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硅酸盐通报 ›› 2022, Vol. 41 ›› Issue (8): 2954-2962.

• 新型功能材料 • 上一篇    

KBaB5O9的两步法制备及其过程动力学研究

全志林1, 李志祥1, 焦斌1, 周贤委1, 向德兴1, 冯晓琴1,2, 黄宏升1,2   

  1. 1.贵州理工学院化学工程学院,贵阳 550003;
    2.贵州省普通高等学校能源化学特色重点实验室,贵阳 550003
  • 收稿日期:2022-04-18 修回日期:2022-06-03 出版日期:2022-08-15 发布日期:2022-08-30
  • 通讯作者: 黄宏升,博士,教授。E-mail:36959784@qq.com
  • 作者简介:全志林(2001—),男。主要从事无机功能材料研究。E-mail:3021394279@qq.com
  • 基金资助:
    国家自然科学基金(21963006);贵州理工学院高层次人才科研启动项目(XJGC2019614);国家级大学生创新创业训练项目(202114440030)

Preparation of KBaB5O9 by Two-Step Method and Its Process Kinetics

QUAN Zhilin1, LI Zhixiang1, JIAO Bin1, ZHOU Xianwei1, XIANG Dexing1, FENG Xiaoqin1,2, HUANG Hongsheng1,2   

  1. 1. School of Chemical Engineering, Guizhou Institute of Technology, Guiyang 550003, China;
    2. Key Laboratory of Energy Chemistry for General Higher Education in Guizhou Province, Guiyang 550003, China
  • Received:2022-04-18 Revised:2022-06-03 Online:2022-08-15 Published:2022-08-30

摘要: 本文利用溶液法制备了K2Ba[B4O5(OH)4]2·8H2O,并将其进行热处理制备得到了KBaB5O9,利用XRD、FT-IR、TG-DTA-DTG对样品进行了表征。分析研究了由K2Ba[B4O5(OH)4]2·8H2O热处理制备KBaB5O9过程中的物相变化过程,其物相变化经历脱结晶水、脱羟基、重结晶、再分解、熔融再结晶5个阶段,其中结晶水的脱失分两步进行。运用Kissinger法、Flynn-Wall-Ozawa法、Šatava-Šesták法对K2Ba[B4O5(OH)4]2·8H2O结晶水第二步脱失过程的动力学参数进行了计算,可知K2Ba[B4O5(OH)4]2·8H2O结晶水第二步脱失过程的活化能Es为151.94 kJ/mol,指前因子的对数值lg As为21.25 min-1,机理函数G(α)=(1-2α/3)-(1-α)2/3(其中α为转化率)。

关键词: 多金属硼酸盐, 硼酸钾钡, 湿化学法, 热分解, 动力学, 活化能

Abstract: In this paper, K2Ba[B4O5(OH)4]2·8H2O was prepared by solution method, and KBaB5O9 was prepared by heat treatment of K2Ba[B4O5(OH)4]2·8H2O. The samples were characterized by XRD, FT-IR, and TG-DTA-DTG. The phase change process in the preparation of KBaB5O9 by heat treatment of K2Ba[B4O5(OH)4]2·8H2O was analyzed and studied. The phase change experiences five stages: the loss of crystal water, the loss of hydroxyl, recrystallization, redecomposition, and recrystallization after melting. The loss of crystal water is divided into two steps. The kinetic parameters of the second step loss process of crystal water in K2Ba[B4O5(OH)4]2·8H2O were calculated by Kissinger method, Flynn-Wall-Ozawa method, and Šatava-Šesták method. The activation energy Es of the second-step loss process of crystal water in K2Ba[B4O5(OH)4]2·8H2O is 151.94 kJ/mol, the logarithm of pre-exponential factor lg As is 21.25 min-1, and the mechanism function is G(α)=(1-2α/3)-(1-α)2/3 (α is conversion rate).

Key words: polymetallic borate, potassium borate barium, wet chemical method, thermal decomposition, kinetics, activation energy

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