新颖螯合树脂的合成及在重金属检测中的应用
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摘要
重金属污染已成为影响人类以及其它生物生存的重大问题。因此对微量及痕量重金属元素的分析检测对于保护人民身体健康,增强人民体质有非常重要的意义。而要实现微量及痕量重金属检测的常规分析化就要预先对其进行分离富集。因此,寻求一种物美价廉,既不产生污染又能有效分离富集重金属离子的吸附剂,在分析检测、资源回收等方面有着重要的研究价值和广泛的应用前景。
本文从十种配体中筛选合成了五种具有较强吸附功能的螯合树脂,利用元素分析、FTIR进行了结构表征;分别研究了其对几种重金属离子的螯合吸附性能和机理;采用模拟及应用试验为筛选出性能优良的螯合树脂在水体中重金属分离、富集和检测等方面的应用探索出一条新路。
1、采用以氯甲基化聚苯乙烯为母体,与含氮、硫的杂环和直链化合物发生亲核反应来制备新的螯合树脂。从反应溶剂、反应温度、反应摩尔比和反应时间等方面确定了树脂的最佳合成条件。利用元素分析及FTIR对合成的树脂进行了结构表征。
2、详细研究了五种树脂对Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)重金属离子的静态吸附性能和动态吸附性能,并对其吸附机理进行了探讨。结果表明:(1)在T=298K,HAc-NaAc体系中,五种树脂对Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)三种重金属离子有较强的吸附性能。在各自最佳pH值下,其静态饱和吸附量如下:3-AT-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为382.5、157.6、24.80 mg/g;TETA-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为332.6、189.1、137.4 mg/g;ADMP-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(在)分别为101.8、180.9、51.06 mg/g;TSC-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为619.5、227.3、152.3 mg/g;ATZL-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为263.7、154.6、28.61 mg/g。用浓度为0.5～3.0 mol/L的HCl或含0.1%硫脲的0.5mol/L HCl做解吸剂,一次解吸率可达100%。(2)在实验研究的浓度范围内,树脂对重金属离子的吸附可用Langmuir等温方程来描述;吸附动力学显示,五种树脂对三种重金属离子的交换动力学符合Boyd G.E.方程,即交换由液膜扩散控制。在一定浓度范围内,树脂吸附重金属离子对Na~+、K~+有较强的抗干扰能力。(3)动态吸附结果显示:TSC-R、TETA-R、3-AT-R树脂吸附Hg(Ⅱ)的动态吸附容量分别为587.1 mg/g、360.3 mg/g、374.8 mg/g;TSC-R、TETA-R、ADMP-R树脂吸附Cd(Ⅱ)的动态吸附容量分别为237.2 mg/g、215.3 mg/g、207.9 mg/g;TSC-R、TETA-R树脂吸附Pb(Ⅱ)的动态吸附容量分别为143.4 mg/g、139.0mg/g。用相应解吸剂的解吸效果都比较好,用含0.1%硫脲的0.5 mol/L HCl解吸TSC-R吸附Hg(Ⅱ)柱的解吸率为91.85%,其余均能完全解吸。且前25mL解吸液中吸附质的浓度较高,基本接近50%或其以上。因此可用作浓度较高溶液,或用于重金属的回收利用等。(4)初步探讨了树脂对重金属离子的吸附机理,研究认为树脂功能基上的氮或硫原子与重金属离子形成配位键引起的。
3、研究了单一重金属离子和混合重金属离子的模拟及实际水样的吸附和解吸试验。结果表明:(1)单一离子试验表明,在海水条件下,其相应吸附量略有下降,这可能是海水中的其它成分对其吸附有一定影响的缘故。(2)分别研究了3-AT-R树脂吸附Hg(Ⅱ),TETA-R树脂吸附Cd(Ⅱ),TSC-R树脂吸附Pb(Ⅱ)的动态吸附曲线,其动态吸附容量分别为325.5 mg/g、197.8mg/g、156.0 mg/g。用相应解吸剂均能完全解吸。(3)混合重金属离子的模拟试验表明,在实验体系中,树脂对Cd(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)三种重金属离子的吸附能力不同,个别相差较大,这主要是由于竞争性吸附引起的。三种重金属的回收率都比较高,均在90%以上,因此可用于微量重金属离子的富集及回收利用。动力学试验表明,树脂对三种重金属离子的吸附速率较快,总体来说,五种树脂对Cu(Ⅱ)的吸附力较强,对Pb(Ⅱ)较弱。因此,可用于含Cu(Ⅱ)水体或海水的纯化及含Cu(Ⅱ)、Pb(Ⅱ)废水中对Cu(Ⅱ)的分离富集。
The pollution of heavy metal ions(HMI)has already become serious problems that influence the survival of human being and other creatures.So the determination and analysis of trace heavy metal elements have very important significance to protecting people's health and strengthening people's constitution. And it is necessary to separate and concentrate before using the conventional instruments to analyze.It will have wide application prospect and research value in detection,analysis,resources recovery and reclamation to find a good and cheap adsorbent,which are both environmental friendly and can adsorb HMI effectively.
In this thesis,five kinds of novel chelating resins that function as adsorption and separation from ten ligand were prepared.The structures were characterized by element analysis and FTIR.The properties of the chelating adsorption and the mechanism for several metal ions were studied.The simulated application test was used to screen out resins with excellent property which are applied to the separation,detection and analysis of HMI in water.
1.New types of chelating resins were synthesized by cholromethylated polystyrene reacted with nitrogen-containing and sulfur-containing compounds of linear and heterocycle.The influence of synthesis conditions such as reaction solvents,temperatures,molar ratio and time on the reactions were studied.The structures and patterns are characterized by element analysis and FTIR.
2.The adsorption properties of five resins for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were systematically investigated by means of static and dynamic method,the adsorption mechanism was also discussed.The experimental results showed that: (1)The resins had powerful adsorption capacities for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)in HAc-NaAc medium at 298K.The statically saturated adsorption capacity of resins as follows:3-AT-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 382.5,157.6, 24.80 mg/g,TETA-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 332.6,189.1,137.4 mg/g,ADMP-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 101.8,180.9,51.06 mg/g, TSC-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 619.5,227.3,152.3 mg/g,ATZL-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 263.7,154.6,28.61 mg/g,respectively. 0.5～3.0 mol/L HCl and 0.1%thiourea in 0.5mol/L HCl were tested for the recovery of heavy metals loaded in the resins adsorption operation,with elution percentage of 100%.(2)The adsorption isotherms approximately fitted the Langmuir equation within the range of experimental concentrations.The adsorption dynamics of five resins for three HMI indicated that adsorption fitted the Boyd G.E.equation and was controlled by the liquid film diffusion.The resins for HMI had strong ability of anti-jamming to Na~+,K~+ within certain concentration.(3)From the study of dynamic adsorption,the dynamic saturated adsorption Capacity of resins as follows:TSC-R,TETA-R,3-AT-R resin for Hg(Ⅱ)were 587.1 mg/g,360.3 mg/g,374.8 mg/g,TSC-R,TETA-R,ADMP-R resin for Cd(Ⅱ)were 5237.2 mg/g,215.3 mg/g,207.9 mg/g,TSC-R,TETA-R resin for Pb(Ⅱ)were 143.4 mg/g,139.0 mg/g,respectively.Hg(Ⅱ)adsorbed on TSC-R resin could be eluted by 0.1%thiourea in 0.5mol/L HCl and the elution percentage was up to 91.85%,others could be completely eluted.The HMI concentration of first 25mL desorption solution was approximately or over 50%. So it can be used as high concentration solution or recovery of heavy metals.(4) The adsorption mechanism of resins for HMI was also discussed.The research on mechanism showed that N or S atom on functional group of resins combined with HMI formed coordinate bond.
3.The adsorption and desorption properties of resins for model and real water samples including single and mixed heavy metals were investigated.The experimental results showed that:(1)From the study of resins for single heavy metal,it could be found out that the adsorption capacities of resins for HMI were slightly reduced under the seawater condition,that may because other component of seawater could decrease the adsorption capacity of HMI.(2)The dynamic adsorption curves of 3-AT-R resin for Hg(Ⅱ),TETA-R resin for Cd(Ⅱ),TSC-R resin for Pb(Ⅱ)were investigated,and the dynamic saturated adsorption capacity were 325.5 mg/g,197.8 mg/g,156.0 mg/g respectively.The HMI adsorbed on the resins could be completely eluted with corresponding eluant.(3) From the study of resins for mixed heavy metals of Cd(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ),it was demonstrated that the adsorption capacity of resins for HMI was different within the range of experimental condition because of the competitive adsorption.The recovery of three heavy metals was over 90%.The adsorption dynamics of resins for three HMI indicated that the adsorption rate was considerably high.As a whole,the adsorbability of five resins for Cu(Ⅱ)was much stronger than Pb(Ⅱ). So they could be used for separation and concentration of Cu(Ⅱ)from waste water which containing Cu(Ⅱ)and Pb(Ⅱ),and purification of water or sea water containing Cu(Ⅱ).
本文从十种配体中筛选合成了五种具有较强吸附功能的螯合树脂,利用元素分析、FTIR进行了结构表征;分别研究了其对几种重金属离子的螯合吸附性能和机理;采用模拟及应用试验为筛选出性能优良的螯合树脂在水体中重金属分离、富集和检测等方面的应用探索出一条新路。
1、采用以氯甲基化聚苯乙烯为母体,与含氮、硫的杂环和直链化合物发生亲核反应来制备新的螯合树脂。从反应溶剂、反应温度、反应摩尔比和反应时间等方面确定了树脂的最佳合成条件。利用元素分析及FTIR对合成的树脂进行了结构表征。
2、详细研究了五种树脂对Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)重金属离子的静态吸附性能和动态吸附性能,并对其吸附机理进行了探讨。结果表明:(1)在T=298K,HAc-NaAc体系中,五种树脂对Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)三种重金属离子有较强的吸附性能。在各自最佳pH值下,其静态饱和吸附量如下:3-AT-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为382.5、157.6、24.80 mg/g;TETA-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为332.6、189.1、137.4 mg/g;ADMP-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(在)分别为101.8、180.9、51.06 mg/g;TSC-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为619.5、227.3、152.3 mg/g;ATZL-R树脂吸附Hg(Ⅱ)、Cd(Ⅱ)、Pb(Ⅱ)分别为263.7、154.6、28.61 mg/g。用浓度为0.5～3.0 mol/L的HCl或含0.1%硫脲的0.5mol/L HCl做解吸剂,一次解吸率可达100%。(2)在实验研究的浓度范围内,树脂对重金属离子的吸附可用Langmuir等温方程来描述;吸附动力学显示,五种树脂对三种重金属离子的交换动力学符合Boyd G.E.方程,即交换由液膜扩散控制。在一定浓度范围内,树脂吸附重金属离子对Na~+、K~+有较强的抗干扰能力。(3)动态吸附结果显示:TSC-R、TETA-R、3-AT-R树脂吸附Hg(Ⅱ)的动态吸附容量分别为587.1 mg/g、360.3 mg/g、374.8 mg/g;TSC-R、TETA-R、ADMP-R树脂吸附Cd(Ⅱ)的动态吸附容量分别为237.2 mg/g、215.3 mg/g、207.9 mg/g;TSC-R、TETA-R树脂吸附Pb(Ⅱ)的动态吸附容量分别为143.4 mg/g、139.0mg/g。用相应解吸剂的解吸效果都比较好,用含0.1%硫脲的0.5 mol/L HCl解吸TSC-R吸附Hg(Ⅱ)柱的解吸率为91.85%,其余均能完全解吸。且前25mL解吸液中吸附质的浓度较高,基本接近50%或其以上。因此可用作浓度较高溶液,或用于重金属的回收利用等。(4)初步探讨了树脂对重金属离子的吸附机理,研究认为树脂功能基上的氮或硫原子与重金属离子形成配位键引起的。
3、研究了单一重金属离子和混合重金属离子的模拟及实际水样的吸附和解吸试验。结果表明:(1)单一离子试验表明,在海水条件下,其相应吸附量略有下降,这可能是海水中的其它成分对其吸附有一定影响的缘故。(2)分别研究了3-AT-R树脂吸附Hg(Ⅱ),TETA-R树脂吸附Cd(Ⅱ),TSC-R树脂吸附Pb(Ⅱ)的动态吸附曲线,其动态吸附容量分别为325.5 mg/g、197.8mg/g、156.0 mg/g。用相应解吸剂均能完全解吸。(3)混合重金属离子的模拟试验表明,在实验体系中,树脂对Cd(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)三种重金属离子的吸附能力不同,个别相差较大,这主要是由于竞争性吸附引起的。三种重金属的回收率都比较高,均在90%以上,因此可用于微量重金属离子的富集及回收利用。动力学试验表明,树脂对三种重金属离子的吸附速率较快,总体来说,五种树脂对Cu(Ⅱ)的吸附力较强,对Pb(Ⅱ)较弱。因此,可用于含Cu(Ⅱ)水体或海水的纯化及含Cu(Ⅱ)、Pb(Ⅱ)废水中对Cu(Ⅱ)的分离富集。
The pollution of heavy metal ions(HMI)has already become serious problems that influence the survival of human being and other creatures.So the determination and analysis of trace heavy metal elements have very important significance to protecting people's health and strengthening people's constitution. And it is necessary to separate and concentrate before using the conventional instruments to analyze.It will have wide application prospect and research value in detection,analysis,resources recovery and reclamation to find a good and cheap adsorbent,which are both environmental friendly and can adsorb HMI effectively.
In this thesis,five kinds of novel chelating resins that function as adsorption and separation from ten ligand were prepared.The structures were characterized by element analysis and FTIR.The properties of the chelating adsorption and the mechanism for several metal ions were studied.The simulated application test was used to screen out resins with excellent property which are applied to the separation,detection and analysis of HMI in water.
1.New types of chelating resins were synthesized by cholromethylated polystyrene reacted with nitrogen-containing and sulfur-containing compounds of linear and heterocycle.The influence of synthesis conditions such as reaction solvents,temperatures,molar ratio and time on the reactions were studied.The structures and patterns are characterized by element analysis and FTIR.
2.The adsorption properties of five resins for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were systematically investigated by means of static and dynamic method,the adsorption mechanism was also discussed.The experimental results showed that: (1)The resins had powerful adsorption capacities for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)in HAc-NaAc medium at 298K.The statically saturated adsorption capacity of resins as follows:3-AT-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 382.5,157.6, 24.80 mg/g,TETA-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 332.6,189.1,137.4 mg/g,ADMP-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 101.8,180.9,51.06 mg/g, TSC-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 619.5,227.3,152.3 mg/g,ATZL-R resin for Hg(Ⅱ),Cd(Ⅱ),Pb(Ⅱ)were 263.7,154.6,28.61 mg/g,respectively. 0.5～3.0 mol/L HCl and 0.1%thiourea in 0.5mol/L HCl were tested for the recovery of heavy metals loaded in the resins adsorption operation,with elution percentage of 100%.(2)The adsorption isotherms approximately fitted the Langmuir equation within the range of experimental concentrations.The adsorption dynamics of five resins for three HMI indicated that adsorption fitted the Boyd G.E.equation and was controlled by the liquid film diffusion.The resins for HMI had strong ability of anti-jamming to Na~+,K~+ within certain concentration.(3)From the study of dynamic adsorption,the dynamic saturated adsorption Capacity of resins as follows:TSC-R,TETA-R,3-AT-R resin for Hg(Ⅱ)were 587.1 mg/g,360.3 mg/g,374.8 mg/g,TSC-R,TETA-R,ADMP-R resin for Cd(Ⅱ)were 5237.2 mg/g,215.3 mg/g,207.9 mg/g,TSC-R,TETA-R resin for Pb(Ⅱ)were 143.4 mg/g,139.0 mg/g,respectively.Hg(Ⅱ)adsorbed on TSC-R resin could be eluted by 0.1%thiourea in 0.5mol/L HCl and the elution percentage was up to 91.85%,others could be completely eluted.The HMI concentration of first 25mL desorption solution was approximately or over 50%. So it can be used as high concentration solution or recovery of heavy metals.(4) The adsorption mechanism of resins for HMI was also discussed.The research on mechanism showed that N or S atom on functional group of resins combined with HMI formed coordinate bond.
3.The adsorption and desorption properties of resins for model and real water samples including single and mixed heavy metals were investigated.The experimental results showed that:(1)From the study of resins for single heavy metal,it could be found out that the adsorption capacities of resins for HMI were slightly reduced under the seawater condition,that may because other component of seawater could decrease the adsorption capacity of HMI.(2)The dynamic adsorption curves of 3-AT-R resin for Hg(Ⅱ),TETA-R resin for Cd(Ⅱ),TSC-R resin for Pb(Ⅱ)were investigated,and the dynamic saturated adsorption capacity were 325.5 mg/g,197.8 mg/g,156.0 mg/g respectively.The HMI adsorbed on the resins could be completely eluted with corresponding eluant.(3) From the study of resins for mixed heavy metals of Cd(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ),it was demonstrated that the adsorption capacity of resins for HMI was different within the range of experimental condition because of the competitive adsorption.The recovery of three heavy metals was over 90%.The adsorption dynamics of resins for three HMI indicated that the adsorption rate was considerably high.As a whole,the adsorbability of five resins for Cu(Ⅱ)was much stronger than Pb(Ⅱ). So they could be used for separation and concentration of Cu(Ⅱ)from waste water which containing Cu(Ⅱ)and Pb(Ⅱ),and purification of water or sea water containing Cu(Ⅱ).
引文
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