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In Situ FBRM Analysis of Additive-Controlled Reactive Crystallization of Lithium Carbonate
Eder Piceros1, Ricardo I Jeldres2, Karien I García3
1Facultad de Ingeniería y Arquitectura, Universidad Arturo Prat, Iquique 1110939, Chile.
Molecules (Basel, Switzerland)
|March 14, 2026
Summary
This study explores lithium carbonate (Li₂CO₃) crystallization using additives. Poly(acrylic acid) (PAA), sodium hexametaphosphate (SHMP), and sodium tripolyphosphate (STPP) control nucleation and growth dynamics for tailored Li₂CO₃ precipitation.
Area of Science:
- Materials Science
- Chemical Engineering
- Crystallization Science
Background:
- Reactive crystallization is crucial for producing solid compounds like lithium carbonate (Li₂CO₃).
- Controlling particle size and morphology during Li₂CO₃ precipitation is essential for its applications.
- Understanding nucleation and growth kinetics is key to optimizing reactive crystallization processes.
Purpose of the Study:
- To investigate the reactive crystallization of Li₂CO₃ under high supersaturation.
- To analyze the impact of poly(acrylic acid) (PAA), sodium hexametaphosphate (SHMP), and sodium tripolyphosphate (STPP) on Li₂CO₃ nucleation and growth dynamics.
- To provide mechanistic insights for controlling Li₂CO₃ precipitation processes through additive selection.
Main Methods:
- Focused beam reflectance measurement (FBRM) for in situ monitoring of crystallization.
- Rapid mixing of concentrated LiCl and Na₂CO₃ solutions at 65 °C.
- Systematic analysis of additive effects (PAA, SHMP, STPP) on nucleation and growth.
- Scanning electron microscopy (SEM) for characterizing Li₂CO₃ aggregate morphology.
Main Results:
- The process is characterized by an initial supersaturation pulse governing early nucleation and population restructuring.
- PAA suppressed fines and promoted coarse fraction formation, with concentration- and time-dependent effects.
- SHMP strongly inhibited both nucleation and growth, particularly growth.
- STPP showed a dose-dependent response, maintaining nucleation but limiting growth.
- SEM confirmed spherulitic Li₂CO₃ aggregates, with morphology influenced by the additives.
Conclusions:
- Targeted additive selection enables precise control over population dynamics and solid properties in Li₂CO₃ reactive crystallization.
- The study provides valuable mechanistic guidance for designing and controlling Li₂CO₃ precipitation processes.
- Additive choice significantly influences the interplay between nucleation and growth under high supersaturation conditions.
