四氧化三铁基磁性聚合物的合成、表征及应用研究
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摘要
四氧化三铁基磁性聚合物材料由于其具有独特的超顺磁性、生物相容性以及其他可调节的优异的光、催化、吸附等性能,而在磁分离、催化、生物医学以及生物医药等领域有着广泛的应用前景。
本论文围绕四氧化三铁基磁性聚合物材料的制备、结构表征、形貌表征、磁性能、吸附性能和催化性能等,展开对不同形貌、结构和组成的四氧化三铁基磁性聚合物材料的合成、磁分离性能以及催化性能的研究：
(1)以油酸包覆的Fe3O4纳米粒子作为磁核,以MMA和DVB作为单体,分别使用正已烷、环已烷、甲苯等小分子致孔剂,采用改性悬浮聚合制备了10种磁性多孔微球(FMD),用氮气吸脱附法和压汞法表征了产物的孔结构,用TEM和SEM观察了产物的形貌,用TGA考察了四氧化三铁的包覆率。并尝试利用UV考察其脱除水体中的苯酚的能力。研究发现,FMD微球中存在类似于墨水瓶状孔的小口径大腹腔的孔。致孔剂类型和用量对FMD微球孔结构的影响是显著而复杂的。使用两种体系良溶剂作致孔剂(环已烷(CHX)和正已烷(n-HX))制备的产物均具有相对较高的比表面积。减少致孔剂用量,增加交联剂DVB的用量,都有利于形成较为完整的交联网络,从而提高FMD微球的四氧化三铁包覆率。此外,增加磁流体的用量,也可以提高四氧化三铁的包覆率。FMD磁性微球表现出明显Fe304晶相结构,并在室温下,表现为超顺磁性。研究发现,FMD磁性多孔微球可有效地去除水溶液中的苯酚,去除率可达99.32%。
(2)以油酸包覆的Fe304纳米粒子作为磁核,以St和DVB作为单体,采用乳液聚合法制备了10种磁性Fe3O4/poly (St-co-DVB)微球,进一步以TEOS为硅源,制备了14种Fe3O4/poly (St-co-DVB)/SiO2有机/无机杂化的磁性微球。考察了单体组成、表面活性剂类型和磁流体的加入量对微球表面形貌、四氧化三铁包覆率及微球粒径等的影响。然后尝试以上述微球作为磁性基体,采用了水热法制备了Fe3O4/poly (St-co-DVB)/SiO2/TiO2磁性纳米催化剂,进一步研究其对罗丹明B(RhB)降解的光催化性能。研究发现,所制备的磁性纳米催化剂可在UV照射下有效地降解RhB。重复使用5次,其RhB的降解率仍在90%以上,仍具有高效的催化效果。此催化剂因其采用磁性无机.有机杂化磁性微球作为磁性基体,易于磁分离,有利于工业化使用。
(3)制备了三个系列不同结构和形貌的磁性聚(六氯环三磷腈-co-双酚S)。以水热法制备了16种中空多孔的Fe3O4微球,并以此为磁核,以TEOS为硅源,在CTAB的存在下,在制得的Fe3O4微球外层包覆一层介孔二氧化硅制备了6种中空多孔Fe3O4/mSiO2和1种中空Fe3O4/nSiO2微球,再以BPS和HCCP作为单体,制备了4种中空多孔Fe3O4/mSiO2/PZS和4种中空Fe3O4/nSiO2/PZS微球。以共沉淀法制备的4种Fe3O4/OA纳米粒子为磁核,以BPS和HCCP作为单体,在TEA存在下,制备了9种Fe3O4/PZS磁性纳米线。以水热法制备了21种Fe304纳米线,并以此为磁核,以BPS和HCCP作为单体,在TEA存在下,制备了5种Fe3O4/PZS磁性纳米线。使用TEM和SEM观察了产物的形貌,用TGA考察了四氧化三铁的包覆率,XRD表征了产物的晶相结构,并采用DLS和SEM测试了产物的粒径,用SQUID测试了产物的磁性能,采用氮气吸脱附法表征了产物的比表面积和孔结构,此外,以上述制备的磁性聚磷腈复合材料为磁性基体,分别以Fe3O4/mSiO2/PZS为磁性基体,以二茂铁二甲酰氯为原料,利用酯化反应制备了Fe3O4/mSiO2/PZS/Fc磁性微球;以HAuCl4作为金源,采用化学沉积法制备了13种磁性聚磷腈纳米金催化剂,其对4.硝基苯酚在NaBH4存在下还原反应有较好的催化性能,并且此催化剂可循环使用。所得的聚膦腈磁性材料具有良好亲水性、良好热稳定性、生物相容性及较好的磁响应能力等等,有良好的工业应用前景。
Fe3O4-based magnetic polymer composite materials have been applied in many areas, including magnetic separation, catalysis, biomedical, bio-medicine and so on, because of their unique superparamagnetic, biocompatibility and excellent optical, catalytic and adsorption properties.
In this thesis, we have focused on the studies of synthesis, structure, morphology, magnetic property, adsorption property and catalytic activity of the Fe3O4-based magnetic polymer composite materials. We have studied the synthesis, magnetic separation and catalytic property of Fe3O4-based magnetic polymer composite materials which have different morphology, structure, composite.
(1) Ten different magnetic porous microspheres (FMD) were synthesized by modified suspension polymerization of methacrylate and divinylbenzene, in the presence of oleic acid coated Fe3O4nanopaticles, using n-hexane, cyclohexane, toluene as small molecules progent, respectively. The morphologies and properties of the magnetic porous microspheres were charaterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), superconducting quantum interference device (SQUID), Fourier transform infrared spectroscopy (FT-IR), thermogravimetry (TGA), and X-ray powder diffraction (XRD). The pore size distribution and the specific surface area of magnetic porous microspheres were measured by nitrogen sorption and mercury porosimetry technique. The obtained microspheres were applied in the removal of phenol from aqueous solution, and the concentration of phenol aqueous solutions was measured by ultraviolet analyses (UV). It was found that magnetic porous microspheres had the ink bottle shape hole, some minor-caliber and big celiac hole. The amount and type of progents complicated and dramaticlly affected the pore structure of FMD microsphere. The magnetic porous microspheres possessed a high specific surface area by using n-hexane and cyclehexane as porogent. It was further demonstrated that the amounts of divinylbenzene and methacrylate, the volume ratio of porogents, and the dosage amount of ferrofluids affected the specific surface area of magnetic microspheres as well. Furthermore, results showed that obtained magnetic microspheres had a superparamagnetic behavior at room temperature due to the existence of Fe3O4crystalline structure. The results showed that magnetic microspheres had a high adsorption capacity and high separation efficiency (removal ratio reach to99.32%), due to their porous structure, polar groups, and superparamagnetic properties.
(2) Ten kinds of Fe3O4/poly(styrene-co-divinylbenzene) microspheres were synthesized by emulsion polymerization with oleic acid coated Fe3O4nanoparticles as magnetic core, and styrene and divinylbenzene as monomer. Then, the above obtained microspheres were used to fourteen kinds of prepare Fe3O4/poly(styrene-co-divinylbenzene)/SiO2microspheres by sol-gel technology in the presence of tetraethoxysilane. The effects of the composite of monomer, the kinds of surfactant, and the content of oleic acid coated Fe3O4nanoparticles on the morphology, magnetic content and size of microspheres were investigated. The magnetic hybrid FesU4/poly(St-co-DVB)/SiO2/TiO2photocatalyst was prepared by one-pot solvothermal reactions by using the above silica modified microspheres as magnetic matrix. We investigated the catalytic property of as-prepared magnetic hybrid photocatalyst on the degration of RhodamineB (RhB). The results showed that the magnetic hybrid photocatalysts exhibited good photocatalytic activity under UV light irradiation and could be reused five times by magnetic separation without major loss of activity, and the degradation ratio of RhB still reached to90%.
(3) Three series of magnetic poly(hexachlorocyclotriphosphazene-co-4,4'-dihydroxydiphenylsulfone) were synthesized with different structures and morphologies. Firstly, Fe3O4microspheres with hollow porous structures were prepared by hydrothermal method, and were used as the magnetic core to fabricate hollow porous Fe3O4/mSiO2and hollow Fe3O4/nSiO2microspheres, in the presence of TEOS and CTAB; Then, hollow porous Fe3O4/mSiO2/PZS and hollow Fe3O4/nSiO2/PZS microspheres were prepared by using BPS and HCCP as the monomer, hollow porous Fe3O4/mSiO2and hollow Fe3O4/nSiO2microspheres as magnetic matrix, respectively. Secondly, Fe3O4/OA nanoparticles were prepared by co-precipitation method, and were used as magnetic core to frabricate Fe3O4/PZS magnetic nanowires by inclusion polymerization with BPS and HCCP as monomer, in the presence of TEA. Thirdly, Fe3O4/PZS magnetic nanowires were prepared by in-situ polymerization method with as-prepared Fe3O4nanowires as magnetic core, BPS and HCCP as monomer, in the presence of TEA. The effects of experimental conditions on the morphology, size and performance of as-synthesized products were investigated. The morphology, structure and magnetic content of obtained products were examined by means of SEM, TEM, TGA and XRD, respectively. Moreover, the particle size of the products was characterized by dynamic light scattering (DLS) and nanomeasurer analyses, and the magnetic property of the products was measured by SQUID, and the specific surface area and pore structure of the products were characterized by nitrogen adsorption-desorption analyzer. In addition, the above-prepared magnetic polyphosphazene-containing materials were used as magnetic matrix to prepare Fe3O4/mSiO2/PZS/Fc microspheres by the esterification reaction, and magnetic polyphosphazenes-containing gold nanocatalysts by the chemical deposition method with HAuCl4as gold source, respectively. Furthermore, catalytic activity and reusability of these magnetic polyphosphazenes-containing gold nanocatalysts was investigated by choosing a model reaction, reduction reaction of n-nitroaniline to benzenediamine by NaBH4. It was found that as-prepared polyphosphazenes-based magnetic nanocatalysts had good hydrophilicity, good thermal stability, biocompatibility and better magnetic response ability and so on, and had good prospect in the field of industrial applications.
本论文围绕四氧化三铁基磁性聚合物材料的制备、结构表征、形貌表征、磁性能、吸附性能和催化性能等,展开对不同形貌、结构和组成的四氧化三铁基磁性聚合物材料的合成、磁分离性能以及催化性能的研究：
(1)以油酸包覆的Fe3O4纳米粒子作为磁核,以MMA和DVB作为单体,分别使用正已烷、环已烷、甲苯等小分子致孔剂,采用改性悬浮聚合制备了10种磁性多孔微球(FMD),用氮气吸脱附法和压汞法表征了产物的孔结构,用TEM和SEM观察了产物的形貌,用TGA考察了四氧化三铁的包覆率。并尝试利用UV考察其脱除水体中的苯酚的能力。研究发现,FMD微球中存在类似于墨水瓶状孔的小口径大腹腔的孔。致孔剂类型和用量对FMD微球孔结构的影响是显著而复杂的。使用两种体系良溶剂作致孔剂(环已烷(CHX)和正已烷(n-HX))制备的产物均具有相对较高的比表面积。减少致孔剂用量,增加交联剂DVB的用量,都有利于形成较为完整的交联网络,从而提高FMD微球的四氧化三铁包覆率。此外,增加磁流体的用量,也可以提高四氧化三铁的包覆率。FMD磁性微球表现出明显Fe304晶相结构,并在室温下,表现为超顺磁性。研究发现,FMD磁性多孔微球可有效地去除水溶液中的苯酚,去除率可达99.32%。
(2)以油酸包覆的Fe304纳米粒子作为磁核,以St和DVB作为单体,采用乳液聚合法制备了10种磁性Fe3O4/poly (St-co-DVB)微球,进一步以TEOS为硅源,制备了14种Fe3O4/poly (St-co-DVB)/SiO2有机/无机杂化的磁性微球。考察了单体组成、表面活性剂类型和磁流体的加入量对微球表面形貌、四氧化三铁包覆率及微球粒径等的影响。然后尝试以上述微球作为磁性基体,采用了水热法制备了Fe3O4/poly (St-co-DVB)/SiO2/TiO2磁性纳米催化剂,进一步研究其对罗丹明B(RhB)降解的光催化性能。研究发现,所制备的磁性纳米催化剂可在UV照射下有效地降解RhB。重复使用5次,其RhB的降解率仍在90%以上,仍具有高效的催化效果。此催化剂因其采用磁性无机.有机杂化磁性微球作为磁性基体,易于磁分离,有利于工业化使用。
(3)制备了三个系列不同结构和形貌的磁性聚(六氯环三磷腈-co-双酚S)。以水热法制备了16种中空多孔的Fe3O4微球,并以此为磁核,以TEOS为硅源,在CTAB的存在下,在制得的Fe3O4微球外层包覆一层介孔二氧化硅制备了6种中空多孔Fe3O4/mSiO2和1种中空Fe3O4/nSiO2微球,再以BPS和HCCP作为单体,制备了4种中空多孔Fe3O4/mSiO2/PZS和4种中空Fe3O4/nSiO2/PZS微球。以共沉淀法制备的4种Fe3O4/OA纳米粒子为磁核,以BPS和HCCP作为单体,在TEA存在下,制备了9种Fe3O4/PZS磁性纳米线。以水热法制备了21种Fe304纳米线,并以此为磁核,以BPS和HCCP作为单体,在TEA存在下,制备了5种Fe3O4/PZS磁性纳米线。使用TEM和SEM观察了产物的形貌,用TGA考察了四氧化三铁的包覆率,XRD表征了产物的晶相结构,并采用DLS和SEM测试了产物的粒径,用SQUID测试了产物的磁性能,采用氮气吸脱附法表征了产物的比表面积和孔结构,此外,以上述制备的磁性聚磷腈复合材料为磁性基体,分别以Fe3O4/mSiO2/PZS为磁性基体,以二茂铁二甲酰氯为原料,利用酯化反应制备了Fe3O4/mSiO2/PZS/Fc磁性微球;以HAuCl4作为金源,采用化学沉积法制备了13种磁性聚磷腈纳米金催化剂,其对4.硝基苯酚在NaBH4存在下还原反应有较好的催化性能,并且此催化剂可循环使用。所得的聚膦腈磁性材料具有良好亲水性、良好热稳定性、生物相容性及较好的磁响应能力等等,有良好的工业应用前景。
Fe3O4-based magnetic polymer composite materials have been applied in many areas, including magnetic separation, catalysis, biomedical, bio-medicine and so on, because of their unique superparamagnetic, biocompatibility and excellent optical, catalytic and adsorption properties.
In this thesis, we have focused on the studies of synthesis, structure, morphology, magnetic property, adsorption property and catalytic activity of the Fe3O4-based magnetic polymer composite materials. We have studied the synthesis, magnetic separation and catalytic property of Fe3O4-based magnetic polymer composite materials which have different morphology, structure, composite.
(1) Ten different magnetic porous microspheres (FMD) were synthesized by modified suspension polymerization of methacrylate and divinylbenzene, in the presence of oleic acid coated Fe3O4nanopaticles, using n-hexane, cyclohexane, toluene as small molecules progent, respectively. The morphologies and properties of the magnetic porous microspheres were charaterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), superconducting quantum interference device (SQUID), Fourier transform infrared spectroscopy (FT-IR), thermogravimetry (TGA), and X-ray powder diffraction (XRD). The pore size distribution and the specific surface area of magnetic porous microspheres were measured by nitrogen sorption and mercury porosimetry technique. The obtained microspheres were applied in the removal of phenol from aqueous solution, and the concentration of phenol aqueous solutions was measured by ultraviolet analyses (UV). It was found that magnetic porous microspheres had the ink bottle shape hole, some minor-caliber and big celiac hole. The amount and type of progents complicated and dramaticlly affected the pore structure of FMD microsphere. The magnetic porous microspheres possessed a high specific surface area by using n-hexane and cyclehexane as porogent. It was further demonstrated that the amounts of divinylbenzene and methacrylate, the volume ratio of porogents, and the dosage amount of ferrofluids affected the specific surface area of magnetic microspheres as well. Furthermore, results showed that obtained magnetic microspheres had a superparamagnetic behavior at room temperature due to the existence of Fe3O4crystalline structure. The results showed that magnetic microspheres had a high adsorption capacity and high separation efficiency (removal ratio reach to99.32%), due to their porous structure, polar groups, and superparamagnetic properties.
(2) Ten kinds of Fe3O4/poly(styrene-co-divinylbenzene) microspheres were synthesized by emulsion polymerization with oleic acid coated Fe3O4nanoparticles as magnetic core, and styrene and divinylbenzene as monomer. Then, the above obtained microspheres were used to fourteen kinds of prepare Fe3O4/poly(styrene-co-divinylbenzene)/SiO2microspheres by sol-gel technology in the presence of tetraethoxysilane. The effects of the composite of monomer, the kinds of surfactant, and the content of oleic acid coated Fe3O4nanoparticles on the morphology, magnetic content and size of microspheres were investigated. The magnetic hybrid FesU4/poly(St-co-DVB)/SiO2/TiO2photocatalyst was prepared by one-pot solvothermal reactions by using the above silica modified microspheres as magnetic matrix. We investigated the catalytic property of as-prepared magnetic hybrid photocatalyst on the degration of RhodamineB (RhB). The results showed that the magnetic hybrid photocatalysts exhibited good photocatalytic activity under UV light irradiation and could be reused five times by magnetic separation without major loss of activity, and the degradation ratio of RhB still reached to90%.
(3) Three series of magnetic poly(hexachlorocyclotriphosphazene-co-4,4'-dihydroxydiphenylsulfone) were synthesized with different structures and morphologies. Firstly, Fe3O4microspheres with hollow porous structures were prepared by hydrothermal method, and were used as the magnetic core to fabricate hollow porous Fe3O4/mSiO2and hollow Fe3O4/nSiO2microspheres, in the presence of TEOS and CTAB; Then, hollow porous Fe3O4/mSiO2/PZS and hollow Fe3O4/nSiO2/PZS microspheres were prepared by using BPS and HCCP as the monomer, hollow porous Fe3O4/mSiO2and hollow Fe3O4/nSiO2microspheres as magnetic matrix, respectively. Secondly, Fe3O4/OA nanoparticles were prepared by co-precipitation method, and were used as magnetic core to frabricate Fe3O4/PZS magnetic nanowires by inclusion polymerization with BPS and HCCP as monomer, in the presence of TEA. Thirdly, Fe3O4/PZS magnetic nanowires were prepared by in-situ polymerization method with as-prepared Fe3O4nanowires as magnetic core, BPS and HCCP as monomer, in the presence of TEA. The effects of experimental conditions on the morphology, size and performance of as-synthesized products were investigated. The morphology, structure and magnetic content of obtained products were examined by means of SEM, TEM, TGA and XRD, respectively. Moreover, the particle size of the products was characterized by dynamic light scattering (DLS) and nanomeasurer analyses, and the magnetic property of the products was measured by SQUID, and the specific surface area and pore structure of the products were characterized by nitrogen adsorption-desorption analyzer. In addition, the above-prepared magnetic polyphosphazene-containing materials were used as magnetic matrix to prepare Fe3O4/mSiO2/PZS/Fc microspheres by the esterification reaction, and magnetic polyphosphazenes-containing gold nanocatalysts by the chemical deposition method with HAuCl4as gold source, respectively. Furthermore, catalytic activity and reusability of these magnetic polyphosphazenes-containing gold nanocatalysts was investigated by choosing a model reaction, reduction reaction of n-nitroaniline to benzenediamine by NaBH4. It was found that as-prepared polyphosphazenes-based magnetic nanocatalysts had good hydrophilicity, good thermal stability, biocompatibility and better magnetic response ability and so on, and had good prospect in the field of industrial applications.
引文
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