分散支撑液膜中重金属离子的传输与分离研究
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摘要
重金属污染来源广泛且日趋严重,对生态环境安全和饮用水安全构成了巨大威胁。支撑液膜分离技术由于具有传质速度快、选择性好、分离效率高、成本低、无二次污染等优点,近年来备受关注,特别适合于重金属离子的分离与浓缩。但由于膜不稳定、膜寿命短而限制了其大规模工业应用。
本论文在现有支撑液膜分离技术的理论研究基础上,探索合适的液膜分离体系,提出分散支撑液膜的概念,研究了几种常见二价重金属离子以及贵金属离子在分散支撑液膜体系中的传输行为,解决了支撑液膜体系的稳定性问题,建立了混合金属离子分离回收的新方法,并通过传质机制分析,建立相应的动力学模型,取得了以下研究结果：
1.以常见二价重金属离子Co(II)、Zn(II)、Cd(II)、Cu(II)和Pb(II)为研究对象,有机膦酸酯PC-88A为流动载体,煤油为膜溶剂,研究了重金属离子在分散支撑液膜体系中的传输行为,探讨了影响金属离子传输的各种因素。其最佳传输条件为：料液相pH分别为6.00、4.00、5.00、5.25、5.25；解析相中液膜相和解析液体积比均为160：40；解析液HCl浓度分别为4.00mol·L-1、4.00mol·L-1、4.00mol·L-1、4.00mol·L-1和5.00mol·L-1。在最佳条件下,传输率分别为94.4%(190min)、90.0%(190min)、82.7%(190min)、90.0%(130min)和88.9%(190min)。通过比较,发现分散支撑液膜不仅具有较高的传输效率,而且膜体系稳定,膜的使用寿命长。
2.以贵金属离子Ag(I)、Au(III)、Pt(IV)和Pd(II)为研究对象,选择合适的流动载体,研究了金属离子在分散支撑液膜中的迁移行为和规律,探讨了影响金属离子传输的各种因素。最佳传输条件为：流动载体分别为TOA、TOA、PC-88A和N503；料液相介质分别为0.10mol·L-1 HNO3和0.10mol·L-1KSCN、2.00 mol·L-1HCl、0.50 mol·L-1 HCl和0.l0mol·L-1HCl;解析相中液膜相和解析液体积比分别为40：20、40：20、140：60和30：30；解析液分别为0.125 mol·L-1Na2S2O3、0.33mol·L-1KCN.7.00 mol·L-1HCl(?)1.60mol·L-1KSCN；在最佳条件下,传输130min,传输率分别为80.0%、100.0%、100.0%和79.8%。通过比较,发现分散支撑液膜具有较高的传输效率。
3.通过传质过程分析,建立了重金属离子在分散支撑液膜体系中的传质动力学方程,计算出重金属离子通过分散支撑液膜传输时的传输动力学参数d0和δa,并通过实验得以验证。
4.利用建立的分散支撑液膜体系,分别对Zn(II)和Cu(II).Zn(II)和Co(II).Cu(II)和Co(II).Pt(Ⅳ)和Co(II).Pt(Ⅳ)和Cu(II).Au(III)和Ag(I)以及Zn(II).Cu(II)和Co(II)进行分离。结果表明,该体系能够实现混合离子的有效分离。
Wide variety of sources and increasingly serious heavy metal pollution is a major threat to the ecological environment security and safety of drinking water. Supported liquid membrane separation processes have been recently receiving considerable attention due to characteristics such as the fast mass transfer, high selectivity and separation efficiency, lower operation costs and no secondary pollution. And they are particularly suitable for the separation and enrichment of heavy metal ions. However, supported liquid membrane separation processes can be limited in a large-scale industrial applications due to membrane instability and shortly membrane life.
In this paper, dispersion supported liquid membrane (DSLM)separation processes, a new liquid membrane separation system,can be advanced based on the theoretical study of the existing supported liquid membrane(SLM) separation technology. The transport behavior of conventional divalent heavy metal ions and the noble metal ions have been studied in this thesis. The stability problem of SLM have been solved. A new separation method of mixed metal ion separation and recovery is obtained. The mathematical model of heavy metal ions transport through DSLM is established by the analysis of mass transfer. The results are sumrnarized as follows:
1. The transport behavior of conventional divalent heavy metal ions including Co(Ⅱ), Zn(Ⅱ), Cd (Ⅱ), Cu (Ⅱ) and Pb(Ⅱ) through DSLM with 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (commercially known as PC-88A) as mobile carrier and kerosene as a membrane solvent was studied. Various factors affecting heavy metal ions transfer were discussed. The optimum conditions of transport are summarized as follows:feed solution pH 6.00,4.00,5.00,5.25 and 5.25 respectively; the volume ratio of liquid membrane to stripping solution 160:40; HCl concentrations in stripping solution 4.00 mol-L-1,4.00mol·L-1, 400mol·L-1,4.00mol·L-1 and 5.OOmol-L"1 respectively. Under the optimum transport conditions, the transport rate can reach 94.4%(in 190min),90.0%(in 190min),82.7% (in 190min),90.0%(in 130min) and 88.9%(in 190min) respectively. We can see that DSLM has a high transmission efficiency in comparison with conventional SLM. At the same time the system can improve the stability of the membrane and extend the life of the membrane.
2. The transport behavior and rules of noble metal ions including Ag(I), Au(III), Pt(IV) and Pd(II) through DSLM with appropriate mobile carrier were studied. Various factors affecting noble metal ions transfer were discussed. The optimal conditions of transport are summarized as follows:mobile carrier tri-n-octylamine, tri-n-octylamine, PC-88A, N503 respectively; medium in feed solution 0.20mol·L-1 HNO3and 0.10 mol·L-1 KSCN,2.00mol·L-1 HCl, 0.50mol·L-1 HCl,0.10 mol·L"1 HCl respectively; the volume ratio of liquid membrane to stripping solution 40:20,40:20,140:60 and 30:30 respectively; stripping solution 0.125mol·L-1Na2S2O3, 0.33mol·L-1KCN, 7.00mol·L-1HCl and 1.60mol-L-1KSCN respectively. Under the optimum transport conditions, the transport rate can reach 80.0%,100.0%,100.0% and 79.8% respectively during the transport time of 130min. We can see that DSLM has a high transmission efficiency in comparison with conventional SLM.
3. The transport kinetics equation of heavy metal ions through DSLM is derived based on the transfer process analysis. The transport kinetics parameters do andδa are calculated through the DSLM.The calculated results are in good agreement with experimental results.
4. Through the DSLM the selective separation of mixed heavy metal ions,such as Zn(II) and Cu(II), Zn(II) and Co(II), Cu(II) and Co(II), Pt(IV) and Co(II), Pt(IV) and Cu(II), Au(III) and Ag(I), Zn(II) and Cu(II) and Co(II), are explored. The results showed the mixed ions can be separated effectively through the DSLM.
本论文在现有支撑液膜分离技术的理论研究基础上,探索合适的液膜分离体系,提出分散支撑液膜的概念,研究了几种常见二价重金属离子以及贵金属离子在分散支撑液膜体系中的传输行为,解决了支撑液膜体系的稳定性问题,建立了混合金属离子分离回收的新方法,并通过传质机制分析,建立相应的动力学模型,取得了以下研究结果：
1.以常见二价重金属离子Co(II)、Zn(II)、Cd(II)、Cu(II)和Pb(II)为研究对象,有机膦酸酯PC-88A为流动载体,煤油为膜溶剂,研究了重金属离子在分散支撑液膜体系中的传输行为,探讨了影响金属离子传输的各种因素。其最佳传输条件为：料液相pH分别为6.00、4.00、5.00、5.25、5.25；解析相中液膜相和解析液体积比均为160：40；解析液HCl浓度分别为4.00mol·L-1、4.00mol·L-1、4.00mol·L-1、4.00mol·L-1和5.00mol·L-1。在最佳条件下,传输率分别为94.4%(190min)、90.0%(190min)、82.7%(190min)、90.0%(130min)和88.9%(190min)。通过比较,发现分散支撑液膜不仅具有较高的传输效率,而且膜体系稳定,膜的使用寿命长。
2.以贵金属离子Ag(I)、Au(III)、Pt(IV)和Pd(II)为研究对象,选择合适的流动载体,研究了金属离子在分散支撑液膜中的迁移行为和规律,探讨了影响金属离子传输的各种因素。最佳传输条件为：流动载体分别为TOA、TOA、PC-88A和N503；料液相介质分别为0.10mol·L-1 HNO3和0.10mol·L-1KSCN、2.00 mol·L-1HCl、0.50 mol·L-1 HCl和0.l0mol·L-1HCl;解析相中液膜相和解析液体积比分别为40：20、40：20、140：60和30：30；解析液分别为0.125 mol·L-1Na2S2O3、0.33mol·L-1KCN.7.00 mol·L-1HCl(?)1.60mol·L-1KSCN；在最佳条件下,传输130min,传输率分别为80.0%、100.0%、100.0%和79.8%。通过比较,发现分散支撑液膜具有较高的传输效率。
3.通过传质过程分析,建立了重金属离子在分散支撑液膜体系中的传质动力学方程,计算出重金属离子通过分散支撑液膜传输时的传输动力学参数d0和δa,并通过实验得以验证。
4.利用建立的分散支撑液膜体系,分别对Zn(II)和Cu(II).Zn(II)和Co(II).Cu(II)和Co(II).Pt(Ⅳ)和Co(II).Pt(Ⅳ)和Cu(II).Au(III)和Ag(I)以及Zn(II).Cu(II)和Co(II)进行分离。结果表明,该体系能够实现混合离子的有效分离。
Wide variety of sources and increasingly serious heavy metal pollution is a major threat to the ecological environment security and safety of drinking water. Supported liquid membrane separation processes have been recently receiving considerable attention due to characteristics such as the fast mass transfer, high selectivity and separation efficiency, lower operation costs and no secondary pollution. And they are particularly suitable for the separation and enrichment of heavy metal ions. However, supported liquid membrane separation processes can be limited in a large-scale industrial applications due to membrane instability and shortly membrane life.
In this paper, dispersion supported liquid membrane (DSLM)separation processes, a new liquid membrane separation system,can be advanced based on the theoretical study of the existing supported liquid membrane(SLM) separation technology. The transport behavior of conventional divalent heavy metal ions and the noble metal ions have been studied in this thesis. The stability problem of SLM have been solved. A new separation method of mixed metal ion separation and recovery is obtained. The mathematical model of heavy metal ions transport through DSLM is established by the analysis of mass transfer. The results are sumrnarized as follows:
1. The transport behavior of conventional divalent heavy metal ions including Co(Ⅱ), Zn(Ⅱ), Cd (Ⅱ), Cu (Ⅱ) and Pb(Ⅱ) through DSLM with 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (commercially known as PC-88A) as mobile carrier and kerosene as a membrane solvent was studied. Various factors affecting heavy metal ions transfer were discussed. The optimum conditions of transport are summarized as follows:feed solution pH 6.00,4.00,5.00,5.25 and 5.25 respectively; the volume ratio of liquid membrane to stripping solution 160:40; HCl concentrations in stripping solution 4.00 mol-L-1,4.00mol·L-1, 400mol·L-1,4.00mol·L-1 and 5.OOmol-L"1 respectively. Under the optimum transport conditions, the transport rate can reach 94.4%(in 190min),90.0%(in 190min),82.7% (in 190min),90.0%(in 130min) and 88.9%(in 190min) respectively. We can see that DSLM has a high transmission efficiency in comparison with conventional SLM. At the same time the system can improve the stability of the membrane and extend the life of the membrane.
2. The transport behavior and rules of noble metal ions including Ag(I), Au(III), Pt(IV) and Pd(II) through DSLM with appropriate mobile carrier were studied. Various factors affecting noble metal ions transfer were discussed. The optimal conditions of transport are summarized as follows:mobile carrier tri-n-octylamine, tri-n-octylamine, PC-88A, N503 respectively; medium in feed solution 0.20mol·L-1 HNO3and 0.10 mol·L-1 KSCN,2.00mol·L-1 HCl, 0.50mol·L-1 HCl,0.10 mol·L"1 HCl respectively; the volume ratio of liquid membrane to stripping solution 40:20,40:20,140:60 and 30:30 respectively; stripping solution 0.125mol·L-1Na2S2O3, 0.33mol·L-1KCN, 7.00mol·L-1HCl and 1.60mol-L-1KSCN respectively. Under the optimum transport conditions, the transport rate can reach 80.0%,100.0%,100.0% and 79.8% respectively during the transport time of 130min. We can see that DSLM has a high transmission efficiency in comparison with conventional SLM.
3. The transport kinetics equation of heavy metal ions through DSLM is derived based on the transfer process analysis. The transport kinetics parameters do andδa are calculated through the DSLM.The calculated results are in good agreement with experimental results.
4. Through the DSLM the selective separation of mixed heavy metal ions,such as Zn(II) and Cu(II), Zn(II) and Co(II), Cu(II) and Co(II), Pt(IV) and Co(II), Pt(IV) and Cu(II), Au(III) and Ag(I), Zn(II) and Cu(II) and Co(II), are explored. The results showed the mixed ions can be separated effectively through the DSLM.
引文
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