聚氯乙烯锂离子筛膜的制备及其在卤水中的锂吸附性能

王蕾; 王磊

doi:10.13801/j.cnki.fhclxb.20221124.002

聚氯乙烯锂离子筛膜的制备及其在卤水中的锂吸附性能

doi: 10.13801/j.cnki.fhclxb.20221124.002

王蕾,
王磊^,

西安建筑科技大学　环境与市政工程学院，陕西省膜分离重点实验室，陕西省膜分离技术研究院，西安 710055

基金项目: 陕西省自然科学基础研究专项基金(2019 JM-596)；陕西省技术创新引导计划基金(S2019-YD-CGXNX-0049)；陕西省科技成果转移与推广计划(2018 SJRG-X-02)

详细信息

通讯作者:
王磊，博士，教授，博士生导师，研究方向为膜分离技术　E-mail: wl0178@126.com

中图分类号: TQ131.11；TQ028.8；TB331
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出版历程
- 收稿日期: 2022-09-30
- 修回日期: 2022-11-06
- 录用日期: 2022-11-12
- 网络出版日期: 2022-11-25
- 刊出日期: 2023-09-15

Preparation of polyvinyl chloride lithium ion sieve membrane and its lithium adsorption properties in brine

WANG Lei,
WANG Lei^,

School of Environmental and Municipal Engineering, Xi'an University of Architecture and Technology, Key Laboratory of Membrane Separation of Shaanxi Province, Research Institute of Membrane Separation Technology of Shaanxi Province, Xi’an 710055, China

Funds: Project Supported by Natural Science Basic Research Plan in Shaanxi Province of China (2019 JM-596); Technology Innovation Leading Program of Shaanxi (S2019-YD-CGXNX-0049); Guidance Fund for Transformation of Scientific and Technological Achievements (2018 SJRG-X-02)

摘要

摘要: 锂离子筛的成型技术对于其在卤水中的工业化生产应用具有重要意义。以聚氯乙烯(PVC)为成膜材料，聚甲基丙烯酸甲酯(PMMA)和聚乙烯吡咯烷酮(PVP_k30)为改性剂，制备了负载Li_1.6Mn_1.6O₄的PVC锂离子筛前驱体膜，研究了膜经稀盐酸抽锂后得到的PVC锂离子筛膜对锂的吸附性能及循环吸附解吸性能等，并对离子筛膜进行了吸附动力学及吸附等温模型分析。结果表明：PVC浓度为10wt%，PMMA的添加量为6wt%，PVP_k30的添加量为2wt%，Li_1.6Mn_1.6O₄含量为20wt%联用时，制得的离子筛膜吸附量为1336.30 mg/m²。经0.1 mol·L⁻¹ HCl溶液解吸，约2 h时解吸达到平衡，锰的溶损率为0.56%左右。在卤水中进行了10次循环吸附解吸过程，吸附量降至1294.16 mg/m²，吸附量仅损失了3%。在含有多种复杂离子如Na⁺、K⁺、Mg²⁺和Ca²⁺的卤水中，锂离子筛膜对Li⁺有很高的选择性。说明该PVC锂离子筛膜结构稳定，循环利用性能优异，有利于其工业化应用。PVC锂离子筛膜的吸附过程更符合伪二级动力学方程及Langmuir吸附等温模型，说明该吸附过程的吸附类型为单分子层化学吸附。膜状的离子筛对于从盐湖卤水等液态锂资源中提取锂具有很大的开发潜力。
- 锂离子筛 /
- 聚氯乙烯 /
- 盐湖卤水 /
- 吸附 /
- 膜 /
- 分离
Abstract: Lithium ion sieve formation technology for Li⁺ recovery industrial production and application from brine is very important. Polyvinyl chloride (PVC)-Li_1.6Mn_1.6O₄ lithium ion sieve precursor membrane was prepared by blend of Li_1.6Mn_1.6O₄ with PVC, polymethyl methacrylate (PMMA) and polyvinylpyrrolidone (PVP_k30). After the precursor membrane was treated with HCl solution it can uptake lithium. A series of experiments for examining its adsorption and cyclic performance were carried out. The adsorption isotherm model and the adsorption kinetics of PVC lithium ion sieve membrane were analyzed. The results showed that the adsorption capacity of PVC lithium ion sieve membrane was 1336.30 mg/m² when the concentration of PVC was 10wt%, the content of PMMA was 6wt%, the content of PVP_k30 was 2wt%, and the amount of loading of Li_1.6Mn_1.6O₄ was 20wt%. After treated with 0.1 mol·L⁻¹ HCl for 2 h, the lithium extraction reached equilibrium and the dissolution loss rate of Mn²⁺ was about 0.56%. After 10 cycles of adsorption and desorption in brine, the Li⁺ adsorption capacity was lost only 3.0% (from 1336.30 mg/m² to 1294.16 mg/m²). The PVC lithium ion sieve membrane showed great selectivity for Li⁺ in brine containing a variety of complex ions such as Na⁺, K⁺, Mg²⁺ and Ca²⁺. The PVC lithium ion sieve membrane has stable structure and excellent recycling performance, which is conducive to its industrial application. The PVC lithium ion sieve membrane accords with the pseudo second order kinetic equation and Langmuir adsorption isotherm model, indicating a monolayer chemisorption. It is potential to be used in enrichment and recovery of lithium from salt lake brine and other liquid lithium sources.
- lithium ion-sieve /
- polyvinyl chlorides /
- brine /
- absorption /
- membranes /
- separation

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图 1 聚氯乙烯(PVC)浓度对膜拉力和断裂伸长率的影响

Figure 1. Effects of polyvinyl chloride (PVC) concentration on tensile force and elongation at break of membranes

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图 2 PVC浓度对锂离子筛膜吸附量的影响

Figure 2. Relation between Li⁺ adsorptive capacity and concentration of PVC

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图 3 不同PVC浓度条件下制备的锂离子筛膜的SEM图像

Figure 3. SEM images of PVC lithium ion sieve membranes of different PVC concentration

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图 4 Li_1.6Mn_1.6O₄的添加量对锂离子筛膜吸附量的影响

Figure 4. Relation between Li⁺ adsorptive capacity and the content of Li_1.6Mn_1.6O₄

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图 5 不同Li_1.6Mn_1.6O₄含量的PVC锂离子筛膜的SEM图像

Figure 5. SEM images of PVC lithium ion sieve membranes of different Li_1.6Mn_1.6O₄ contents

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图 6 聚甲基丙烯酸甲酯(PMMA)添加量对PVC锂离子筛膜吸附性能的影响

Figure 6. Relation between Li⁺ adsorptive capacity and the content of polymethyl methacrylate (PMMA)

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图 7 PMMA含量对膜拉力和断裂伸长率的影响

Figure 7. Tensile force and elongation at break of membranes with different PMMA contents

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图 8 不同PMMA添加量的PVC锂离子筛膜接触角θ测试

Figure 8. Contact angle θ measurement of PVC lithium ion sieve membranes with different PMMA contents

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图 9 不同PMMA含量的PVC锂离子筛膜的SEM图像

Figure 9. SEM images of PVC lithium ion sieve membranes of different PMMA contents

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图 10 聚乙烯吡咯烷酮(PVP_k30)添加量对 PVC 锂离子筛膜吸附性能的影响

Figure 10. Relation between Li⁺ adsorptive capacity and the content of polyvinylpyrrolidone (PVP_k30)

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图 11 PVP_k30含量对膜拉力和断裂伸长率的影响

Figure 11. Tensile force and elongation at break of membranes with different PVP_k30 contents

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图 12 不同PVP_k30含量PVC锂离子筛膜的SEM表面 ((a₁)~(d₁)) 和断面 ((a₂)~(d₂)) 图像

Figure 12. SEM images of the surface ((a₁)-(d₁)) and section ((a₂)-(d₂)) in PVC lithium ion sieve membranes of different PVP_k30 contents

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图 13 PVC锂离子筛膜的FTIR图谱

Figure 13. FTIR spectra of PVC lithium ion sieve membrane

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图 14 不同Li_1.6Mn_1.6O₄添加量的PVC锂离子筛膜的XRD图谱

Figure 14. XRD patterns of PVC lithium ion sieve membrane with different Li_1.6Mn_1.6O₄ contents

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图 15 PVC锂离子筛膜吸附量

Figure 15. Adsorption capacity of PVC lithium ion sieve membrane

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图 16 PVC锂离子筛膜锂解吸率及锰溶损率

Figure 16. Extraction of Li⁺ and dissolution loss rate of Mn²⁺ from PVC lithium ion sieve membrane

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图 17 PVC锂离子筛膜循环过程的锰溶损率及锂吸附量

Figure 17. Dissolution loss rate of Mn²⁺ and lithium adsorption capacity of PVC lithium ion sieve membrane in the cycling process

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图 18 锂离子筛膜吸附锂的动力学曲线

Figure 18. Kinetics of Li⁺ adsorption by PVC lithium ion sieve membrane

Q_t—Li⁺ adsorption capacity at time t

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图 19 PVC锂离子筛膜的等温吸附拟合曲线

Figure 19. Adsorption isotherm of Li⁺ adsorption by PVC lithium ion sieve membrane

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表 1 青海昆特依盐湖卤水水质成分

Table 1. Components of the Qinghai Kunty salt lake brine

Metal ion	Li⁺	Mg²⁺	Ca²⁺	K⁺	Na⁺	Mn²⁺	Cd²⁺	Cr³⁺	Cu²⁺	Fe²⁺	Mg²⁺/Li⁺
Initial concentration/(g·L⁻¹)	0.15	10.52	0.072	3.63	5.39	−	0.0034	0.0069	0.0024	0.01	70

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表 2 不同致孔剂聚乙烯吡咯烷酮PVP_k30添加量的PVC锂离子筛膜的膜通量参数

Table 2. Membrane flux performance of PVC lithium ion sieve membrane with different pore-causing agent polyvinylpyrrolidone PVP_k30 contents

PVP_k30 content/wt%	Brine flux /(L·m²·h⁻¹)
0	228.06
1	311.20
2	488.83
3	593.78
4	669.69

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表 3 锂离子筛膜从卤水中分离锂离子的性能

Table 3. Performance of PVC lithium ion sieve membrane the separation of Li⁺ from other cations in brine

Cations	C₀/(mg·L⁻¹)	C_e/(mg·L⁻¹)	Q/(mg·m⁻²)	Q/(mmol·m⁻²)	K_d/(L·m⁻²)	$\alpha_{\rm{M}}^{{\rm{L i}}} $	C_F/(L·m⁻²)
Li⁺	128.98	89.22	1335.78	192.45	14.972	1.00	10.356
Mg²⁺	10155.32	10054.91	3373.78	138.81	0.335	44.69	0.332
K⁺	3820.16	3804.65	521.14	13.33	0.137	109.28	0.136
Na⁺	4370.87	4336.58	1152.14	50.09	0.266	56.29	0.264
Ca²⁺	72	71	–	–	–	–	–
Notes: C₀ and C_e—Initial and equilibrium Li⁺ concentrations in brine, respectively; Q—Li⁺ adsorption capacity; K_d—Distribution coefficient; α—Separation factor; C_F—Concentration factor; M—Li, Na, K, Mg and Ca.

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