反应结晶制备硼氢化钾  

Preparation of Potassium Borohydride by Reactive Crystallization

作　　者：王泽临 王日杰[1] 杨晓霞[1] Wang Zelin;Wang Rijie;Yang Xiaoxia(School of Chemical Engineering and Technology ,Tianjin University ,Tianjin 300072, Chin)

机构地区：[1]天津大学化工学院,天津300072

出　　处：《化学工业与工程》2018年第4期52-57,共6页Chemical Industry and Engineering

摘　　要：针对Schlesinger法生产碱金属硼氢化物工艺存在的结晶母液循环成本较高和副产物累积导致产品质量降低等问题,设计开发了反应结晶制备硼氢化钾这一过程,用于处理生产过程中的结晶母液,以提高硼氢化物收率,同时生产出具备一定经济效益的硼氢化钾。采用了容量分析中的碘量法、光学显微镜分析技术和马尔文粒度分析仪、X射线粉末衍射仪等设备,考察了反应结晶过程各项因素对最终产品性质的影响。结果表明:控制反应物质的量之比为1.05~1.10,反应温度为50℃,降温速度10℃·h-1,养晶温度0℃,可以得到符合行业标准的硼氢化钾产品。As for the existing problems for the production of alkali metal borohydride via Schlesinger method,to illustrate,high costs for the cycle of mother liquor,lower quality for product caused by the accumulation of by-products,preparation of potassium borohydride by reactive crystallization was established to dispose of the crystallization mother liquor from the production and increase the yield for alkali metal borohydride while maintaining moderate economic benefits. Iodometric method from volumetric analysis,optical microscopy,Malvern Mastersizer 3000 and X-ray diffraction were employed to test the influence of various operating conditions on the product. The result shows that controlling the molar ratio between1. 05 and 1. 10,reaction temperature 50 ℃,cooling rate 10 ℃·h-1,keeping temperature 0 ℃,can ensure the product meet the standards of the chemical industry.

关 键 词：硼氢化钠 硼氢化钾 反应结晶 冷却结晶 

分 类 号：TQ128.2[化学工程—无机化工]