新型功能化吸附材料的制备及其分离富集痕量组分的应用研究
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摘要
经济和工业生产的快速发展，导致重金属离子和有毒有机小分子的消耗和排放与日俱增，造成日趋严重的环境污染。准确测定地质、生物和环境样品中的痕量元素是分析化学中的一项十分重要的研究内容。虽然现代分析仪器有了很大的发展，但在进行地质、生物、环境、农业和工业等样品中的痕量和超痕量组分分析时，由于方法的灵敏度不够及大量共存元素的干扰，直接测定常常很困难。所以在分析实践中，复杂样品需要经过一定的预处理——富集分离以后才能进入分析仪器进行准确的测定。而样品的富集分离通常需要借助选择性高、吸附容量大的各种吸附材料和合适的分离方法。因此，本论文以建立痕量组分的富集分离及分析为目的，合成了几种功能化吸附分离材料，并对材料的选择性吸附性能开展了系统研究。同时，对纳米氢氧化镍电极材料进行了研究。主要进行了以下几方面的研究工作。
1．应用硅胶表面印迹技术，以Fe(Ⅲ)，Ni(Ⅱ)和Al(Ⅲ)为印迹离子、3-氨基丙基-三乙氧基硅烷为功能单体，制备了Fe(Ⅲ)，Ni(Ⅱ)和Al(Ⅲ)的氨基功能化表面印迹聚合物。研究了印迹聚合物和非印迹聚合物对Fe(Ⅲ)，Ni(Ⅱ)和Al(Ⅲ)的分离富集特性。结果如下：(1)相比传统吸附剂和非印迹材料，Fe(Ⅲ)印迹聚合物对Fe(Ⅲ)具有较好的选择性和吸附容量。Fe(Ⅲ)印迹聚合物和非印迹聚合物的最大静态吸附容量分别是25．21和5．10mg g~(-1)；在Fe(Ⅲ)和Cr(Ⅲ)的相同浓度的混合溶液中，Fe(Ⅲ)印迹硅胶对Fe(Ⅲ)的最大选择性系数为451，Fe(Ⅲ)／Cr(Ⅲ)的相对选择性因子为49．9。Fe(Ⅲ)印迹硅胶固相萃取痕量铁的检出限为0．34μg L~(-1)，方法的相对标准偏差为1．5％，将该法用于水样和植物样品中痕量Fe(Ⅲ)的测定，得到满意的结果。(2)相比传统吸附剂和非印迹硅胶，Ni(Ⅱ)印迹吸附剂对Ni(Ⅱ)具有很高的吸附选择性和吸附容量。Ni(Ⅱ)印迹聚合物和非印迹聚合物的最大静态吸附容量分别是12．61和4．25mg g~(-1)；在Ni(Ⅱ)和干扰离子具有相同浓度的混合溶液中，Ni(Ⅱ)／Cu(Ⅱ)，Ni(Ⅱ)／Co(Ⅱ)，Ni(Ⅱ)／Zn(Ⅱ)和Ni(Ⅱ)／Pd(Ⅱ)的相对选择性因子分别为45．99，32．83，43．79和28．36。Ni(Ⅱ)印迹硅胶固相萃取痕量Ni(Ⅱ)的检出限为0．16μg L~(-1)，该方法的相对标准偏差为1．48％，将该法用于水样和植物样品中痕量Ni(Ⅱ)的测定，得到满意的结果。(3)相比传统吸附剂和非印迹硅胶，Al(Ⅲ)印迹吸附剂对Al(Ⅲ)具有很高的吸附选择性和吸附容量。Al(Ⅲ)印迹聚合物和非印迹聚合物的最大静态吸附容量分别是11．46mg g~(-1)和6．28mg g~(-1)；在Al(Ⅲ)和干扰离子Cr(Ⅲ)具有相同浓度的混合溶液中，Al(Ⅲ)／Cr(Ⅲ)的相对选择性因子分别为6．73。Al(Ⅲ)印迹硅胶固相萃取痕量Al(Ⅲ)的检出限为0．36μg L~(-1)，该方法的相对标准偏差为3．2％。
2．以丙烯酰胺为功能单体、季戊四醇三丙烯酸酯为交联剂、偶氮二异丁腈做引发剂，以姜黄素分子作模板分子制备了姜黄素分子的印迹聚合物，研究了印迹聚合物和非印迹聚合物对姜黄素分子的选择吸附性能。结果表明，经过印迹的聚合物对模板分子具有很好的特异性结合能力，为复杂样品中的姜黄素物质的选择性富集及快速检测提供了新的途径。
3．采用加表面活性剂于缓冲溶液中的化学沉淀法直接合成了具有纳米结构特征的氢氧化镍／碳纳米管(CNTs)粉末。分析了不同直径和含量的CNTs对Ni(OH)_2电化学性能的影响。首先，CNTs被分散在氢氧化钠溶液中，然后在合成纳米Ni(OH)_2的过程中引入CNTs，经过化学反应形成复合材料。本实验中，分别选用了10-20nm、20-40nm、60-100nm质量百分含量分别为2wt％、5wt％、10wt％、25wt％和50wt％的CNTs，结果发现合成过程中用20-40nm 25wt％的CNTs的复合材料电化学性能最好。其放电比容量可以达到280mAh／g，而且比较稳定，循环寿命长。同时将超声波条件引入合成过程中，可以使电极在充放电效率、放电比容量、活性物质利用率、放电电压、抗膨胀能力及高速率放电性能等方面得到明显改善和提高。
The rapid development of science, technology and proceeding industrializationleads to the consumption and draining of heavy metals and organic substance. Thepollution caused by heavy metals and poisonous organic substance become more andmore serious. The accurate determination of trace element in geological, biologicaland environmental samples is very important in analytical chemistry. Although manyinstrument analysis methods have been developed recently and reached trace level orsuper trace level sensitivity, the direct analysis is still difficult because of the highcomplexity of samples and severe interference caused by matrix effects. So, variouspre-treatment procedures are necessary before the more accurate measurement byanalytical instruments. It is obvious that the pre-treatment procedures of traceelements depend on appropriate separation methods and different functionaladsorption materials with higher selectivity and adsorption capacity. This papermainly described the preparation of several adsorption materials based on thepre-concentration and separation of trace components. The behaviors of thesematerials that have high selectivity for targets have been studied systematically anddetailedly. At the same time, study on nano-scale nickel hydroxide-CNTs composedmaterial used as electrode material has been done by me. The more detailed noveltyof this work can be categorized as follows:
1. The imprinted and non-imprinted amino-functionalized silica gel adsorbents forFe(Ⅲ), Ni(Ⅱ) and Al(Ⅲ) were obtained by a surface imprinting technique forselective extraction of Fe(Ⅲ), Ni(Ⅱ) and Al(Ⅲ) prior to its determination byICP-AES. The results are: (1) Compared with the traditional solid sorbents andnon-imprinted sorbent, the Fe(Ⅲ)-imprinted amino-functionalized silica gel adsorbentexhibited excellent selectivity and adsorption capacity for Fe(Ⅲ). The maximumstatic adsorption capacity of the Fe(Ⅲ)-imprinted and non-imprinted sorbent forFe(Ⅲ) was 25.21 and 5.10 mg g~(-1), respectively. The largest selectivity coefficient of the Fe(Ⅲ)-imprinted sorbent for Fe(Ⅲ) in the presence of Cr(Ⅲ) that is the sameconcentration with Fe(Ⅲ) was 451. The relatively selective factor (ar) value ofFe(Ⅲ)/Cr(Ⅲ) was 49.9, which were greater than 1. The detection limit (3σ) of themethod was 0.34μg L~(-1). The relative standard deviation (R.S.D.) was 1.5 %. Theproposed method has been successfully applied to the determination and speciation ofiron in biological and water samples with satisfactory results. (2) Compared with thetraditional solid sorbents and non-imprinted sorbent, Ni(Ⅱ)-imprinted sorbent presentshigher selectivity and adsorption capacity for Ni(Ⅱ). The maximum static adsorptioncapacity of the ion-imprinted and non-imprinted sorbent for Ni(Ⅱ) was 12.61 and 4.25mg g~(-1), respectively. The relatively selective factor (α_r) values of Ni(Ⅱ)/Cu(Ⅱ),Ni(Ⅱ)/Co(Ⅱ), Ni(Ⅱ)/Zn(Ⅱ) and Ni(Ⅱ)/Pd(Ⅱ) were 45.99, 32.83, 43.79 and 28.36,which were greater than 1. The detection limit (3σ) of the method was 0.16 ng mL~(-1).The relative standard deviation of the method was 1.48 %. The method wassuccessfully applied to the determination of trace nickel in plants and water sampleswith satisfactory results. (3) Compared with the traditional solid sorbents andnon-imprinted sorbent, Al(Ⅲ)-imprinted sorbent presents higher selectivity andadsorption capacity for Al(Ⅲ). The maximum static adsorption capacity of theion-imprinted and non-imprinted sorbent for Al(Ⅲ) was 11.46 and 6.28 mg g~(-1),respectively. The relatively selective factor (α_r) value of Al(Ⅲ)/Cr(Ⅲ) was 6.73. Therelative standard deviation of the method was 3.2 %. The detection limit (3σ) of themethod was 0.36 ng mL~(-1).
2. A molecularly imprinted polymer was prepared by molecular imprintingtechnique using aerylamide (AA) as monomer, curcumin as template molecule, alarge excess of pentaerythritol triacylate (PETRA) as the cross-linking agent and 2,2-Azobisisobutyronitrile (AIBN) as the initiator. The bulk polymer obtained wasinvestigated in equilibrium binding experiments to evaluate the molecular recognitionand binding characteristics of the curcumin molecularly imprinted polymer. Thesubstrate selectivity of imprinted polymers and non-imprinted polymers wereinvestigated. The results showed that the imprinted polymers exhibited much higher affinity for curcumin among the tested compounds. It is possible to be a goodadsorption and binding material in the selective enrichment and determination of tracecurcumin in complex biosamples.
3. Nanometer Ni(OH)_2 were prepared by chemistry-deposition method with addingthe buffer solution and surfactant. Firstly, carbon nanotubes (CNTs) were dispersed inNaOH solution, then CNTs were chemically synthesized with nanometer Ni(OH)_2. Inthis experiment, 10-20 nm, 20-40 nm, 60-100 nm of 2 wt%, 5 wt%, 10 wt%, 25 wt%and 50 wt% CNTs were used to study the electrochemical performances ofNi(OH)_2/CNTs composed electrode. The results showed that Ni(OH)_2/CNTscomposed electrode presents the best performance with using 20-40 nm of 25 wt%CNTs. The specific capacity is 280 mAh/g. And the electrode using ultrasoniccondition has a better cycling stability, a higher charging efficiency, greater specificdischarge capacity, higher discharge voltage, better high-rote capability and superiorcycling stability.
1．应用硅胶表面印迹技术，以Fe(Ⅲ)，Ni(Ⅱ)和Al(Ⅲ)为印迹离子、3-氨基丙基-三乙氧基硅烷为功能单体，制备了Fe(Ⅲ)，Ni(Ⅱ)和Al(Ⅲ)的氨基功能化表面印迹聚合物。研究了印迹聚合物和非印迹聚合物对Fe(Ⅲ)，Ni(Ⅱ)和Al(Ⅲ)的分离富集特性。结果如下：(1)相比传统吸附剂和非印迹材料，Fe(Ⅲ)印迹聚合物对Fe(Ⅲ)具有较好的选择性和吸附容量。Fe(Ⅲ)印迹聚合物和非印迹聚合物的最大静态吸附容量分别是25．21和5．10mg g~(-1)；在Fe(Ⅲ)和Cr(Ⅲ)的相同浓度的混合溶液中，Fe(Ⅲ)印迹硅胶对Fe(Ⅲ)的最大选择性系数为451，Fe(Ⅲ)／Cr(Ⅲ)的相对选择性因子为49．9。Fe(Ⅲ)印迹硅胶固相萃取痕量铁的检出限为0．34μg L~(-1)，方法的相对标准偏差为1．5％，将该法用于水样和植物样品中痕量Fe(Ⅲ)的测定，得到满意的结果。(2)相比传统吸附剂和非印迹硅胶，Ni(Ⅱ)印迹吸附剂对Ni(Ⅱ)具有很高的吸附选择性和吸附容量。Ni(Ⅱ)印迹聚合物和非印迹聚合物的最大静态吸附容量分别是12．61和4．25mg g~(-1)；在Ni(Ⅱ)和干扰离子具有相同浓度的混合溶液中，Ni(Ⅱ)／Cu(Ⅱ)，Ni(Ⅱ)／Co(Ⅱ)，Ni(Ⅱ)／Zn(Ⅱ)和Ni(Ⅱ)／Pd(Ⅱ)的相对选择性因子分别为45．99，32．83，43．79和28．36。Ni(Ⅱ)印迹硅胶固相萃取痕量Ni(Ⅱ)的检出限为0．16μg L~(-1)，该方法的相对标准偏差为1．48％，将该法用于水样和植物样品中痕量Ni(Ⅱ)的测定，得到满意的结果。(3)相比传统吸附剂和非印迹硅胶，Al(Ⅲ)印迹吸附剂对Al(Ⅲ)具有很高的吸附选择性和吸附容量。Al(Ⅲ)印迹聚合物和非印迹聚合物的最大静态吸附容量分别是11．46mg g~(-1)和6．28mg g~(-1)；在Al(Ⅲ)和干扰离子Cr(Ⅲ)具有相同浓度的混合溶液中，Al(Ⅲ)／Cr(Ⅲ)的相对选择性因子分别为6．73。Al(Ⅲ)印迹硅胶固相萃取痕量Al(Ⅲ)的检出限为0．36μg L~(-1)，该方法的相对标准偏差为3．2％。
2．以丙烯酰胺为功能单体、季戊四醇三丙烯酸酯为交联剂、偶氮二异丁腈做引发剂，以姜黄素分子作模板分子制备了姜黄素分子的印迹聚合物，研究了印迹聚合物和非印迹聚合物对姜黄素分子的选择吸附性能。结果表明，经过印迹的聚合物对模板分子具有很好的特异性结合能力，为复杂样品中的姜黄素物质的选择性富集及快速检测提供了新的途径。
3．采用加表面活性剂于缓冲溶液中的化学沉淀法直接合成了具有纳米结构特征的氢氧化镍／碳纳米管(CNTs)粉末。分析了不同直径和含量的CNTs对Ni(OH)_2电化学性能的影响。首先，CNTs被分散在氢氧化钠溶液中，然后在合成纳米Ni(OH)_2的过程中引入CNTs，经过化学反应形成复合材料。本实验中，分别选用了10-20nm、20-40nm、60-100nm质量百分含量分别为2wt％、5wt％、10wt％、25wt％和50wt％的CNTs，结果发现合成过程中用20-40nm 25wt％的CNTs的复合材料电化学性能最好。其放电比容量可以达到280mAh／g，而且比较稳定，循环寿命长。同时将超声波条件引入合成过程中，可以使电极在充放电效率、放电比容量、活性物质利用率、放电电压、抗膨胀能力及高速率放电性能等方面得到明显改善和提高。
The rapid development of science, technology and proceeding industrializationleads to the consumption and draining of heavy metals and organic substance. Thepollution caused by heavy metals and poisonous organic substance become more andmore serious. The accurate determination of trace element in geological, biologicaland environmental samples is very important in analytical chemistry. Although manyinstrument analysis methods have been developed recently and reached trace level orsuper trace level sensitivity, the direct analysis is still difficult because of the highcomplexity of samples and severe interference caused by matrix effects. So, variouspre-treatment procedures are necessary before the more accurate measurement byanalytical instruments. It is obvious that the pre-treatment procedures of traceelements depend on appropriate separation methods and different functionaladsorption materials with higher selectivity and adsorption capacity. This papermainly described the preparation of several adsorption materials based on thepre-concentration and separation of trace components. The behaviors of thesematerials that have high selectivity for targets have been studied systematically anddetailedly. At the same time, study on nano-scale nickel hydroxide-CNTs composedmaterial used as electrode material has been done by me. The more detailed noveltyof this work can be categorized as follows:
1. The imprinted and non-imprinted amino-functionalized silica gel adsorbents forFe(Ⅲ), Ni(Ⅱ) and Al(Ⅲ) were obtained by a surface imprinting technique forselective extraction of Fe(Ⅲ), Ni(Ⅱ) and Al(Ⅲ) prior to its determination byICP-AES. The results are: (1) Compared with the traditional solid sorbents andnon-imprinted sorbent, the Fe(Ⅲ)-imprinted amino-functionalized silica gel adsorbentexhibited excellent selectivity and adsorption capacity for Fe(Ⅲ). The maximumstatic adsorption capacity of the Fe(Ⅲ)-imprinted and non-imprinted sorbent forFe(Ⅲ) was 25.21 and 5.10 mg g~(-1), respectively. The largest selectivity coefficient of the Fe(Ⅲ)-imprinted sorbent for Fe(Ⅲ) in the presence of Cr(Ⅲ) that is the sameconcentration with Fe(Ⅲ) was 451. The relatively selective factor (ar) value ofFe(Ⅲ)/Cr(Ⅲ) was 49.9, which were greater than 1. The detection limit (3σ) of themethod was 0.34μg L~(-1). The relative standard deviation (R.S.D.) was 1.5 %. Theproposed method has been successfully applied to the determination and speciation ofiron in biological and water samples with satisfactory results. (2) Compared with thetraditional solid sorbents and non-imprinted sorbent, Ni(Ⅱ)-imprinted sorbent presentshigher selectivity and adsorption capacity for Ni(Ⅱ). The maximum static adsorptioncapacity of the ion-imprinted and non-imprinted sorbent for Ni(Ⅱ) was 12.61 and 4.25mg g~(-1), respectively. The relatively selective factor (α_r) values of Ni(Ⅱ)/Cu(Ⅱ),Ni(Ⅱ)/Co(Ⅱ), Ni(Ⅱ)/Zn(Ⅱ) and Ni(Ⅱ)/Pd(Ⅱ) were 45.99, 32.83, 43.79 and 28.36,which were greater than 1. The detection limit (3σ) of the method was 0.16 ng mL~(-1).The relative standard deviation of the method was 1.48 %. The method wassuccessfully applied to the determination of trace nickel in plants and water sampleswith satisfactory results. (3) Compared with the traditional solid sorbents andnon-imprinted sorbent, Al(Ⅲ)-imprinted sorbent presents higher selectivity andadsorption capacity for Al(Ⅲ). The maximum static adsorption capacity of theion-imprinted and non-imprinted sorbent for Al(Ⅲ) was 11.46 and 6.28 mg g~(-1),respectively. The relatively selective factor (α_r) value of Al(Ⅲ)/Cr(Ⅲ) was 6.73. Therelative standard deviation of the method was 3.2 %. The detection limit (3σ) of themethod was 0.36 ng mL~(-1).
2. A molecularly imprinted polymer was prepared by molecular imprintingtechnique using aerylamide (AA) as monomer, curcumin as template molecule, alarge excess of pentaerythritol triacylate (PETRA) as the cross-linking agent and 2,2-Azobisisobutyronitrile (AIBN) as the initiator. The bulk polymer obtained wasinvestigated in equilibrium binding experiments to evaluate the molecular recognitionand binding characteristics of the curcumin molecularly imprinted polymer. Thesubstrate selectivity of imprinted polymers and non-imprinted polymers wereinvestigated. The results showed that the imprinted polymers exhibited much higher affinity for curcumin among the tested compounds. It is possible to be a goodadsorption and binding material in the selective enrichment and determination of tracecurcumin in complex biosamples.
3. Nanometer Ni(OH)_2 were prepared by chemistry-deposition method with addingthe buffer solution and surfactant. Firstly, carbon nanotubes (CNTs) were dispersed inNaOH solution, then CNTs were chemically synthesized with nanometer Ni(OH)_2. Inthis experiment, 10-20 nm, 20-40 nm, 60-100 nm of 2 wt%, 5 wt%, 10 wt%, 25 wt%and 50 wt% CNTs were used to study the electrochemical performances ofNi(OH)_2/CNTs composed electrode. The results showed that Ni(OH)_2/CNTscomposed electrode presents the best performance with using 20-40 nm of 25 wt%CNTs. The specific capacity is 280 mAh/g. And the electrode using ultrasoniccondition has a better cycling stability, a higher charging efficiency, greater specificdischarge capacity, higher discharge voltage, better high-rote capability and superiorcycling stability.
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