水相法制备双乙二酸硼酸锂的中试工艺研究  

The study of double oxalate lithium borate preparation technology by aqueous phase method

作　　者：刘艳蕊[1] 宋从从[1] 石桂珍[1] 王坤 Liu Yanrui;Song Congcong;Shi Guizhen;Wang Kun(Collegel of Applied Chemistry and Food and Drug,Weifang Engineering College,Weifang 262500,China;CenerTech Tianjin Chemical Research and Design Institute Co.,Ltd.)

机构地区：[1]潍坊工程职业学院应用化学与食品药品学院,山东潍坊262500 [2]中海油天津化工研究设计院有限公司

出　　处：《无机盐工业》2020年第10期100-105,共6页Inorganic Chemicals Industry

基　　金：潍坊工程职业学院2019年度科研课题资助项目。

摘　　要：以水相法制备双乙二酸硼酸锂(LiBOB)。研究了中试条件下的反应物料比、反应温度、反应时间、析晶溶剂加入量对产品质量的影响,所得产品利用FTIR、TG-DSC和XRD进行了确认,目前中试装置已实现10 t/a的生产规模。实验结果表明,较优工艺条件为:物料比(草酸、硼酸、碳酸锂的物质的量比)为4∶2∶1.1,反应温度为80℃,反应时间为8 h,在浓缩析晶过程中浓缩比(蒸发溶剂占总溶剂的质量比)为80%左右,析晶剂加入量为产品质量的4倍。干燥采用动态干燥方式,干燥时间为8 h。经过分析,该工艺制备的产品质量超过市售产品水平。The double oxalate lithium borate(LiBOB)was prepared by aqueous-phase method.The effect of material ratio,reaction temperature,reaction time and amount of crystallization solvent on the product quality under the condition of pilot test was studied.The result of products was confirmed by FTIR,TG-DSC and XRD.The pilot plant had achieved a production scale of 10 t/a at present.The experimental results showed the optimum operating parameters which were material ratio(the amount-of-substance ratio of oxalic acid to lithium carbonate to boric acid)of 4∶2∶1.1,reaction temperature of 80℃,reaction time of 8 h,the concentration amount(the mass ratio of residual solvent to total solvent mass)of about 80%in the process of concentration and crystallization,and the addition amount of crystallization agent of 4 times of the product mass.The dynamic drying was adopted for 8 h.After analysis,the quality of the product prepared by this process exceeded the level of the market products.

关 键 词：双乙二酸硼酸锂 水相法 析晶剂 

分 类 号：TQ131.11[化学工程—无机化工]