Battery-grade lithium carbonate(Li_(2)CO_(3))with a purity of higher than 99.5 wt%is of great importance as a high value-added lithium salt.However,influences of different reaction systems and process control on produ...Battery-grade lithium carbonate(Li_(2)CO_(3))with a purity of higher than 99.5 wt%is of great importance as a high value-added lithium salt.However,influences of different reaction systems and process control on product purity remain unclear.Herein,a membrane dispersion microreactor was used to enhance the mass transfer of preparation and purification processes in homogeneous and heterogeneous system.Synthetic systems of Na_(2)CO_(3)–LiCl,NH_(4)HCO_(3)–LiCl,and NH_(3)·H_(2)O−CO_(2)−LiCl,CO_(2)purification based on carbonation and decomposition were adopted.The Li_(2)CO_(3)purity was increased by the improvement of mixing performance.The carbonation time was reduced by 62.5%and 58.3%for the NH_(3)·H_(2)O−CO_(2)and CO_(2)purification systems,respectively.In the two ammonia-based systems,Li_(2)CO_(3)particles with a purity of 99.7–99.8 wt%were one-step prepared with a size of 3–5μm,which also met the requirement of the battery-grade standard.The purity was further increased to 99.9 wt%by CO_(2)purification and LiHCO_(3)decomposition.The investigation could provide a feasible alternative for the controllable preparation of battery-grade Li_(2)CO_(3)in one or multiple steps.展开更多
This work investigates the flow and agglomeration behaviors of battery grade Li_(2)CO_(3)powder and the influence of stearic acid surface modification.The degree of agglomeration is directly related to the uniformity ...This work investigates the flow and agglomeration behaviors of battery grade Li_(2)CO_(3)powder and the influence of stearic acid surface modification.The degree of agglomeration is directly related to the uniformity of Li_(2)CO_(3)and its powder mixtures.According to the Chinese National Nonferrous Metal Industry Standard,battery grade Li_(2)CO_(3)powder has D50 equal to 3–8μm which belongs to a micron-sized superfine powder.Therefore,with the extension of storage time,the serious agglomeration phenomenon occurs due to the large specific surface area and rough and irregular powder particles.The Hausner ratio(HR)of the unmodified sample increases from 1.14 to 1.41,and the corresponding flowability is classified as good to poor.Instead,among samples with doping stearic acid,the optimum amount of it is 0.10 wt%which exhibits an extremely stable HR value from 1.14 to 1.16.Meanwhile,after 156 days,the repose angle(AR)obtained for samples without surface modification and using 0.10 wt%stearic acid are calculated to be 49°and 28°,respectively.Based on the values of HR and AR,the flowability of the unmodified sample is poor while the sample modified with 0.10 wt%of stearic acid still maintain excellent powder flow property.Moreover,The LiMn_(2)O_(4)cathode material synthesized from modified Li_(2)CO_(3)powder with a stearic acid content of 0.10 wt%exhibits good crystallinity and comparable electrochemical performance to that prepared by commercial Li_(2)CO_(3).These results indicate that stearic acid has the potential to be an ideal modifier for battery grade Li_(2)CO_(3)powder that needs to be kept for a long time.展开更多
基金the support from the National Natural Science Foundation of China(grant Nos.22278014,2227801521978008,21606008)the Innovation Fund of SIN0PEC Catalyst Co.Ltd-State Key Laboratory of Chemical Resource Engineering(grant No.36100000-22-ZC0607-0041).
文摘Battery-grade lithium carbonate(Li_(2)CO_(3))with a purity of higher than 99.5 wt%is of great importance as a high value-added lithium salt.However,influences of different reaction systems and process control on product purity remain unclear.Herein,a membrane dispersion microreactor was used to enhance the mass transfer of preparation and purification processes in homogeneous and heterogeneous system.Synthetic systems of Na_(2)CO_(3)–LiCl,NH_(4)HCO_(3)–LiCl,and NH_(3)·H_(2)O−CO_(2)−LiCl,CO_(2)purification based on carbonation and decomposition were adopted.The Li_(2)CO_(3)purity was increased by the improvement of mixing performance.The carbonation time was reduced by 62.5%and 58.3%for the NH_(3)·H_(2)O−CO_(2)and CO_(2)purification systems,respectively.In the two ammonia-based systems,Li_(2)CO_(3)particles with a purity of 99.7–99.8 wt%were one-step prepared with a size of 3–5μm,which also met the requirement of the battery-grade standard.The purity was further increased to 99.9 wt%by CO_(2)purification and LiHCO_(3)decomposition.The investigation could provide a feasible alternative for the controllable preparation of battery-grade Li_(2)CO_(3)in one or multiple steps.
文摘This work investigates the flow and agglomeration behaviors of battery grade Li_(2)CO_(3)powder and the influence of stearic acid surface modification.The degree of agglomeration is directly related to the uniformity of Li_(2)CO_(3)and its powder mixtures.According to the Chinese National Nonferrous Metal Industry Standard,battery grade Li_(2)CO_(3)powder has D50 equal to 3–8μm which belongs to a micron-sized superfine powder.Therefore,with the extension of storage time,the serious agglomeration phenomenon occurs due to the large specific surface area and rough and irregular powder particles.The Hausner ratio(HR)of the unmodified sample increases from 1.14 to 1.41,and the corresponding flowability is classified as good to poor.Instead,among samples with doping stearic acid,the optimum amount of it is 0.10 wt%which exhibits an extremely stable HR value from 1.14 to 1.16.Meanwhile,after 156 days,the repose angle(AR)obtained for samples without surface modification and using 0.10 wt%stearic acid are calculated to be 49°and 28°,respectively.Based on the values of HR and AR,the flowability of the unmodified sample is poor while the sample modified with 0.10 wt%of stearic acid still maintain excellent powder flow property.Moreover,The LiMn_(2)O_(4)cathode material synthesized from modified Li_(2)CO_(3)powder with a stearic acid content of 0.10 wt%exhibits good crystallinity and comparable electrochemical performance to that prepared by commercial Li_(2)CO_(3).These results indicate that stearic acid has the potential to be an ideal modifier for battery grade Li_(2)CO_(3)powder that needs to be kept for a long time.
