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    β-（N，N-二甲胺基乙氧基）酞菁锌在硅胶表面的固载及其光催化活性

    Immobilization of β-(N, N-dimethylaminoethoxy) Phthalocyanine Zinc on Silica Surface and Its Photocatalytic Activity

      摘要
    • 摘要: 通过4-硝基邻苯二腈分别与对羟基苯甲酸和N，N-二甲基乙醇胺反应制备了4-（4-羧基苯氧基）邻苯二腈（CPPN）和4-（N，N-二甲胺基乙氧基）邻苯二腈（ePN），然后利用开环反应将CPPN键合到聚甲基丙烯酸缩水甘油酯改性的硅胶（PGMA/SiO2）表面，得到键合有邻苯二腈的硅胶CPPN-PGMA/SiO2。在“分子碎片”ePN和催化剂1, 8-二氮杂双环5.4.0十一碳-7-烯（DBU）作用下，通过“同步合成与固载”的方法在PGMA/SiO2表面固载金属酞菁（β-（N，N-二甲胺基乙氧基）酞菁锌，ePcZn）或无金属酞菁（ePc），从而制备了固载化的酞菁ePcZn-PGMA/SiO2或ePc-PGMA/SiO2。通过FT-IR、紫外-可见光谱、TG等对其结构和酞菁键合量进行表征和测定。考察了DBU的用量对“同步合成与固载”酞菁过程的影响。以亚甲基蓝（MB）为目标降解物，研究所制得的固载化酞菁催化剂ePc-PGMA/SiO2或ePcZn-PGMA/SiO2的可见光催化活性。结果表明，借助“同步合成与固载”的方法能够成功在PGMA/SiO2表面固载ePc或ePcZn，得到固载化酞菁光催化剂ePc-PGMA/SiO2或ePcZn-PGMA/SiO2，它们均具有较好的可见光催化活性。在可见光照射下，ePcZn-PGMA/SiO2和ePc-PGMA/SiO2在较低的质量浓度下凭借吸附-光催化耦合协同作用均能有效降解MB，且随催化剂用量的增大，MB的降解率增大，0.03 g的ePcZn-PGMA/SiO2能使MB的降解率高达92%。催化剂重复使用5次后仍具有较好的光催化稳定性。

       

      Abstract: 4-(4-Carboxyl group)-O-benzene phthalonitrile (CPPN) and 4-(N, N-dimethylaminoethoxy) phthalonitrile (ePN) were first prepared by the reactions between 4-nitrophthalonitrile and p-hydroxybenzoic acid, and N, N-dimethylethanolamine, respectively. The silica gel bonded with phthalonitrile CPPN-PGMA/SiO2 was then obtained by the ring opening reaction between CPPN and polyglycidyl methacrylate-modified silica (PGMA/SiO2). Finally, in the presence of " molecular fragment” of ePN and catalyst of 1,8-diazabicyclo 5.4.0 undec-7-ene (DBU), β-(N, N-dimethylaminoethoxy) zinc phthalocyanine (ePcZn) or metal-free phthalocyanine (ePc) was immobilized on the surface of PGMA/SiO2 by the method of " synchronous synthesis and immobilization”, leading to the ePc-PGMA/SiO2 or ePcZn-PGMA/SiO2 with immobilized phthalocyanine; Their structures were characterized by FT-IR and TG, and their UV-visible spectra were measured as well. The binding amount of phthalocyanine was determined by FT-IR, UV-Vis diffuse reflectance spectroscopy, and TG. The effect of the content of DBU on the immobilization of phthalocyanine was investigated. In addition, upon using the organic dye methylene blue (MB) as the target degradation material, the photocatalytic properties of the immobilized phthalocyanine catalysts, ePc-PGMA/SiO2 and ePcZn-PGMA/SiO2, were investigated. The results showed that phthalocyanine was successfully immobilized onto the surface of PGMA/SiO2 through the method of synchronous synthesis and immobilization, giving rise to photocatalysts ePc-PGMA/SiO2 and ePcZn-PGMA/SiO2. Both of the prepared ePcZn-PGMA/SiO2 and ePc-PGMA/SiO2 exhibit good photocatalytic activities. They can effectively catalyze the degradation of MB relying on the effect of adsorption-photocatalysis at a lower mass concentration under the irradiation of visible light. The degradation rate of MB increases with the concentration of ePcZn-PGMA/SiO2; and the degradation rate of MB is higher than 92% with addition of 0.03 g of ePcZn-PGMA/SiO2. Moreover, the ePcZn-PGMA/SiO2 shows reliable photocatalytic activity after five times recycles.

       

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