无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2014, Vol. 46 ›› Issue (6): 38-.

• 论文 • 上一篇    下一篇

降膜结晶法在高纯硫酸制备中的应用

朱 静1,丁雪峰1,李天祥1,2,刘 飞2   

  1. 1.贵州大学化学与化工学院,贵州贵阳550003;2.瓮福(集团)有限责任公司技术开发中心
  • 发布日期:2014-06-09

Application of falling film crystallization process in preparation of high-purity sulfuric acid

Zhu Jing1,Ding Xuefeng1,Li Tianxiang1,2,Liu Fei2   

  1. 1.School of Chemistry and Chemical Engineering,Guizhou University,Guiyang 550003,China;
    2.Technology Research & Development Center,Wengfu (Group) Co.,Ltd.
  • Published:2014-06-09

摘要: 现行高纯硫酸生产工艺复杂、能耗大且成本高。降膜结晶法具有绿色环保、节能和工艺简单的优势。采用减压蒸馏、降膜结晶工艺对工业硫酸进行净化提纯,可以制备出达到BV-Ⅲ级的高纯硫酸。最佳工艺条件:1)通过减压蒸馏将工业硫酸中的大部分杂质除去;2)通过降膜结晶获得粗晶体,结晶条件为初始结晶温度-5 ℃、降温步长每10 min降温0.6 ℃、结晶时间80 min、料液流量20 mL/min;3)对粗晶体进行发汗提纯,发汗条件为发汗终温 6 ℃、升温速度3 ℃/h、升温方式每10 min升温0.5 ℃。该工艺在高纯硫酸的制备方面有着广阔的应用前景。

关键词: 减压蒸馏, 降膜结晶, 高纯硫酸

Abstract: The existing production processes of highly pure sulfuric acid are complicated,high energy wasting,and high cost. Falling film crystallization process has advantages of environmentally friendly,energy-saving,and simple flow.Vacuum distillation and repeated falling film crystallization processes were applied to purify industrial sulfuric acid,and then the highly pure sulfuric acid reaching BV-Ⅲ level was achieved.The optimal process conditions were acquired:1) most of the impurities in industrial sulfuric acid were moved off by vacuum distillation;2) to obtain coarse crystals by falling film crystallization, crystallization conditions were the initial crystallization temperature of -5 ℃,the cooling step of 0.6 ℃ per 10 min,crystallization time of 80 min,and feed flow rate of 20 mL/min;3) to purify the crude crystals,sweating conditions were the final sweating temperature of 6 ℃,the heating rate of 3 ℃/h,and heating temperature of 0.5 ℃ per 10 min.Therefore,falling film crystallization process  has a wide application prospect to produce high purity sulfuric acid.

Key words: vacuum distillation, falling film crystallization, highly pure sulfuric acid

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