0.38:1的比例称取钼酸钠和硫脲溶于去离子水中,完全溶解后再超声分散30min以上,得到混合溶液,混合溶液中钼酸钠浓度为0.19~0.20mol/L;
将混合溶液转移至反应釜中,充填度为65%,在240℃条件下反应24h后自然冷却至室温;用去离子水和乙醇分别洗涤后,在60℃条件下干燥,得到片状MoS2。
4.根据权利要求2所述的MoS2/C60/g-C3N4复合光催化剂的制备方法,其特征在于,步骤2)制备g-C3N4的具体步骤如下:
将三聚氰胺以2.0~2.3℃/min的升温速率为从室温加热到550℃,并于550℃保温4h,然后以相同的速率降温至室温后得到淡黄色粉末状的g-C3N4。
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