CN115155621A - Co-MoS2/CNT光催化改性膜及其制备方法和应用 - Google Patents
Co-MoS2/CNT光催化改性膜及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种Co‑MoS2/CNT光催化改性膜的制备方法，先将(NH4)6Mo7O24·4H2O、CH4N2S和Co(NO3)2•6H2O溶于水，加入CNT粉末，搅拌后在220℃下保持18h，经洗涤、冷冻干燥，得到Co‑MoS2/CNT粉末；再通过真空抽滤将其负载至基底膜上，得到光催化改性膜。本发明中光催化改性膜由Co‑MoS2纳米花和分散的CNT管组成，CNT作为载体可以提供良好的导电性、降低MoS2结构的团聚，这种结构增加了膜表面的光子吸收和电子转移，可以实现高效的PDS活化。同时，将Co‑MoS2/CNT粉末负载至商用PTFE/PP基底膜上，可以提高MoS2/CNT粉末的可回收性。
Description
技术领域
本发明属于光催化材料技术领域，具体涉及一种Co-MoS2/CNT光催化改性膜及其制备方法和应用。
背景技术
近年来，二硫化钼由于其独特的电子、光学、力学和电化学性质而引起了人们的广泛关注，特别是在光催化析氢反应中，同时，其光催化活性也引起了人们的极大兴趣。MoS2是一种层状过度金属硫化物，作为一种二维层状晶体材料，不饱和硫原子被认为是MoS2的活性位点。快速的电子转输能力对催化剂至关重要，表现为高导电性。通过掺杂过渡金属可以降低MoS2的电荷转移阻抗。有研究表明，Co的掺杂可以降低MoS2晶格的层间相互作用、MoS2的层间范德华力，同时增加电子的产生和转移，从而提高MoS2的光催化效率。
本发明中，由Co-MoS2纳米花和分散的CNT管制成的Co-MoS2/CNT粉末，其结构可以增加膜表面的光子吸收和电子转移，从而实现了高效的PDS活化。Co-MoS2/CNT粉末一种很有前途的类芬顿催化降解材料，可以去除水中的剧毒和不可生物降解的污染物。但是，Co-MoS2/CNT粉末用来降解水中污染物时，其回收较为困难，可回收性较差，因此，本发明将Co-MoS2/CNT粉末负载至商用PTFE/PP基底膜上，可以提高MoS2/CNT粉末的可回收性。
发明内容
针对目前的问题，本发明采用一步水热法合成Co-MoS2/CNT粉末，再通过真空抽滤法将Co-MoS2/CNT粉末负载至商用PTFE/PP基底膜上。Co-MoS2/CNT是一种很有前景的类芬顿催化降解材料，可以去除水中的剧毒和不可生物降解的污染物。本发明中，Co-MoS2/CNT膜由Co-MoS2纳米花和分散的CNT管组成，CNT作为载体可以提供良好的导电性、降低MoS2结构的团聚，这种结构增加了膜表面的光子吸收和电子转移，可以实现高效的PDS活化。同时，将Co-MoS2/CNT粉末负载至商用PTFE/PP基底膜上，可以提高MoS2/CNT粉末的可回收性。
为实现上述目的，本发明采用如下技术方案：
一种Co-MoS2/CNT光催化改性膜的制备方法包括以下步骤：
（1）Co-MoS2/CNT粉末的制备：将(NH4)6Mo7O24·4H2O、CH4N2S和Co(NO3)2•6H2O溶解在去离子水中，随后加入CNT粉末，剧烈搅拌30 min后装入反应釜在220℃下保持18h，反应结束后，产物用乙醇和水洗涤，随后在-60℃下冷冻干燥24h，得到Co-MoS2/CNT粉末；
（2）通过真空抽滤的方法将Co-MoS2/CNT粉末负载至基底膜上，得到Co-MoS2/CNT光催化改性膜，可用于降解水中染料RhB。
进一步地，所述(NH4)6Mo7O24·4H2O、CH4N2S和Co(NO3)2•6H2O的使用量为1mmol、28mmol和0.5mmol。
进一步地，所述Co-MoS2/CNT粉末在基底膜上负载量为0.6 mg/cm2。
进一步地，所述基底膜为商用PTFE/PP基底膜。
具体实施方式
为了使本发明所述的内容更加便于理解，下面结合具体实施方式对本发明所述的技术方案做进一步的说明，但是本发明不仅限于此。
实施例1
Co-MoS2/CNT粉末通过一步水热法合成，1 mmol的(NH4)6Mo7O24·4H2O、28mmol的CH4N2S和少量Co(NO3)2•6H2O溶解在70 mL的去离子水中，随后加入100 mg CNT粉末，剧烈搅拌30 min后装入反应釜在220℃下保持18h。反应结束后，产物用乙醇和水洗涤数次，随后在-60℃下冷冻干燥24h。通过修改初始Co(NO3)2•6H2O的量来处理样品的共掺量，将添加了xmmol Co(NO3)2•6H2O的MoS2/CNT混合物记为Co-MoS2/CNT-x。在确定Co最佳掺量为0.5mmol后，首先将适量Co-MoS2/CNT-0.5粉末材料分散在乙醇溶液中，超声处理30 min后，通过真空抽滤的方法将Co-MoS2/CNT-0.5粉末材料负载至商用PTFE/PP基底膜上，负载量为0.6mg/cm2。
使用Co-MoS2/CNT-0.5光催化改性膜在单独芬顿条件下对RhB溶液进行处理，RhB的初始浓度为20 mg/L，运行1 h后，水中的RhB浓度可以被降解58.4%，Co-MoS2/CNT-0.5光催化改性膜的产水率为1.91kg/(m2·h)。
实施例2
Co-MoS2/CNT粉末通过一步水热法合成，1 mmol的(NH4)6Mo7O24·4H2O、28mmol的CH4N2S和少量Co(NO3)2•6H2O溶解在70 mL的去离子水中，随后加入100 mg CNT粉末，剧烈搅拌30 min后装入反应釜在220℃下保持18h。反应结束后，产物用乙醇和水洗涤数次，随后在-60℃下冷冻干燥24h。通过修改初始Co(NO3)2•6H2O的量来处理样品的共掺量，将添加了xmmol Co(NO3)2•6H2O的MoS2/CNT混合物记为Co-MoS2/CNT-x。在确定Co最佳掺量为0.5mmol后，首先将适量Co-MoS2/CNT-0.5粉末材料分散在乙醇溶液中，超声处理30 min后，通过真空抽滤的方法将Co-MoS2/CNT-0.5粉末材料负载至商用PTFE/PP基底膜上，负载量为0.6mg/cm2。
使用Co-MoS2/CNT-0.5光催化改性膜在芬顿条件下对RhB溶液进行处理，RhB的初始浓度为20 mg/L，在光芬顿条件下，Co-MoS2/CNT-0.5改性膜活化PDS产生·SO4 -、1O2和·OH这三种活性自由基。运行1 h后，水中的RhB浓度可以被降解78.5%，Co-MoS2/CNT-0.5光催化改性膜的产水率为3.43kg/(m2·h)。
对比例1
通过简单的一步真空抽滤制备CNT/PTFE/PP膜。首先，称取适量的碳纳米管粉末加入到乙醇溶液中，剧烈搅拌30 min后，再超声处理2 h得到分散均匀的碳纳米管分散液，最后将分散液抽滤至孔径为0.45 μm的聚丙烯衬底的聚四氟乙烯商用空白膜（5cm×5cm）基底上,得到的复合光热催化蒸馏膜（CNT/PTFE/PP）在室温下干燥一夜。CNT/PTFE/PP膜上CNT的负载量为0.6 mg/cm2。
使用CNT/PTFE/PP膜对RhB溶液进行处理，RhB的初始浓度为20 mg/L。预先将RhB溶液用恒温加热磁力搅拌器加热至50℃，然后加入10 mM的PDS再持续搅拌进行RhB降解实验。在光类芬顿的条件下，CNT/PTFE/PP-PDS光类芬顿降解染料体系产生自由基·SO4 -和·OH，运行3 h后，RhB浓度被降解77.8%。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (6)
1.一种Co-MoS2/CNT光催化改性膜的制备方法，其特征在于：包括以下步骤：
（1）Co-MoS2/CNT粉末的制备：将(NH4)6Mo7O24·4H2O、CH4N2S和Co(NO3)2•6H2O溶解在去离子水中，随后加入CNT粉末，剧烈搅拌30 min后装入反应釜在220℃下保持18h，反应结束后，产物用乙醇和水洗涤，随后在-60℃下冷冻干燥24h，得到Co-MoS2/CNT粉末；
（2）通过真空抽滤的方法将Co-MoS2/CNT粉末负载至基底膜上，得到Co-MoS2/CNT光催化改性膜。
2.根据权利要求1所述的制备方法，其特征在于：所述(NH4)6Mo7O24·4H2O、CH4N2S和Co(NO3)2•6H2O的使用量为1mmol、28mmol和0.5mmol。
3.根据权利要求1所述的制备方法，其特征在于：所述Co-MoS2/CNT粉末在基底膜上负载量为0.6 mg/cm2。
4.根据权利要求1所述的制备方法，其特征在于：所述基底膜为商用PTFE/PP基底膜。
5.一种如权利要求1-4任一项所述的制备方法制得的Co-MoS2/CNT光催化改性膜。
6.一种如权利要求5所述的Co-MoS2/CNT光催化改性膜在降解水中染料RhB的应用。
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