Fe_3O_4@离子印迹聚(St-HPMA-DVB)复合材料的合成及其对水中高氯酸盐选择性吸附
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摘要
采用超声协助悬浮聚合法以高氯酸根(ClO-4)为模板制备了Fe_3O_4@离子印迹聚(苯乙烯-3-(2-氨基三乙基四胺)-2-甲基丙烯酸羟丙酯-二乙烯苯)(Fe_3O_4@IIP(St-HPMA-DVB))磁性复合材料,通过TEM、振动样品磁强计(VSM)、TGA、XRD、元素分析(EA)、FTIR等对其进行表征,考察了交联剂DVB用量对材料结构与性能的影响。结果表明:合成的Fe_3O_4@IIP(St-HPMA-DVB)磁性复合材料平均粒径为500～2 000nm,随DVB用量的增加而增大;磁化强度为9.77～12.78emu/g,随DVB用量的增加而减小;DVB的加入有利于Fe_3O_4@IIP(StHPMA-DVB)磁性复合材料的离子印迹空腔的形成和稳定。考察了不同溶液pH值、ClO-4的初始浓度、吸附时间等条件下Fe_3O_4@IIP(St-HPMA-DVB)吸附水中ClO-4的性能,发现溶液pH值能显著影响Fe_3O_4@IIP(St-HPMA-DVB)磁性复合材料对ClO-4的吸附效果,pH为3.0时效果最佳;不同DVB用量Fe_3O_4@IIP(St-HPMADVB)磁性复合材料对ClO-4的吸附量和选择性有影响,当DVB用量为0.5g时,Fe_3O_4@IIP(St-HPMA-DVB)磁性复合材料的吸附量和选择性最佳;吸附机制以离子交换和静电引力为主。等温吸附线符合Langmuir模型,Fe_3O_4@IIP(St-HPMA-DVB)磁性复合材料的饱和吸附量(qm,c=76.9～111.1mg/g)高于非离子印迹材料Fe_3O_4@非离子印迹聚(NIP)(St-HPMA-DVB)磁性复合材料(qm,c=62.5mg/g)。吸附过程可在10min内达到平衡,符合准二级动力学模型;Fe_3O_4@IIP(St-HPMA-DVB)磁性复合材料能高选择性地有效吸附水中ClO-4,对ClO-4的印迹因子α为1.8,对几种常见共存离子的选择性因子β>5.8,是潜在的高选择性吸附和回收ClO-4的功能材料。
A Fe_3O_4@ion imprinted poly(Styrene-3-(2-amino triethylenetetramine)-2-hydroxypropyl methacrylatedivinylbenzene)(Fe_3O_4@IIP(St-HPMA-DVB))magnetic composite was synthesized via ultrasonic assisted suspension polymerization with perchlorate(ClO-4)as the ion imprinting template.The Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite was characterized by TEM,vibrating sample magnetometer(VSM),TGA,XRD,elemental analysis(EA).The effect of the usage amount of crosslinking agent DVB while preparation on the structure and performance of Fe_3O_4 @IIP(St-HPMA-DVB)magnetic composite was investigated.The results show that the Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite has an average size of 500-2 000 nm,which increases with the increase of the amount of DVB.The saturation magnetization intensity is 9.77-12.78 emu/g,which decreases withthe increase of the amount of DVB.The addition of DVB is beneficial to the formation and stability of the ion imprinted cavity of Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite.The effects of solution pH value,initial concentration of ClO-4,and adsorption time on the adsorption properties of ClO-4 in aqueous solutions were investigated.The results show that the adsorption capability is affected significantly by solution pH value and reaches the maximum at pH=3.0.The best adsorption capacity and selectivity of Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite to ClO-4 can be obtained when the usage amount of DVB is 0.5 g for synthesis.The adsorption mechanisms may be including both ion exchange and electrostatic interaction.The isothermal adsorption curves mainly obey the Langmuir mode with the maximum adsorption capacity(qm,c=76.9-111.1 mg/g)much higher than that of none-ion imprinted polymer magnetic material Fe_3O_4@non-ion imprinted poly(NIP)(St-HPMA-DVB)magnetic composite(qm,c=62.5 mg/g).The adsorption kinetic studies show that the adsorption processes reach the equilibrium within10 min and the kinetic data are well fitted to the pseudo-second-order model.There is almost no interference by the coexisting components in water for the adsorption of ClO-4,with imprinting factorαat 1.8,and selectivity factorβlager than 5.8 for several kinds of common co-existing anions,respectively.The Fe_3O_4 @IIP(St-HPMA-DVB)magnetic composite is an ideal candidate for adsorption and recycle ClO-4 from aqueous solution.
A Fe_3O_4@ion imprinted poly(Styrene-3-(2-amino triethylenetetramine)-2-hydroxypropyl methacrylatedivinylbenzene)(Fe_3O_4@IIP(St-HPMA-DVB))magnetic composite was synthesized via ultrasonic assisted suspension polymerization with perchlorate(ClO-4)as the ion imprinting template.The Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite was characterized by TEM,vibrating sample magnetometer(VSM),TGA,XRD,elemental analysis(EA).The effect of the usage amount of crosslinking agent DVB while preparation on the structure and performance of Fe_3O_4 @IIP(St-HPMA-DVB)magnetic composite was investigated.The results show that the Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite has an average size of 500-2 000 nm,which increases with the increase of the amount of DVB.The saturation magnetization intensity is 9.77-12.78 emu/g,which decreases withthe increase of the amount of DVB.The addition of DVB is beneficial to the formation and stability of the ion imprinted cavity of Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite.The effects of solution pH value,initial concentration of ClO-4,and adsorption time on the adsorption properties of ClO-4 in aqueous solutions were investigated.The results show that the adsorption capability is affected significantly by solution pH value and reaches the maximum at pH=3.0.The best adsorption capacity and selectivity of Fe_3O_4@IIP(St-HPMA-DVB)magnetic composite to ClO-4 can be obtained when the usage amount of DVB is 0.5 g for synthesis.The adsorption mechanisms may be including both ion exchange and electrostatic interaction.The isothermal adsorption curves mainly obey the Langmuir mode with the maximum adsorption capacity(qm,c=76.9-111.1 mg/g)much higher than that of none-ion imprinted polymer magnetic material Fe_3O_4@non-ion imprinted poly(NIP)(St-HPMA-DVB)magnetic composite(qm,c=62.5 mg/g).The adsorption kinetic studies show that the adsorption processes reach the equilibrium within10 min and the kinetic data are well fitted to the pseudo-second-order model.There is almost no interference by the coexisting components in water for the adsorption of ClO-4,with imprinting factorαat 1.8,and selectivity factorβlager than 5.8 for several kinds of common co-existing anions,respectively.The Fe_3O_4 @IIP(St-HPMA-DVB)magnetic composite is an ideal candidate for adsorption and recycle ClO-4 from aqueous solution.
引文
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[26]李小倩,方玲,张梦南,等.地下水中ClO-4浓度测定的分光光度法优化[J].环境科学与技术,2014,37(12):96-99.LI X Q,FANG L,ZHANG M N,et al.Measurement of perchlorate concentration in groundwater using methylene blue complexation-spectrophotometry[J].Environmental Science&Technology,2014,37(12):96-99(in Chinese).
[27] SHEN H Y,CHEN J L,DAI H F,et al.New insights into the sorption and detoxification of chromium(VI)by tetraethylenepentamine functionalized nano-sized magnetic polymer adsorbents:Mechanism and pH effect[J].Industrial&Engineering Chemistry Research,2013,52(36):12723-12732.
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[29] ZHANG W,QIN L,HE X W,et al.Novel surface modified molecularly imprinted polymer using acryloyl-β-cyclodextrin and acrylamide as monomers for selective recognition of lysozyme in aqueous solution[J].Journal of Chromatography A,2009,1216(21):4560-4567.
[30]刘晨,吕小王,张少民,等.高氯酸红外红外光谱法鉴定爆炸物[J].化学推进剂与高分子材料,2017,15(1):82-84.LIU C,LV X W,ZHANG S M,et al.Identification of explosives by infrared spectroscopy[J].Chemical Propellants&Polymeric Materials,2017,15(1):82-84(in Chinese).
[31] LU W S,SHEN Y H,XIE A J,et al.Novel bifunctional one-dimensional Fe3O4/Se nano-composites via facile green synthesis[J].Journal of Physical Chemistry C,2010,114(11):4846-4851.
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[2]吴春笃,李顺,许小红,等.高氯酸盐的环境毒理学效应及其机制的研究进展[J].环境与健康杂志,2013,30(1):85-89.WU C D,LI S,XU X H,et al.Environmental toxicological effect and mechanism of perchlorate[J].Journal of Environment and Health,2013,30(1):85-89(in Chinese).
[3] PRASANNA K,CHRISTOPHER O,INDRARATNE S P,et al.Perchlorate as an emerging contaminant in soil,water and food[J].Chemosphere,2016,150:667.
[4] CARR J A,MURALI S,HU F,et al.Changes in gastric sodium-iodide symporter(NIS)activity are associated with differences in thyroid gland sensitivity to perchlorate during metamorphosis[J].General and Comparative Endocrinology,2015,219:16-23.
[5]刘燕燕,吴耀国,晁吉福,等.含高氯酸盐废水处理技术的研究进展[J].工业水处理,2010,30(7):1-4.LIU Y Y,WU Y G,CHAO J F,et al.Research progress in the perchlorate-containing wastewater treatment techniques[J].Industrial Water Treatment,2010,30(7):1-4(in Chinese).
[6] GAO M C,WANG S,REM Y,et al.Simultaneous removal of perchlorate and nitrate in a combined reactor of sulfur autotrophy and electrochemical hydrogen autotrophy[J].Chemical Engineering Journal,2016,284:1008-1016.
[7] LIN S Y,CHEN W F,CHENG M T,et al.Investigation of factors that affect cationic surfactant loading on activated carbon and perchlorate adsorption[J].Colloids and Surfaces A:Physicochemical and Engineering Aspects, 2013, 434:236-242.
[8] WU X M,WANG Y L,XU L L,et al.Removal of perchlorate contaminants by calcined Zn/Al layered double hydroxides:Equilibrium,kinetics,and column studies[J].Desalination,2010,256(1-3):136-140.
[9] XIE Y H,LI S Y,WANG F,et al.Removal of perchlorate from aqueous solution using protonated cross-linked chitosan[J].Chemical Engineering Journal,2010,156(1):56-63.
[10]杨一琼,白皓,秦静.磁性离子交换树脂对饮用水中高氯酸盐的去除效能[J].中国给水排水,2015,31(21):5-8.YANG Y Q,BAI H,QIN J,et al.Removal efficiency of perchlorate from drinking water by magnetic ion exchange resin[J].China Water&Wastewater,2015,31(21):5-8(in Chinese).
[11] XIONG Z,ZHAO D Y,PAN G.Rapid and complete destruction of perchlorate in water and ion-exchange brine using stabilized zero-valent iron nanoparticles[J].Water Research,2007,41(15):3497-3505.
[12] HURLEY K D,SHAPLEY J R.Efficient heterogeneous catalytic reduction of perchlorate in water[J].Environmental Science and Technology,2007,41(6):2044-2049.
[13] MAHMUDOV R,SHU Y,RYKOV S,et al.The reduction of perchlorate by hydrogenation catalysts[J].Applied Catalysis B:Environmental,2008,81(1-2):78-87.
[14]张媛媛,郭延凯,张超,等.非水溶性醌加速菌GWF生物还原高氯酸盐的研究[J].环境科学,2016,37(3):988-993.ZHANG Y Y,GUO Y K,ZHANG C,et al.Effect of nondissolved quinone on perchlorate reduction by strain GWF[J].Environmental Science,2016,37(3):988-993(in Chinese).
[15] WU D L,HE P,XU X H,et al.The effect of various reaction parameters on bioremediation of perchlorate-contaminated water[J].Journal of Hazardous Materials,2008,150(2):419-423.
[16] FU J Q,CHEN L X,LI J H,et al.Current status and challenges of ion imprinting[J].Journal of Materials Chemistry A,2015,3:13598-13627.
[17]傅骏青,王晓艳,李金花,等.重金属离子印迹技术[J].化学进展,2016,28(1):83-90.FU J Q,WANG X Y,LI J H,et al.Ion imprinting technology for heavy metal ions[J].Progress in Chemistry,2016,28(1):83-90(in Chinese).
[18] GIL R,AMORIM C G,CROMBIE L,et al.Study of a novel bisnaphthalimidopropyl polyamine as electroactive material for perchlorate-selective potentiometric sensors[J].Electroanalysis,2015,27(12):2809-2819.
[19] CARUSO F,SPASOVA M,MACEIRA V S,et al.Nan engineering of particle surfaces[J].Advanced Materials,2001,13(1):11-22.
[20] SHEN H Y,ZHU Y,WEN X E,et al.Preparation of Fe3O4-C18 nano-magnetic composite materials and their cleanup properties for organophosphorous pesticides[J].Analytical and Bioanalytical Chemistry, 2007, 387(6):2227-2237.
[21]陈君良,姚屠鹏,朱宏亮,等.巯基功能化纳米Fe3O4磁性高分子复合材料的合成及其对水中亚甲基蓝的吸附作用[J].复合材料学报,2014,31(2):323-330.CHEN J L,YAO T P,ZHU H L,et al.Preparation of thiol-functionalized nano-Fe3O4-polymer magnetic composite material and its adsorption properties on methylene blue in water[J].Acta Materiae Compositae Sinica,2014,31(2):323-330(in Chinese).
[22]李冉冉,黄昊,董星龙,等.碳包覆磁性镍纳米粒子对亚甲基蓝的吸附性能[J].材料研究学报,2015,29(9):663-669.LI R R,HUANG H,DONG X L,et al.Adsorption performance of methylene blue onto nanoparticles of carbon-encapsulated magnetic nickel[J].Chinese Journal of Materials Research,2015,29(9):663-669(in Chinese).
[23] SHEN H Y,CHEN Z X,LI Z H,et al.Controlled synthesis of 2,4,6-trichlorophenol-imprinted amino-functionalized nano-Fe3O4-polymer magnetic composite for highly selective adsorption[J].Colloids and Surfaces A:Physicochemical and Engineering Aspects,2015,481:439-450.
[24] PAN S D,SHEN H Y,XU Q H,et al.Surface mercapto engineered magnetic Fe3O4nano adsorbent for the removal of mercury from aqueous solutions[J].Journal of Colloid and Interface Science,2012,365(1):204-212.
[25]王燕,叶思,吕珊珊,等.磁性Fe3O4@离子印迹聚(MMAHPMA-DVB)复合材料的合成及其对水中Ni(II)选择性吸附[J].复合材料学报,2017,34(12):2846-2855.WANG Y,YE S,LV S S,et al.Preparation of ion imprinted Fe3O4@IIP(MMA-HPMA-DVB)magnetic composite and its selective adsorption to Ni(II)[J].Acta Materiae Compositae Sinica,2017,34(12):2846-2855(in Chinese).
[26]李小倩,方玲,张梦南,等.地下水中ClO-4浓度测定的分光光度法优化[J].环境科学与技术,2014,37(12):96-99.LI X Q,FANG L,ZHANG M N,et al.Measurement of perchlorate concentration in groundwater using methylene blue complexation-spectrophotometry[J].Environmental Science&Technology,2014,37(12):96-99(in Chinese).
[27] SHEN H Y,CHEN J L,DAI H F,et al.New insights into the sorption and detoxification of chromium(VI)by tetraethylenepentamine functionalized nano-sized magnetic polymer adsorbents:Mechanism and pH effect[J].Industrial&Engineering Chemistry Research,2013,52(36):12723-12732.
[28] FOO K Y,HAMEED B H.Insights into the modeling of adsorption isotherm systems[J].Chemical Engineering Journal,2010,156(1):2-10.
[29] ZHANG W,QIN L,HE X W,et al.Novel surface modified molecularly imprinted polymer using acryloyl-β-cyclodextrin and acrylamide as monomers for selective recognition of lysozyme in aqueous solution[J].Journal of Chromatography A,2009,1216(21):4560-4567.
[30]刘晨,吕小王,张少民,等.高氯酸红外红外光谱法鉴定爆炸物[J].化学推进剂与高分子材料,2017,15(1):82-84.LIU C,LV X W,ZHANG S M,et al.Identification of explosives by infrared spectroscopy[J].Chemical Propellants&Polymeric Materials,2017,15(1):82-84(in Chinese).
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