纳滤膜对硫酸型解吸液锂镁分离的实验研究与模拟

doi:10.11949/0438-1157.20240743

化工学报 ›› 2024, Vol. 75 ›› Issue (12): 4563-4575.DOI: 10.11949/0438-1157.20240743

纳滤膜对硫酸型解吸液锂镁分离的实验研究与模拟

吴雨茜¹^,²^,³^,⁴(), 唐元晖¹^,²^,⁴, 郭强¹, 林亚凯²(), 余立新², 王晓琳²()

^1.北京低碳清洁能源研究院，煤炭开采水资源保护与利用全国重点实验室，北京 102209
^2.清华大学化学工程系，膜材料与工程北京市重点实验室，北京 100084
^3.国家能源集团国华投资河北分公司，河北张家口 075000
^4.中国矿业大学（北京）化学与环境工程学院，北京 100083

收稿日期:2024-07-01 修回日期:2024-08-06 出版日期:2024-12-25 发布日期:2025-01-03
通讯作者: 林亚凯,王晓琳
作者简介:吴雨茜（1997—），女，硕士研究生，1863138750@163.com
基金资助:
煤炭开采水资源保护与利用国家重点实验室2020年开放基金课题项目(GJNY-20-113-09);北京市自然科学基金项目(2232018);国家自然科学基金面上项目(22378225);国家重点研发计划项目(2022YFC2105103)

Experimental study and simulation on nanofiltration separation of lithium and magnesium from sulfate desorption solution

Yuxi WU¹^,²^,³^,⁴(), Yuanhui TANG¹^,²^,⁴, Qiang GUO¹, Yakai LIN²(), Lixin YU², Xiaolin WANG²()

^1.State Key Laboratory of Water Resource Protection and Utilization in Coal Mining, National Institute of Clean-and-Low-Carbon Energy, Beijing 102209, China
^2.Beijing Key Laboratory of Membrane Materials and Engineering, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China
^3.Hebei Branch, CHN Guohua Energy Investment Co. Ltd. , Zhangjiakou 075000, Hebei, China
^4.School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083, China

Received:2024-07-01 Revised:2024-08-06 Online:2024-12-25 Published:2025-01-03
Contact: Yakai LIN, Xiaolin WANG

摘要/Abstract

摘要：

为了探究“吸附-膜”法从盐湖卤水中提锂的可行性，采用NF270纳滤膜对从卤水得到的硫酸型解吸液中的锂镁分离开展了实验研究和“浓缩-渗滤”模拟计算。首先，测定了NF270膜的基本结构和分离特征，初步确定了压力和pH对Li₂SO₄和MgSO₄单盐溶液的体积通量及截留率的影响。其次，探究了NF270膜对Li₂SO₄/MgSO₄混合溶液的分离效果，结果发现中性条件下NF270纳滤膜对 $S O_{4}^{2 -}$ 的静电排斥效应较强，导致对Li⁺和Mg²⁺的截留率均较高，只有降低pH到等电点以下，才能实现分离；且相对于锂离子摩尔分数（ $x_{L i^{+}}$ ），pH对于锂镁分离性能影响更明显，当 $x_{L i^{+}}$ 为0.40、pH达到1.7时，分离因子可达到10以上。接着，研究了NF270膜对加入其他离子的模拟解吸液中的锂镁分离性能，发现Na⁺、K⁺和Ca²⁺等由于浓度较低，基本不影响膜的锂镁分离因子，且可以同时实现对Ca²⁺和Mg²⁺高截留，降低了后续处理中的结垢风险。最后，基于模拟解吸液的组成和截留率，对含有0.023 mol/L MgSO₄和0.125 mol/L Li₂SO₄的混合溶液进行了预浓缩-连续恒容渗滤过程的模拟计算，得到料液中的Mg²⁺和Li⁺浓度分别为0.20 mol/L和0.66 mol/L，透过液中的浓度分别为0.0025 mol/L和0.17 mol/L，此时Li⁺回收率可以达到75%，证实了通过纳滤渗滤过程实现解吸液中锂镁分离的可行性。

关键词: 纳滤, 锂镁分离, 解吸液, 浓缩-渗滤

Abstract:

In order to explore the feasibility of lithium extraction from salt lake brine by “adsorption-membrane” method, experimental study and “concentration-diafiltration” simulation calculation of lithium-magnesium separation in sulfuric acid desorption solution obtained from brine were carried out by using NF270 nanofiltration membrane. First, the basic structure and separation characteristics of NF270 membranes were determined, and the effects of pressure and pH on the flux and retention of Li₂SO₄ and MgSO₄ for the single salt solution were initially investigated. Secondly, the separation of magnesium and lithium at different pH and Li⁺ mole fraction ( $x_{L i^{+}}$ ) was evaluated and an analysis of the separation was performed. The results showed that under neutral conditions, the strong electrostatic repulsion between the NF270 membrane and $S O_{4}^{2 -}$ resulted in high retention rates of Li⁺ and Mg²⁺. The separation could only be achieved by lowering the pH below the isoelectric point. Compared with $x_{L i^{+}}$ , the effect of pH on the separation of lithium and magnesium was more significant. When $x_{L i^{+}}$ was 0.40 and pH was 1.7, the separation factor could reach more than 10. Then, the separation performance of the NF270 membrane on lithium and magnesium for the simulated desorption solution with other ions was studied. It was found that ions of Na⁺, K⁺ and Ca²⁺ with low concentrations did not affect the separation factors of lithium and magnesium, and the membrane could achieve high retention to Ca²⁺ and Mg²⁺, reducing the risk of scaling in subsequent treatment. Finally, based on the composition and retention rate of the simulated adsorption solution, the selective separation of Li⁺and Mg²⁺ by the NF diafiltration was simulated for the binary solution containing 0.023 mol/L MgSO₄ and 0.125 mol/L Li₂SO₄. After pre-concentration and diafiltration, the concentrations of Mg²⁺ and Li⁺ were 0.20 mol/L and 0.66 mol/L in the feed solution, and 0.0025 mol/L and 0.17 mol/L in the permeate, respectively. At this time, the Li⁺recovery could be up to 75%, proving the feasibility of realizing the separation of magnesium and lithium in the desorption solution by the NF diafiltration process.

Key words: nanofiltration, magnesium and lithium separation, desorption solutions, pre-concentration and diafiltration

中图分类号:

TQ 028

吴雨茜, 唐元晖, 郭强, 林亚凯, 余立新, 王晓琳. 纳滤膜对硫酸型解吸液锂镁分离的实验研究与模拟[J]. 化工学报, 2024, 75(12): 4563-4575.

Yuxi WU, Yuanhui TANG, Qiang GUO, Yakai LIN, Lixin YU, Xiaolin WANG. Experimental study and simulation on nanofiltration separation of lithium and magnesium from sulfate desorption solution[J]. CIESC Journal, 2024, 75(12): 4563-4575.

图/表 13

图1 “吸附-膜”法提锂工艺流程[5]

Fig.1 Process flow of lithium extraction by adsorption-membrane separation method[5]

表1 商业NF膜分离盐湖卤水中锂镁的研究工作总结

Table 1 Summary of research work on the separation of lithium and magnesium from brines of salt lakes by commercial NF membranes

年份	商业化 NF膜型号	研究体系		主要离子的浓度范围/(mol/L)	主要结论	文献
2006	DL	稀释老卤（Li⁺、Mg²⁺、Ca²⁺、Na⁺、K⁺、Cl^-、 $S O_{4}^{2 -}$ 、 $C O_{3}^{2 -}$ ）		Li⁺：0.052； Mg²⁺：0.30	探究了DL膜分离盐酸型老卤中锂镁的可行性，发现DL膜具有较好的锂镁分离能力，同时能有效分离Cl^-和 $S O_{4}^{2 -}$ ，但高锂镁比的原料液会降低Li⁺的产率	[8]
2011	DK	模拟卤水（Li⁺、Mg²⁺、Cl^-）		Li⁺：0.014~0.038； Mg²⁺：0.10~0.20	当压力为1.6 MPa时，Li⁺呈现负截留，且Mg²⁺的截留率最高，分离因子最高为3.2，说明采用DK膜在中性条件下可以实现高镁锂比盐酸体系模拟卤水的分离	[9]
2013	NF90	稀释卤水（Li⁺、Mg²⁺、Na⁺、Cl^-）		Li⁺：0.00087； Mg²⁺：0.013	压力为1.5 MPa时，NF90膜对Mg²⁺的截留率为100%，对Li⁺仅为15%，说明NF90膜对于锂镁离子的截留性能与此前的DK体系差异明显	[10]
2014/2015	DK、DL、HL、NF270	模拟卤水（Li⁺、Mg²⁺、Ca²⁺、Na⁺、K⁺、Cl^-）		Li⁺：0.019~0.046； Mg²⁺：0.11~0.64	对比四种商业化纳滤膜分离盐酸性卤水中锂镁的差异，发现高通量膜（DL、NF270）的分离效果较好；且升高操作压力和降低pH均能够提升NF膜对Mg²⁺、Li⁺的选择分离性能，而高镁锂比和升高进料温度不利于分离	[11-12]
2014/2019	DK、NT102、NT103、NT201、NF90、NF270、XN-45		模拟卤水（Li⁺、Mg²⁺、Na⁺、K⁺、Cl^-、 $S O_{4}^{2 -}$ 、H₃BO₃）	Li⁺：0.0016~0.46； Mg²⁺：0.018~4.9	NT103、NT201膜对Mg²⁺的截留性能较高，具有较好的镁锂分离性能；加入一价阳离子Na⁺、K⁺和H₃BO₃均能提升Li⁺透过率；加入 $S O_{4}^{2 -}$ 会降低Li⁺透过率	[13-14]
2014/2019/2021	DK		稀释老卤/模拟卤水（Li⁺、Mg²⁺、Ca²⁺、Cl^-、 $S O_{4}^{2 -}$ 、B₂O₃）	Li⁺：0.019~0.18； Mg²⁺：0.23~2.4	镁锂比增加，锂离子截留率更小，但过高镁离子含量会降低镁的截留率；高膜表面切向流速降低浓差极化，有利于镁锂分离	[15-17]
2019	NF90和NF270		模拟卤水（Li⁺、Mg²⁺、Cl^-）	Li⁺：0.020； Mg²⁺：0.029~0.12	对比了两种纳滤膜的锂镁分离效果，发现高通量NF270膜更好，原料液中镁锂比下降较多	[18]

表1 商业NF膜分离盐湖卤水中锂镁的研究工作总结

Table 1 Summary of research work on the separation of lithium and magnesium from brines of salt lakes by commercial NF membranes

年份	商业化 NF膜型号	研究体系		主要离子的浓度范围/(mol/L)	主要结论	文献
2006	DL	稀释老卤（Li⁺、Mg²⁺、Ca²⁺、Na⁺、K⁺、Cl^-、 $S O_{4}^{2 -}$ 、 $C O_{3}^{2 -}$ ）		Li⁺：0.052； Mg²⁺：0.30	探究了DL膜分离盐酸型老卤中锂镁的可行性，发现DL膜具有较好的锂镁分离能力，同时能有效分离Cl^-和 $S O_{4}^{2 -}$ ，但高锂镁比的原料液会降低Li⁺的产率	[8]
2011	DK	模拟卤水（Li⁺、Mg²⁺、Cl^-）		Li⁺：0.014~0.038； Mg²⁺：0.10~0.20	当压力为1.6 MPa时，Li⁺呈现负截留，且Mg²⁺的截留率最高，分离因子最高为3.2，说明采用DK膜在中性条件下可以实现高镁锂比盐酸体系模拟卤水的分离	[9]
2013	NF90	稀释卤水（Li⁺、Mg²⁺、Na⁺、Cl^-）		Li⁺：0.00087； Mg²⁺：0.013	压力为1.5 MPa时，NF90膜对Mg²⁺的截留率为100%，对Li⁺仅为15%，说明NF90膜对于锂镁离子的截留性能与此前的DK体系差异明显	[10]
2014/2015	DK、DL、HL、NF270	模拟卤水（Li⁺、Mg²⁺、Ca²⁺、Na⁺、K⁺、Cl^-）		Li⁺：0.019~0.046； Mg²⁺：0.11~0.64	对比四种商业化纳滤膜分离盐酸性卤水中锂镁的差异，发现高通量膜（DL、NF270）的分离效果较好；且升高操作压力和降低pH均能够提升NF膜对Mg²⁺、Li⁺的选择分离性能，而高镁锂比和升高进料温度不利于分离	[11-12]
2014/2019	DK、NT102、NT103、NT201、NF90、NF270、XN-45		模拟卤水（Li⁺、Mg²⁺、Na⁺、K⁺、Cl^-、 $S O_{4}^{2 -}$ 、H₃BO₃）	Li⁺：0.0016~0.46； Mg²⁺：0.018~4.9	NT103、NT201膜对Mg²⁺的截留性能较高，具有较好的镁锂分离性能；加入一价阳离子Na⁺、K⁺和H₃BO₃均能提升Li⁺透过率；加入 $S O_{4}^{2 -}$ 会降低Li⁺透过率	[13-14]
2014/2019/2021	DK		稀释老卤/模拟卤水（Li⁺、Mg²⁺、Ca²⁺、Cl^-、 $S O_{4}^{2 -}$ 、B₂O₃）	Li⁺：0.019~0.18； Mg²⁺：0.23~2.4	镁锂比增加，锂离子截留率更小，但过高镁离子含量会降低镁的截留率；高膜表面切向流速降低浓差极化，有利于镁锂分离	[15-17]
2019	NF90和NF270		模拟卤水（Li⁺、Mg²⁺、Cl^-）	Li⁺：0.020； Mg²⁺：0.029~0.12	对比了两种纳滤膜的锂镁分离效果，发现高通量NF270膜更好，原料液中镁锂比下降较多	[18]

表2 解吸液的主要成分

Table 2 The main components of the desorption solution

解吸液编号

Li⁺/

(mol/L)

Na⁺/

(mol/L)

K⁺/(mol/L)

Mg²⁺/(mol/L)

Ca²⁺/

(mol/L)

表3 实验原料液组成

Table 3 The concentrations of the feed solutions

原料液编号	原料液中离子浓度/(mol/L)					pH
原料液编号	Li⁺	Mg²⁺	Ca²⁺	Na⁺	K⁺	pH
1~4	0.19	0	0	0	0	7.7、4.6、3.1、1.7
5~8	0	0.093	0	0	0	7.7、4.6、3.1、1.7
9~12	0.14	0.023	0	0	0	7.7、4.6、3.1、1.7
13	0.019	0.084	0	0	0	1.7
14	0.046	0.070	0	0	0	1.7
15	0.14	0.023	0	0	0	1.7
16	0.17	0.0093	0	0	0	1.7
17	0.25	0.023	0.0014	0.067	0.016	1.7

表4 Stokes半径及扩散系数［22-23］

Table 4 Stokes radius and diffusion coefficients of various ions considered in this study［22-23］

离子	Stokes半径/nm	扩散系数/(10^-9 m²/s)
Li⁺	0.238	1.03
K⁺	0.125	1.96
Na⁺	0.184	1.33
Mg²⁺	0.347	0.706
Ca²⁺	0.310	0.79
$S O_{4}^{2 -}$	0.230	1.065

表4 Stokes半径及扩散系数［22-23］

Table 4 Stokes radius and diffusion coefficients of various ions considered in this study［22-23］

离子	Stokes半径/nm	扩散系数/(10^-9 m²/s)
Li⁺	0.238	1.03
K⁺	0.125	1.96
Na⁺	0.184	1.33
Mg²⁺	0.347	0.706
Ca²⁺	0.310	0.79
$S O_{4}^{2 -}$	0.230	1.065

图2 纳滤透过实验装置示意图1—原料槽;2—柱塞泵;3—膜元件;4—流量计;5—压力表;6—温度计;7—阀门

Fig.2 Schematic diagram for the cross-flow NF equipment adopted in the experiments1—raw material tank; 2—plunger pump; 3—membrane; 4—flowmeter; 5—pressure gauge; 6—thermometer; 7—valve

图3 NF270膜的纯水渗透性能、截留性能和Zeta电位

Fig.3 The pure water permeability, rejection performance, and Zeta potential of the NF270 membrane

图4 pH和操作压力对NF270膜对Li2SO4/MgSO4溶液的分离和透过性能的影响

Fig.4 The effects of pH and operating pressure on the separation and permeation performance of the NF270 membrane for Li₂SO₄/MgSO₄ solutions

图5 pH和操作压力对NF270膜对Li2SO4和MgSO4混合盐溶液的分离和透过性能的影响

Fig.5 The effects of pH and operating pressure on the separation and permeation performance of the NF270 membrane for Li2SO4/MgSO4 mixed solutions

图6 xLi+和操作压力对NF270膜对硫酸型混合盐溶液的分离和透过性能的影响

Fig.6 The effects of xLi+ and operating pressure on the separation and permeation performance of the NF270 membrane for Li2SO4/MgSO4 mixed solutions

图7 不同操作压力下NF270膜对模拟解吸液的分离和渗透性能

Fig.7 Separation and permeation performance of the NF270 membrane for simulated desorption solution under different operating pressures

图8 预浓缩-连续恒容渗滤过程料液中Mg2+和Li+浓度比随浓缩倍数（V0/VF）与水消耗量（Vw/V0′）的变化

Fig.8 Relationship between the concentration ratio of Mg2+and Li+ in the feed solution during preconcentration-continuous constant volume percolation with the concentration factor (V0/VF ) and the water consumption (Vw/V0′) during the percolation process

表5 整个渗滤过程中的水消耗量、料液及透过液的体积、盐浓度和锂离子回收率变化

Table 5 Variations of water consumption， volume，concentration of feed and permeate and the yield of lithium during the whole concentrationinfiltration process

渗滤过程	水消耗量	料液			透过液			Li⁺回收率/%
渗滤过程	水消耗量	体积	c(Mg²⁺)/ (mol/L)	c(Li⁺)/ (mol/L)	体积	c(Mg²⁺)/ (mol/L)	c(Li⁺)/ (mol/L)	Li⁺回收率/%
初始	—	V₀	0.023	0.25	—	—	—	—
预浓缩后	0	(1/10)V₀	0.21	1.22	(9/10)V₀	0.0017	0.14	50
连续恒容渗滤后	1/5V₀	(1/10)V₀	0.20	0.66	(11/10)V₀	0.0025	0.17	75

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纳滤膜对硫酸型解吸液锂镁分离的实验研究与模拟

Experimental study and simulation on nanofiltration separation of lithium and magnesium from sulfate desorption solution

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