溶胶-凝胶软模板法合成锂钛离子筛

摘要/Abstract

摘要： 以乙酸锂和钛酸丁酯为锂源和钛源,十六烷基三甲基溴化铵(CTAB)为软模板,采用溶胶-凝胶法,通过焙烧得到添加CTAB的锂钛化合物(Li₄Ti₅O₁₂),经过盐酸酸洗,制备出锂钛离子筛(H₄Ti₅O₁₂, HTO)。经过热重分析(TG-DTG)、X射线(XRD)、扫描电镜(SEM)、接触角及性能测试,考察了锂钛离子筛的晶相、形貌及时间对吸附容量的影响。对比CTAB的加入量,0.1 g的CTAB的离子筛前驱体杂质更少,晶相比较纯。HTO准二级动力学相关系数R²(0.997 24)大于准一级动力学相关系数R²(0.984 35),该吸附过程符合化学吸附。HTO在Li⁺溶液中24 h的吸附容量达到24.44 mg/g,经过8次吸附脱附后,吸附容量仍保持在23.68 mg/g,仅降低3.1%。因此,HTO有良好的循环吸附性能和稳定性,具有很广阔的市场前景。

关键词: 软模版, 溶胶-凝胶法, 锂钛离子筛, 尖晶石结构, 吸附容量, 循环使用

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

中图分类号:

孙建科, 陈进, 赵坤, 刘璐, 刘莹莹, 易大伟. 溶胶-凝胶软模板法合成锂钛离子筛[J]. 人工晶体学报, 2021, 50(11): 2144-2149.

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.

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