Synthesis of Lithium Titanium Ion Sieve by Sol-Gel Soft Template Method

Abstract

Abstract: With lithium acetate and butyl titanate as lithium and titanium sources, and cetyltrimethylammonium bromide (CTAB) as the soft template, the sol-gel method is used to obtain CTAB-added lithium titanium by roasting. The compound (Li₄Ti₅O₁₂) was pickled with hydrochloric acid to prepare a lithium titanium ion sieve (H₄Ti₅O₁₂, HTO). The effects of crystal phase, morphology and time on the adsorption capacity of lithium titanium ion sieve were investigated by thermogravimetric analysis (TG-DTG), X-ray diffraction (XRD), scanning electron microscopy (SEM), contact angle and performance tests. Compared with the addition amount of CTAB, 0.1 g CTAB ionic sieve precursor has fewer impurities and pure crystal phase. The quasi-second-order kinetic correlation coefficient R²(0.997 24) of HTO is greater than that of first-order kinetic correlation coefficient R²(0.984 35), indicating that the adsorption process is consistent with chemisorption. The adsorption capacity of HTO in Li⁺ solution for 24 h reaches 24.44 mg/g, and after 8 times of adsorption and desorption, the adsorption capacity remains at 23.68 mg/g, only reduces by 3.1%. Therefore, HTO has good cyclic adsorption performance and stability, and has a broad market prospect.

Key words: soft template, sol-gel method, lithium titanium ion sieve, spinel structure, adsorption capacity, recycling

CLC Number:

SUN Jianke, CHEN Jin, ZHAO Kun, LIU Lu, LIU Yingying, YI Dawei. Synthesis of Lithium Titanium Ion Sieve by Sol-Gel Soft Template Method[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2021, 50(11): 2144-2149.

References

[1] PENG S K, WANG C, YAN S J, et al. Facile carbon fluoride/sulfur hybrid cathode for high-rate lithium batteries[J]. ChemElectroChem, 2019, 6(13): 3291-3297.
[2] PENG R, LI Y X, SU H, et al. Experiment and calculation: the Li(Zn, Mn)PO₄ solid solution ceramics with low dielectric constant, high quality factor, and low densification temperature[J]. Journal of Alloys and Compounds, 2020, 842: 155709.
[3] ENTRINGER J, REIMANN M, NORMAN A, et al. Influence of Cu/Li ratio on the microstructure evolution of bobbin-tool friction stir welded Al-Cu-Li alloys[J]. Journal of Materials Research and Technology, 2019, 8(2): 2031-2040.
[4] PERSHINA S V, ANTONOV B D, FARLENKOV A S, et al. Glass-ceramics in Li_1+xAl_xGe_2-x(PO₄)₃ system: the effect of Al₂O₃ addition on microstructure, structure and electrical properties[J]. Journal of Alloys and Compounds, 2020, 835: 155281.
[5] VANYOREK L, KISS D, PREKOB Á, et al. Application of nitrogen doped bamboo-like carbon nanotube for development of electrically conductive lubricants[J]. Journal of Materials Research and Technology, 2019, 8(3): 3244-3250.
[6] 董殿权,王永顺,房超.多孔掺杂型钛系离子筛的制备及吸附性能[J].化工学报,2017,68(7):2812-2817.
DONG D Q, WANG Y S, FANG C. Preparation and adsorption properties of porous doped titanium series[J]. CIESC Journal, 2017, 68(7): 2812-2817(in Chinese).
[7] 郭佳明,刘明言,吴强,等.硝酸锂改性钛系离子筛的制备及其吸附性能[J].化工学报,2020,71(2):879-888.
GUO J M, LIU M Y, WU Q, et al. Preparation and adsorption performance of titanium based lithium ion sieve improved by LiNO₃[J]. CIESC Journal, 2020, 71(2): 879-888(in Chinese).
[8] XUE F, ZHANG X X, NIU Y, et al. Preparation and evaluation of α-Al₂O₃ supported lithium ion sieve membranes for Li⁺ extraction[J]. Chinese Journal of Chemical Engineering, 2020, 28(9): 2312-2318.
[9] 吴静,任秀莲,魏琦峰.盐湖卤水中锂的分离提取研究进展[J].无机盐工业,2020,52(12):1-6.
WU J, REN X L, WEI Q F. Research progress on separation and extraction of lithium from salt-lake brine[J]. Inorganic Chemicals Industry, 2020, 52(12): 1-6(in Chinese).
[10] LI H F, LI L J, JI L M, et al. The extraction ability and mechanism in extraction lithium by several organic extractants[J]. Chemical Physics Letters, 2019, 733: 136668.
[11] MARTHI R, SMITH Y R. Selective recovery of lithium from the great salt lake using lithium manganese oxide-diatomaceous earth composite[J]. Hydrometallurgy, 2019, 186: 115-125.
[12] ZHAO X Y, LI G Y, FENG M H, et al. Semi-continuous electrochemical extraction of lithium from brine using CF-NMMO/AC asymmetric hybrid capacitors[J]. Electrochimica Acta, 2020, 331: 135285.
[13] PRAMANIK B K, ASIF M B, KENTISH S, et al. Lithium enrichment from a simulated salt lake brine using an integrated nanofiltration-membrane distillation process[J]. Journal of Environmental Chemical Engineering, 2019, 7(5): 103395.
[14] LIU G, ZHAO Z W, HE L H. Highly selective lithium recovery from high Mg/Li ratio brines[J]. Desalination, 2020, 474: 114185.
[15] WEI S D, WEI Y F, CHEN T, et al. Porous lithium ion sieves nanofibers: general synthesis strategy and highly selective recovery of lithium from brine water[J]. Chemical Engineering Journal, 2020, 379: 122407.
[16] TIAN X Y, LIAN S X, WEN J, et al. Egg albumin-assisted sol-gel synthesis and photo-catalytic activity of SnO₂ micro/nano-structured biscuits[J]. Journal of Sol-Gel Science and Technology, 2018, 85(2): 402-412.
[17] 张理元,杨东睿,周大利.多孔陶瓷基锂离子吸附剂的制备及性能研究[J].四川大学学报(自然科学版),2017,54(3):611-616.
ZHANG L Y, YANG D R, ZHOU D L. Preparation and adsorption performance of porous ceramic-based lithium ion adsorbent[J]. Journal of Sichuan University (Natural Science Edition), 2017, 54(3): 611-616(in Chinese).
[18] 孟祥坤,贺帅,刘银凤,等.溶剂热法合成锂钛复合氧化物的研究[J].当代化工,2020,49(11):2388-2392.
MENG X K, HE S, LIU Y F, et al. Study on synthesis of lithium-titanium composite oxide by solvothermal method[J]. Contemporary Chemical Industry, 2020, 49(11): 2388-2392(in Chinese).
[19] WANG S L, LI P, ZHANG X, et al. Selective adsorption of lithium from high Mg-containing brines using H_xTiO₃ ion sieve[J]. Hydrometallurgy, 2017, 174: 21-28.
[20] LI X W, CHAO Y H, CHEN L L, et al. Taming wettability of lithium ion sieve via different TiO₂ precursors for effective Li recovery from aqueous lithium resources[J]. Chemical Engineering Journal, 2020, 392: 123731.
[21] LAWAGON C P, NISOLA G M, CUEVAS R A I, et al. Development of high capacity Li⁺ adsorbents from H₂TiO₃/polymer nanofiber composites: systematic polymer screening, characterization and evaluation[J]. Journal of Industrial and Engineering Chemistry, 2019, 70: 124-135.
[22] HONG H J, PARK I S, RYU T, et al. Macroporous hydrogen manganese oxide/Al₂O₃ for effective lithium recovery from seawater: effects of the macropores vs. mesopores[J]. Industrial & Engineering Chemistry Research, 2019, 58(19): 8342-8348.