酞菁功能化纤维素纳米纤维的制备及其染料废水脱色性能研究
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摘要
纤维素纳米纤维综合了纤维素来源广泛、无毒副作用、稳定性高、含大量羟基官能团和纳米纤维比表面积超高、机械性能优异、表面易调控等优点,是功能性分子的理想载体材料。本论文以纤维素纳米纤维为基体,将四氨基钴酞菁(CoPc)催化剂共价固定于其表面制备得到异相催化剂,并应用于模拟染料废水脱色处理。具体研究内容如下：
利用静电纺丝技术制备了乙酸纤维素纳米纤维,将CoPc共价固定于经水解和氧化表面改性后的纳米纤维表面,制备得到酞菁表面功能化纤维素纳米纤维CoPc-NM.以活性艳红X-3B染料溶液模拟工业染料废水,测试CoPc-NM的脱色性能。发现酸性条件下CoPc分子对带负电荷的阴离子染料具有很高的吸附容量,吸附能力的提高可促进催化氧化反应的进行。pH=2时,以H2O2为氧化剂,CoPc-NM能在90min内使90%的染料分子催化氧化降解。
在催化剂与载体之间引入一条间隔臂,制备得到酞菁表面功能化,间隔臂连接纤维素纳米纤维CoPc-spacer-NM。间隔臂的引入可降低纳米纤维载体对CoPc的位阻效应,减少染料分子向CoPc扩散时的扩散阻力,进而提高纳米纤维表面CoPc的催化效率,pH=10时催化氧化速率高达73.85μmol·min-1.g-1。利用电子顺磁共振(EPR)技术证实了催化氧化过程中有高活性的羟基自由基·OH产生。通过气相色谱-质谱联用(GC-MS)技术证实染料分子被深度氧化为顺丁烯二酸、反丁烯二酸、戊二酸和己二酸等易被生物降解的脂肪酸。初步探讨了CoPc-spacer-NM在催化膜反应器中的应用,在最佳操作条件下,反应9min可使染料溶液浓度下降90%以上。
将电子传导性能优异的多壁碳纳米管(MWNT)引入到催化氧化体系,制备碳纳米管掺杂,酞菁表面功能化,间隔臂连接纤维素纳米纤维,研究其对模拟染料废水的脱色性能。结果表明,MWNT能在一定程度上促进催化氧化反应的进行,含5%MWNT的异相催化剂对染料溶液的催化氧化速率比CoPc-spacer-NM快约20%。
Cellulose nanofibers are promising supports for functional molecules immobilization due to several attractive characteristics:low cost, nontoxicity, high physicochemical stability, and high density of hydroxyl groups from cellulose; and very large surface-to-volume ratio, good mechanical properties as well as easily tunable surface from nanofiber. In this thesis, cellulose nanofibers were selected as support of cobalt tetraaminophthalocyanine (CoPc) catalyst. CoPc was covalently immobilized onto the surface of cellulose nanofibers and the prepared heterogeneous catalyst was used for decolorizing simulated dye wastewater. The main experiments and results are summarized as follow.
Cellulose acetate was electrospun into nanofiber mats (CA-NM), CoPc was covalent immobilized onto the surface after hydrolyzation and oxidation. The CoPc functionalized nanofiber mats (CoPc-NM) was used for the treatment of a simulated dye wastewater:reactive red X-3B solution. In acidic solution, CoPc-NM has high adsorption capacity to anionic dye molecules, which can further promote the catalytic oxidation efficiency when H2O2was present as oxidant. At pH2, more than90%of reactive red X-3B can be eliminated by CoPc-NM/H2O2in90min.
To further minimize the effects of diffusion limitation and steric hindrance and improve the decoloration efficiency of the heterogeneous catalyst, a novel CoPc functionalized, spacer arm attached cellulose nanofiber mats (CoPc-spacer-NM) nanomaterial was prepared and used for decoloration of the simulated dye wastewater. Compared with CoPc-NM, CoPc-spacer-NM shows much higher adsorption capacity when conducted under acidic condition, which enhances the catalytic oxidation rate of dye molecules when H2O2was used as oxidant. Dye wastewater can also be efficiently decolorized by CoPc-spacer-NM/H2O2system under basic condition. Despite a relatively weak adsorption capacity, the catalytic oxidation rate was73.85μimol·min-1·g-1at pH10. Electron paramagnetic resonance (EPR) results suggest that the catalytic oxidation process involves the formation and reaction of hydroxyl radicals. Gas chromatography-mass spectra (GC-MS) show that reactive red X-3B is mainly decomposed to biodegradable aliphatic acids, such as maleic acid, fumaric acid, glutaric acid and adipic acid. A catalytic membrane reactor was assembled based on CoPc-spacer-NM. At optimal operational condition,90%of dye molecules can be eliminated within9min.
To enhance the electron transfer efficiency of CoPc during the catalytic oxidation process, a multiwalled carbon nanotube doped, CoPc functionalized, spacer arm attached cellulose nanofiber mats (MWNT/CoPc-spacer-NM) was prepared. Due to its well conductivity, the introduction of MWNT can accelerate the electron transfer of MWNT/CoPc-spacer-NM/H2O2, the catalytic oxidation efficiency is20%higher when compared with CoPc-spacer-NM/H2O2system.
利用静电纺丝技术制备了乙酸纤维素纳米纤维,将CoPc共价固定于经水解和氧化表面改性后的纳米纤维表面,制备得到酞菁表面功能化纤维素纳米纤维CoPc-NM.以活性艳红X-3B染料溶液模拟工业染料废水,测试CoPc-NM的脱色性能。发现酸性条件下CoPc分子对带负电荷的阴离子染料具有很高的吸附容量,吸附能力的提高可促进催化氧化反应的进行。pH=2时,以H2O2为氧化剂,CoPc-NM能在90min内使90%的染料分子催化氧化降解。
在催化剂与载体之间引入一条间隔臂,制备得到酞菁表面功能化,间隔臂连接纤维素纳米纤维CoPc-spacer-NM。间隔臂的引入可降低纳米纤维载体对CoPc的位阻效应,减少染料分子向CoPc扩散时的扩散阻力,进而提高纳米纤维表面CoPc的催化效率,pH=10时催化氧化速率高达73.85μmol·min-1.g-1。利用电子顺磁共振(EPR)技术证实了催化氧化过程中有高活性的羟基自由基·OH产生。通过气相色谱-质谱联用(GC-MS)技术证实染料分子被深度氧化为顺丁烯二酸、反丁烯二酸、戊二酸和己二酸等易被生物降解的脂肪酸。初步探讨了CoPc-spacer-NM在催化膜反应器中的应用,在最佳操作条件下,反应9min可使染料溶液浓度下降90%以上。
将电子传导性能优异的多壁碳纳米管(MWNT)引入到催化氧化体系,制备碳纳米管掺杂,酞菁表面功能化,间隔臂连接纤维素纳米纤维,研究其对模拟染料废水的脱色性能。结果表明,MWNT能在一定程度上促进催化氧化反应的进行,含5%MWNT的异相催化剂对染料溶液的催化氧化速率比CoPc-spacer-NM快约20%。
Cellulose nanofibers are promising supports for functional molecules immobilization due to several attractive characteristics:low cost, nontoxicity, high physicochemical stability, and high density of hydroxyl groups from cellulose; and very large surface-to-volume ratio, good mechanical properties as well as easily tunable surface from nanofiber. In this thesis, cellulose nanofibers were selected as support of cobalt tetraaminophthalocyanine (CoPc) catalyst. CoPc was covalently immobilized onto the surface of cellulose nanofibers and the prepared heterogeneous catalyst was used for decolorizing simulated dye wastewater. The main experiments and results are summarized as follow.
Cellulose acetate was electrospun into nanofiber mats (CA-NM), CoPc was covalent immobilized onto the surface after hydrolyzation and oxidation. The CoPc functionalized nanofiber mats (CoPc-NM) was used for the treatment of a simulated dye wastewater:reactive red X-3B solution. In acidic solution, CoPc-NM has high adsorption capacity to anionic dye molecules, which can further promote the catalytic oxidation efficiency when H2O2was present as oxidant. At pH2, more than90%of reactive red X-3B can be eliminated by CoPc-NM/H2O2in90min.
To further minimize the effects of diffusion limitation and steric hindrance and improve the decoloration efficiency of the heterogeneous catalyst, a novel CoPc functionalized, spacer arm attached cellulose nanofiber mats (CoPc-spacer-NM) nanomaterial was prepared and used for decoloration of the simulated dye wastewater. Compared with CoPc-NM, CoPc-spacer-NM shows much higher adsorption capacity when conducted under acidic condition, which enhances the catalytic oxidation rate of dye molecules when H2O2was used as oxidant. Dye wastewater can also be efficiently decolorized by CoPc-spacer-NM/H2O2system under basic condition. Despite a relatively weak adsorption capacity, the catalytic oxidation rate was73.85μimol·min-1·g-1at pH10. Electron paramagnetic resonance (EPR) results suggest that the catalytic oxidation process involves the formation and reaction of hydroxyl radicals. Gas chromatography-mass spectra (GC-MS) show that reactive red X-3B is mainly decomposed to biodegradable aliphatic acids, such as maleic acid, fumaric acid, glutaric acid and adipic acid. A catalytic membrane reactor was assembled based on CoPc-spacer-NM. At optimal operational condition,90%of dye molecules can be eliminated within9min.
To enhance the electron transfer efficiency of CoPc during the catalytic oxidation process, a multiwalled carbon nanotube doped, CoPc functionalized, spacer arm attached cellulose nanofiber mats (MWNT/CoPc-spacer-NM) was prepared. Due to its well conductivity, the introduction of MWNT can accelerate the electron transfer of MWNT/CoPc-spacer-NM/H2O2, the catalytic oxidation efficiency is20%higher when compared with CoPc-spacer-NM/H2O2system.
引文
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