LiAl-CO₃ layered double hydroxides (LiAl-CO3 LDHs) are adsorbents promising for lithium recovery from low-grade carbonate-type salt-lake brines due to their excellent structural stability and selective lithium-ion affinity. However, conventional synthesis routes, such as chemical precipitation and hydrothermal methods, are limited by high energy consumption, long reaction times, and complex operations procedures, which hinder large-scale application. Herein, a facile and efficient electrochemical strategy was developed for the synthesis of LiAl-CO₃ LDHs. The effects of electrolyte type, Li/Al molar ratio, and reaction temperature on LDHs formation were systematically investigated. Under the optimal conditions (Na₂SO₄ as electrolyte, Li/Al molar ratio of 4.5:1, reaction temperature of 80 °C and pH = 11), LiAl-CO₃ LDHs with a well-defined layered structure, high specific surface area, and the highest lithium content of 15.53 mg/g were obtained. Moreover, real lithium precipitation mother liquor was directly utilized as lithium and carbonate sources to synthesize LiAl-CO₃ LDHs, yielding a lithium content of 4.02 mg/g. Lithium was efficiently desorbed from LiAl-CO₃ LDHs via the hydrothermal process, achieving an average desorption rate of 90.72%. The lithium desorption mechanism was revealed through structural characterization before and after hydrothermal treatment. This work provides a sustainable and scalable synthesis route for aluminum-based lithium adsorbents toward efficient lithium recovery from industrial lithium precipitation mother liquor.
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