微反应法连续制备纳米Li_2CO_3的研究
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摘要
采用微化学反应法连续制备纳米碳酸锂,利用XRD、SEM和激光粒度仪对不同工艺条件制备的碳酸锂的粒径、产率和形貌进行了分析。结果表明,采用微反应法可连续制得平均粒径约为178nm的均匀类球形碳酸锂,产率可达90. 01%;实验最佳工艺条件为:反应物浓度C_(碳酸钠)=6 mol/L,C_(氯化锂)=3 mol/L,C_(碳酸钠):C_(氯化锂)=2:1,进料流量F=40mL/min,反应温度T=20°C。对比传统液相沉淀法与微反应法,微反应法制备碳酸锂的过程连续、产率高,得到的碳酸锂粒径更小、分布更均匀。
The nanosized lithium carbonate was continuously synthesized via microreaction method. The particle size,yield and morphology of lithium carbonate prepared by different process conditions were analyzed by XRD,SEM and laser particle size analyzer. The results show that the uniform spherical lithium carbonate with an average particle size of ca. 178 nm and yield of 90. 01% can be continuously synthesized via the microreaction method. The optimum experimental conditions in microreactor are as follows:reactant concentration C_(Sodium carbonate)= 6 mol/L,C_(Lithium chloride)= 3 mol/L,C_(Sodium carbonate):C_(Lithium chloride)= 2:1,feed flow rate F = 40 mL/min,reaction temperature T = 20 ℃. Compared with the traditional liquid phase precipitation method,the process of synthesizing lithium carbonate via the microreaction method is continuous with higher yield,and the lithium carbonate has smaller particle size and more homogeneous.
The nanosized lithium carbonate was continuously synthesized via microreaction method. The particle size,yield and morphology of lithium carbonate prepared by different process conditions were analyzed by XRD,SEM and laser particle size analyzer. The results show that the uniform spherical lithium carbonate with an average particle size of ca. 178 nm and yield of 90. 01% can be continuously synthesized via the microreaction method. The optimum experimental conditions in microreactor are as follows:reactant concentration C_(Sodium carbonate)= 6 mol/L,C_(Lithium chloride)= 3 mol/L,C_(Sodium carbonate):C_(Lithium chloride)= 2:1,feed flow rate F = 40 mL/min,reaction temperature T = 20 ℃. Compared with the traditional liquid phase precipitation method,the process of synthesizing lithium carbonate via the microreaction method is continuous with higher yield,and the lithium carbonate has smaller particle size and more homogeneous.
引文
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[3] Chen Y,Tian Q,Chen B,et al. Preparation of Lithium Carbonate from Spodumene by A Sodium Carbonate Autoclave Process[J].Hydrometallurgy,2011,109(1):43-46.
[4]魏昊,田欢,张梦龙,等.电池级碳酸锂制备与提纯的研究进展[J].现代化工,2018,38(8):33-37.
[5]赵春龙,孙峙,郑晓洪,等.碳酸锂的制备及其纯化过程的研究进展[J].过程工程学报,2018,18(1):20-28.
[6]潘喜娟,张廷安,豆志河,等.浓度差对电解直接制备碳酸锂过程的影响[J].东北大学学报(自然科学版),2019,40(2):224-227+233.
[7]郭贤慧,王永勤,王建萍,等.碳化分解法制备电池级碳酸锂的工艺研究[J].无机盐工业,2019,51(1):50-52.
[8]尹记帅,孙文亮,郝如斯,等.沉锂反应条件对碳酸锂纯度及杂质影响的研究[J].无机盐工业,2019,51(3):29-33.
[9]段绍君,宋兴福,孙玉柱,等.超重力技术制备分散性碳酸锂超细粉体[J].化学工程,2019,47(1):10-14.
[10]张志强,张彩绵,周鑫,等.利用粗碳酸锂与电石渣制备氢氧化锂的研究[J].化学世界,2014,55(9):541-543.
[11]孙哲.盐湖卤水制备工业级及电池级碳酸锂工艺探讨[J].新疆有色金属,2016,39(6):87+90.
[12] Gao W,Zhang X,Zheng X,et al. Lithium Carbonate Recovery from Cathode Scrap of Spent Lithium-ion Battery———A Closed-loop Process[J].Environmental Science&Technology,2017,51(3):1662-1669.
[13]冯怡利,付希禄,刘尧.锂云母制备碳酸锂工艺的研究[J].中国陶瓷工业,2018,25(3):16-19.
[14]段绍君,孙玉柱,宋兴福.盐湖老卤反应结晶制备碳酸锂的研究[J].山东化工,2018,47(3):5-8+13.
[15]曹伟,孙淑英,宋兴福,等.含锂脱附液制备碳酸锂[J].过程工程学报,2016,16(3):424-430.
[16] Liu Y,Jiang X. Why Microfluidics? Merits and Trends in Chemical Synthesis[J]. Lab on a Chip,2017,17(23):3960-3978.
[17]曹寅,杨晖.微反应器制备无机材料的应用进展[J].无机盐工业,2011,43(5):7-10.
[18] Marre S,Jensen K F. Synthesis of Micro and Nanostructures in Microfluidic Systems[J]. Chemical Society Reviews,2010,39(3):1183-1202.
[19]陈光文,袁权.微化工技术[J].化工学报,2003,54(4):427-439.
[20]骆广生,陈桂光,徐建鸿,等.微混合技术——颗粒材料制备的关键之一[J].现代化工,2004,24(7):17-19.
[21] Wang Y,Zhang C,Bi S,et al. Preparation of ZnO Nanoparticles Using the Direct Precipitation Method in A Membrane Dispersion Microstructured Reactor[J]. Powder Technology,2010,202(1):130-136.