环境有害物质分离富集新材料的合成、表征及应用研究
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摘要
样品前处理技术作为环境有害物质富集、分离与分析的关键技术,备受研究者的广泛关注,其中固相萃取和固相微萃取是目前环境有害物质前处理中广泛应用的技术,而使用的萃取填料将直接决定其对样品中环境有害物质富集分离的效率。因此,开发新型、高效的富集分离材料成为目前该领域的研究热点,也是复杂体系分离分析科学中具有重要意义的研究课题。本文综述了磁性材料、介孔材料以及分子印迹聚合物材料的类型、合成及改性方法、结构特征和性能、及在环境有害物质分离富集等方面的研究进展和发展趋势；研究了均一单分散的磁性核壳碳纳米球的合成、表征及对水体中葸的吸附性能；制备了CeSiO4负载的CeSBA-15介孔材料,并考察了其对环己烷中苯并(a)芘的吸附性能,探讨了其吸附机理；合成了均一单分散的中空分子印迹聚合物纳米球,考察了其对双酚A的吸附以及选择性分离富集性能；合成了具有高比表面积、均一孔径的中空多空分子印迹聚合物纳米球,考察了其对双酚A的吸附以及选择性分离富集性能。
采用改进的Stober法,在水溶液中以间苯二酚和甲醛为前体物制备了Fe3O4@polymer,后经高温碳化得到Fe3O4@C纳米球。使用SEM和TEM对其进行了表征,发现制得的Fe3O4@C具有较好的均一性和单分散度。对合成过程进行了优化,得出影响Fe3O4@polymer的成功合成的关键因素为氨水的浓度和Fe304纳米球表面的柠檬酸基团。通过简单调节反应前体物与Fe304纳米球的质量比例,可以很容地调控Fe3O4@C纳米球的碳壳厚度。以Fe3O4@C作为水体中蒽的分离富集材料,发现Fe3O4@C对蒽具有较快的吸附速率以及较大的平衡吸附容量,这将使其在环境污染物的快速分离富集方面展现较好的应用前景。
采用pH调节原位一步水热法,以三乙胺为碱源,制备了CeSiO4负载的Ce-SBA-15介孔材料。采用粉末X射线衍射、TEM以及氮气吸附-脱附等手段对样品的结构特征进行了表征。结果表明,合成的Ce-SBA-15材料具有均一的大孔分布、高的比表面积、较好的结构有序性；同时发现在预合成的以及焙烧后的Ce-SBA-15样品中均观察到了活性的CeSiO4物相,并均匀地分散在介孔的孔道中。考察了不同铈掺杂量的Ce-SBA-15材料对环己烷溶液中苯并(a)芘的吸附性能,结果表明铈的掺杂量对吸附结果有很大的影响。通过对吸附现象的观察以及对材料吸附苯并(a)芘后的甲醇洗脱液的IR、UV-vis、FLD、EI和NMR等表征,提出了可能的吸附机理,即苯并(a)芘先被吸附到Ce-SBA-15介孔材料上,然后由CeSiO4物相通过自由基氧化机理将其氧化成苯并芘醌,提高了其极性,从而大大提高其对环己烷中苯并(a)芘的吸附性能。
采用一步沉淀聚合技术,以未改性的SiO2球为硬模板,利用功能单体的羰基与SiO2球表面Si-OH的酯化反应来促进分子印迹聚合物包裹在SiO2球表面得到SiO2@MIPs,后经HF刻蚀同时去除SiO2和印迹分子,得到中空分子印迹聚合物纳米球(MHMIPs)。采用SEM和TEM等手段对样品的形貌特征进行了表征,结果表明所制得的SiO2@MIPs和MHMIPs具有较好的均一性和单分散度。优化了印迹前体物的功能单体比例,得出了具有较大吸附容量以及较好选择性的最佳功能单体比例,即BPA:MMA:EGDMA=1:6:20;通过简单调节印迹前体物与SiO2纳米球的质量比例,可以很容地调控印迹壳的厚度；比较了具有不同厚度的MHMIPs对双酚A(BPA)的吸附性能,发现壳厚度的增大对于MHMIPs对BPA的吸附容量的提高是不利的。考察了MHMIPs和MHNIPs对BPA及其结构类似物的吸附性能,结果表明MHMIPs对BPA具有较快的吸附速率以及高的吸附容量,对由BPA及其结构类似物组成的混合液中BPA的吸附具有较高的选择性富集性能。
以介孔SiO2作“纳米反应器”及硬模板,双酚A为印迹分子、4-乙烯基吡啶为功能单体、乙二醇二甲基丙烯酸酯为交联剂,采用控制浸渍策略和刻蚀技术,制备了中空多空分子印迹聚合物纳米球。采用SEM、TEM和BET等手段对样品的形貌及物理结构性能进行了表征,结果表明所制得的印迹聚合物具有中空球形结构,比表面积高达607m2·g-1,孔径分布均一。考察了HPMIPs和HPNIPs对BPA及其结构类似物的吸附性能,结果表明HPMIPs对BPA具有教高的吸附容量以及快的吸附速率,对由BPA及其结构类似物组成的混合液中BPA的吸附具有较高的选择性富集性能。
Sample pretreatment techniques as the key technique of enrichment, separation and analysis of environmentally hazardous substances have caused wide concern, in which the solid phase extraction and solid phase microextraction is widely used, while the used extraction packing will directly determine the efficiency of preconcentration and separation of the sample. Therefore, the development of novel and efficient enrichment separation materials has become a research hotspot in this field, it also plays an important role of separation and analysis of complex system science.
This thesis summarized the type, synthesis and modification methods, structural characteristics and properties of magnetic materials, mesoporous materials and molecular imprinted polymer materials, as well as the current progress and development trend of separation and enrichment of environmentally hazardous substances; studied the synthesis and characterization of uniform and monodisperse magnetic core-shell carbon nanospheres, and its adsorption performance for anthracene in water; prepared Ce-SBA-15, an mesoporous material loaded by CeSiO4, and investigated its adsorption properties for B(a)P in cyclohexane solution, also discussed the adsorption mechanism; synthesized uniform monodispersed hollow molecular imprinted polymer nanospheres and investigated the adsorption of bisphenol A and selective enrichment and separation performance; synthesized hollow porous molecular imprinted polymer nanospheres with high specific surface area and uniform pore size, and investigated the adsorption of bisphenol A and selective enrichment and separation performance.
By adopting improved Stober method, using resorcinol and formaldehyde as precursor in aqueous solution to prepare Fe3O4@polymer, after high temperature carbonization, Fe3O4@C nanoparticles were obtained. The SEM and TEM were used to characterize the prepared Fe3O4@C, found that Fe3O4@C has fairly good uniformity and dispersion. By optimizing the synthesis process, found that the concentration of ammonia and group citric acid on the surface of Fe3O4nanoparticles were the key factors to influence the successful synthesis of Fe3O4@polymer. By simple adjusting the mass ratio of the reaction precursor and Fe3O4nanoparticles, carbon shell thickness of Fe3O4@C nanoparticles can be controlled easily. Taking Fe3O4@C as the separation and enrichment materials of anthracene in aqueous solution, found that Fe3O4@C has a fairly high adsorption rate and large equilibrium adsorption capacity for anthracene, which shows good application prospect in the rapid separation and enrichment of environmental pollutants.
Using in situ one-step hydrothermal method, with three triethylamine as alkali source, Ce-SBA-15mesoporous materials were prepared loading by the CeSiO4. By using XRD, TEM and nitrogen adsorption/desorption to characterize the structures of the samples, the results showed that, the component material Ce-SBA-15possessed relatively large specific surface area and uniform pore diameter distribution, also the structures were highly ordered. At the same time the active CeSiO4phase were observed in the pre-synthesised and the calcined Ce-SBA-15samples, and uniformly dispersed in the mesoporous pore. Through the study of adsorbability of the Ce-SBA-15material with different doping amount of cerium for B(a)P in cyclohexane solution, the results show that the amount of doped cerium has great influence on the adsorption results. Through the observation of the adsorption phenomena and characterization of IR, UV-vis, FLD, El and NMR of methanol eluent of materials after adsorption B(a)P, the possible adsorption mechanism is proposed, that is B(a)P was first adsorbed onto the Ce-SBA-15mesoporous materials, and then the CeSiO4phase oxidizing B(a)P into benzo(a)pyrene-6,12-quinone with high polarity by a free radical oxidation mechanism, which greatly improves the adsorption performance of Ce-SBA-15mesoporous materials for B(a)P in cyclohexane.
Through one-step precipitation polymerization technique, using unmodified SiO2ball as hard template, taking advantage of esterification of the carbonyl of functional monomers and Si-OH on the surface of SiO2sphere to promote the molecularly imprinted polymer coating on the surface of SiO2sphere to obtain SiO2@MIPs, and then by HF etching to simultaneous remove SiO2and molecular imprinting to obtain the hollow molecularly imprinted polymer nanospheres (MHMIPs). SEM and TEM techniques were used to characterize the characteristics of the sample, the results show that the prepared SiO2@MIPs and MHMIPs have fairly uniformity and dispersion. By optimizing ratio of functional monomer of the imprinted precursor, the right ratio of functional monomer which has high adsorption amount and excellent selectivity was found, that is BPA:MMA:EGDMA=1:6:20; by adjusting the mass ratio of imprinted precursor and SiO2nanoparticles, thickness of imprinted shell can be easily adjusted; by comparing adsorption performance of MHMIPs with different thickness for bisphenol A (BPA), it shows that the increase of shell thickness is detrimental to improve the adsorption capacity of MHMIPs for BPA. The adsorption properties of BPA and other structural analogues on MHMIPs and MHNIPs were studied, the results show that the MHMIPs has higher adsorption rate and high adsorption capacity for BPA, and has high selectivity enrichment performance for BPA in mixed solution of BPA and its structural analogs.
Using mesoporous SiO2as "nanoreactors" and hard template, bisphenol A as template molecule,4-vinylpyridine as functional monomer, EGDMA as crosslinking agent, through the control dipping strategy and the etching technology, hollow porous molecular imprinted polymer nanospheres were prepared. SEM, TEM and BET were employed to characterize the morphology and physical properties, the results show that the prepared molecularly imprinted polymers possess hollow spherical structure and high specific surface area up to607m2·g-1, the pore size distribution is uniform. The adsorption properties of HPMIPs and HPNIPs for BPA and other structural analogues were studied, the results show that the HPMIPs has higher adsorption rate and high adsorption capacity for BPA, and has high selectivity of enrichment performance on adsorption of BPA in mixed solution of BPA and its structural analogs.
采用改进的Stober法,在水溶液中以间苯二酚和甲醛为前体物制备了Fe3O4@polymer,后经高温碳化得到Fe3O4@C纳米球。使用SEM和TEM对其进行了表征,发现制得的Fe3O4@C具有较好的均一性和单分散度。对合成过程进行了优化,得出影响Fe3O4@polymer的成功合成的关键因素为氨水的浓度和Fe304纳米球表面的柠檬酸基团。通过简单调节反应前体物与Fe304纳米球的质量比例,可以很容地调控Fe3O4@C纳米球的碳壳厚度。以Fe3O4@C作为水体中蒽的分离富集材料,发现Fe3O4@C对蒽具有较快的吸附速率以及较大的平衡吸附容量,这将使其在环境污染物的快速分离富集方面展现较好的应用前景。
采用pH调节原位一步水热法,以三乙胺为碱源,制备了CeSiO4负载的Ce-SBA-15介孔材料。采用粉末X射线衍射、TEM以及氮气吸附-脱附等手段对样品的结构特征进行了表征。结果表明,合成的Ce-SBA-15材料具有均一的大孔分布、高的比表面积、较好的结构有序性；同时发现在预合成的以及焙烧后的Ce-SBA-15样品中均观察到了活性的CeSiO4物相,并均匀地分散在介孔的孔道中。考察了不同铈掺杂量的Ce-SBA-15材料对环己烷溶液中苯并(a)芘的吸附性能,结果表明铈的掺杂量对吸附结果有很大的影响。通过对吸附现象的观察以及对材料吸附苯并(a)芘后的甲醇洗脱液的IR、UV-vis、FLD、EI和NMR等表征,提出了可能的吸附机理,即苯并(a)芘先被吸附到Ce-SBA-15介孔材料上,然后由CeSiO4物相通过自由基氧化机理将其氧化成苯并芘醌,提高了其极性,从而大大提高其对环己烷中苯并(a)芘的吸附性能。
采用一步沉淀聚合技术,以未改性的SiO2球为硬模板,利用功能单体的羰基与SiO2球表面Si-OH的酯化反应来促进分子印迹聚合物包裹在SiO2球表面得到SiO2@MIPs,后经HF刻蚀同时去除SiO2和印迹分子,得到中空分子印迹聚合物纳米球(MHMIPs)。采用SEM和TEM等手段对样品的形貌特征进行了表征,结果表明所制得的SiO2@MIPs和MHMIPs具有较好的均一性和单分散度。优化了印迹前体物的功能单体比例,得出了具有较大吸附容量以及较好选择性的最佳功能单体比例,即BPA:MMA:EGDMA=1:6:20;通过简单调节印迹前体物与SiO2纳米球的质量比例,可以很容地调控印迹壳的厚度；比较了具有不同厚度的MHMIPs对双酚A(BPA)的吸附性能,发现壳厚度的增大对于MHMIPs对BPA的吸附容量的提高是不利的。考察了MHMIPs和MHNIPs对BPA及其结构类似物的吸附性能,结果表明MHMIPs对BPA具有较快的吸附速率以及高的吸附容量,对由BPA及其结构类似物组成的混合液中BPA的吸附具有较高的选择性富集性能。
以介孔SiO2作“纳米反应器”及硬模板,双酚A为印迹分子、4-乙烯基吡啶为功能单体、乙二醇二甲基丙烯酸酯为交联剂,采用控制浸渍策略和刻蚀技术,制备了中空多空分子印迹聚合物纳米球。采用SEM、TEM和BET等手段对样品的形貌及物理结构性能进行了表征,结果表明所制得的印迹聚合物具有中空球形结构,比表面积高达607m2·g-1,孔径分布均一。考察了HPMIPs和HPNIPs对BPA及其结构类似物的吸附性能,结果表明HPMIPs对BPA具有教高的吸附容量以及快的吸附速率,对由BPA及其结构类似物组成的混合液中BPA的吸附具有较高的选择性富集性能。
Sample pretreatment techniques as the key technique of enrichment, separation and analysis of environmentally hazardous substances have caused wide concern, in which the solid phase extraction and solid phase microextraction is widely used, while the used extraction packing will directly determine the efficiency of preconcentration and separation of the sample. Therefore, the development of novel and efficient enrichment separation materials has become a research hotspot in this field, it also plays an important role of separation and analysis of complex system science.
This thesis summarized the type, synthesis and modification methods, structural characteristics and properties of magnetic materials, mesoporous materials and molecular imprinted polymer materials, as well as the current progress and development trend of separation and enrichment of environmentally hazardous substances; studied the synthesis and characterization of uniform and monodisperse magnetic core-shell carbon nanospheres, and its adsorption performance for anthracene in water; prepared Ce-SBA-15, an mesoporous material loaded by CeSiO4, and investigated its adsorption properties for B(a)P in cyclohexane solution, also discussed the adsorption mechanism; synthesized uniform monodispersed hollow molecular imprinted polymer nanospheres and investigated the adsorption of bisphenol A and selective enrichment and separation performance; synthesized hollow porous molecular imprinted polymer nanospheres with high specific surface area and uniform pore size, and investigated the adsorption of bisphenol A and selective enrichment and separation performance.
By adopting improved Stober method, using resorcinol and formaldehyde as precursor in aqueous solution to prepare Fe3O4@polymer, after high temperature carbonization, Fe3O4@C nanoparticles were obtained. The SEM and TEM were used to characterize the prepared Fe3O4@C, found that Fe3O4@C has fairly good uniformity and dispersion. By optimizing the synthesis process, found that the concentration of ammonia and group citric acid on the surface of Fe3O4nanoparticles were the key factors to influence the successful synthesis of Fe3O4@polymer. By simple adjusting the mass ratio of the reaction precursor and Fe3O4nanoparticles, carbon shell thickness of Fe3O4@C nanoparticles can be controlled easily. Taking Fe3O4@C as the separation and enrichment materials of anthracene in aqueous solution, found that Fe3O4@C has a fairly high adsorption rate and large equilibrium adsorption capacity for anthracene, which shows good application prospect in the rapid separation and enrichment of environmental pollutants.
Using in situ one-step hydrothermal method, with three triethylamine as alkali source, Ce-SBA-15mesoporous materials were prepared loading by the CeSiO4. By using XRD, TEM and nitrogen adsorption/desorption to characterize the structures of the samples, the results showed that, the component material Ce-SBA-15possessed relatively large specific surface area and uniform pore diameter distribution, also the structures were highly ordered. At the same time the active CeSiO4phase were observed in the pre-synthesised and the calcined Ce-SBA-15samples, and uniformly dispersed in the mesoporous pore. Through the study of adsorbability of the Ce-SBA-15material with different doping amount of cerium for B(a)P in cyclohexane solution, the results show that the amount of doped cerium has great influence on the adsorption results. Through the observation of the adsorption phenomena and characterization of IR, UV-vis, FLD, El and NMR of methanol eluent of materials after adsorption B(a)P, the possible adsorption mechanism is proposed, that is B(a)P was first adsorbed onto the Ce-SBA-15mesoporous materials, and then the CeSiO4phase oxidizing B(a)P into benzo(a)pyrene-6,12-quinone with high polarity by a free radical oxidation mechanism, which greatly improves the adsorption performance of Ce-SBA-15mesoporous materials for B(a)P in cyclohexane.
Through one-step precipitation polymerization technique, using unmodified SiO2ball as hard template, taking advantage of esterification of the carbonyl of functional monomers and Si-OH on the surface of SiO2sphere to promote the molecularly imprinted polymer coating on the surface of SiO2sphere to obtain SiO2@MIPs, and then by HF etching to simultaneous remove SiO2and molecular imprinting to obtain the hollow molecularly imprinted polymer nanospheres (MHMIPs). SEM and TEM techniques were used to characterize the characteristics of the sample, the results show that the prepared SiO2@MIPs and MHMIPs have fairly uniformity and dispersion. By optimizing ratio of functional monomer of the imprinted precursor, the right ratio of functional monomer which has high adsorption amount and excellent selectivity was found, that is BPA:MMA:EGDMA=1:6:20; by adjusting the mass ratio of imprinted precursor and SiO2nanoparticles, thickness of imprinted shell can be easily adjusted; by comparing adsorption performance of MHMIPs with different thickness for bisphenol A (BPA), it shows that the increase of shell thickness is detrimental to improve the adsorption capacity of MHMIPs for BPA. The adsorption properties of BPA and other structural analogues on MHMIPs and MHNIPs were studied, the results show that the MHMIPs has higher adsorption rate and high adsorption capacity for BPA, and has high selectivity enrichment performance for BPA in mixed solution of BPA and its structural analogs.
Using mesoporous SiO2as "nanoreactors" and hard template, bisphenol A as template molecule,4-vinylpyridine as functional monomer, EGDMA as crosslinking agent, through the control dipping strategy and the etching technology, hollow porous molecular imprinted polymer nanospheres were prepared. SEM, TEM and BET were employed to characterize the morphology and physical properties, the results show that the prepared molecularly imprinted polymers possess hollow spherical structure and high specific surface area up to607m2·g-1, the pore size distribution is uniform. The adsorption properties of HPMIPs and HPNIPs for BPA and other structural analogues were studied, the results show that the HPMIPs has higher adsorption rate and high adsorption capacity for BPA, and has high selectivity of enrichment performance on adsorption of BPA in mixed solution of BPA and its structural analogs.
引文
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