五水合六硼酸钙的水热合成及其高温相变研究  

Study on hydrothermal synthesis of CaB6O10·5H2O and its phase transition at high tempareture

作　　者：施春辉[1] 吕品[1] 黄霞[2] 仲剑初[2] Shi Chunhui;Lü Pin;Huang Xia;Zhong Jianchu(Liaoning Provincial Industrial Special Resources Protection Office,Shenyang 110032,China;State Key Laboratory of Fine Chemical,Department of Materials Science and Chemical Engineering,College of Chemical Engineering,Dalian University of Technology)

机构地区：[1]辽宁省人民政府工业特种资源保护办公室,辽宁沈阳110032 [2]大连理工大学精细化工国家重点实验室,化工学院材料化工系

出　　处：《无机盐工业》2019年第7期48-50,73,共4页Inorganic Chemicals Industry

摘　　要：在120℃的条件下,利用硼酸和石灰进行水热反应制备五水合六硼酸钙(CaB6O10·5H2O)。五水合六硼酸钙的差热分析结果显示,其脱水分4步,在800℃和900℃附近分别有一个相变放热峰和吸热峰。对五水合六硼酸钙的高温相变行为进行了探讨,化学分析、XRD、TG-DTA和IR分析结果表明:在600℃时,首先发生晶态的五水合六硼酸钙向非晶态的无水六硼酸钙(CaB6O10)转化,至800℃时无定型的无水六硼酸钙转变为晶态的无水六硼酸钙,进一步升温至900℃时无水六硼酸钙分解为晶态的四硼酸钙(CaB4O7)和玻璃态的三氧化二硼。CaB6O10·5H2O was synthesized by hydrothermal method at 120 ℃ with using boric acid and lime as materials.The thermal analysis of CaB6O10·5H2O showed that CaB6O10·5H2O was dehydrated by 4 steps,one exothermic peak near 800 ℃ and one endothermic peak near 900 ℃ were found,respectively.The high temperature phase transition behavior of CaB6O10·5H2O was discussed by chemical analysis,XRD,TG-DTA and IR analysis.The results indicated that:the first crystalline CaB6O10·5H2O was converted to amorphous CaB6O10 at 600 ℃,and the amorphous CaB6O10 was converted to crystalline CaB6O10 at 800 ℃,and finally CaB4O7 and vitreous B2O3 were obtained by the decomposition of crystalline CaB6O10 at 900 ℃.

关 键 词：五水合六硼酸钙 高温相变 CaB6O10 CaB4O7 

分 类 号：TQ132.32[化学工程—无机化工]