柠檬酸铵对水热合成α-CaSO4·0.5H2O结晶过程的影响  

Effects of ammonium citrate on crystallization ofα-CaSO4·0.5H2O in hydrothermal synthesis processes

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作  者:孙祥斌 张楠 窦焰 方羊 郑之银[2] 刘荣[2] 崔鹏 SUN Xiang-bin;ZHANG Nan;DOU Yan;FANG Yang;ZHENG Zhi-yin;LIU Rong;CUI Peng(School of Chemistry and Chemical Engineering,Hefei University of Technology,Hefei 230009,China;Anhui Liuguo Limited Liability Company,Tongling 244000,China)

机构地区:[1]合肥工业大学化学与化工学院,安徽合肥230009 [2]安徽六国化工股份有限公司,安徽铜陵244000

出  处:《高校化学工程学报》2019年第1期96-102,共7页Journal of Chemical Engineering of Chinese Universities

基  金:安徽省创新环境建设专项资助项目(1606a1003040)。

摘  要:以CaSO4·2H2O为原料,柠檬酸铵(C6H17N3O7)为添加剂,在水热温度130℃,搅拌速率60r·min^-1,反应2h的条件下制备α-CaSO4·0.5H2O。采用X射线衍射仪(XRD)、场发射扫描电子显微镜(SEM)、场发射透射电子显微镜(TEM)、热重分析仪(TG)、差热示差扫描量热仪(DSC)、傅里叶红外光谱仪(FT-IR)和X射线光电子能谱测定元素结合能(XPS)表征α-CaSO4·0.5H2O晶体的形貌和结构,探讨不同浓度C6H17N3O7对α-CaSO4·0.5H2O的晶体和结晶过程的影响。研究结果表明,C6H17N3O7会抑制α-CaSO4·0.5H2O沿c轴的生长,随着添加C6H17N3O7浓度的增大,α-CaSO4·0.5H2O的形貌由针状向柱状转变,晶体的直径由1.5~2μm增至10~12μm,长径比由80:1~100:1降至2:1~3:1。并且在CaSO4·2H2O向α-CaSO4·0.5H2O转化过程中,C6H17N3O7的添加导致其诱导时间和转化周期延长,生长速率减慢,晶体的热稳定性提高。α-CaSO4·0.5H2O was prepared using CaSO4·2H2O as a raw material and ammonium citrate(C6H17N3O7)as an additive under conditions of hydrothermal temperature 130℃,stirring rate 60 r·min^-1 and reaction time 2 h.The morphology and structure ofα-CaSO4·0.5H2O crystals were characterized by XRD,SEM,TEM,TG,DSC,FT-IR and XPS.Effects of C6H17N3O7 concentrations on crystallization ofα-CaSO4·0.5H2O were discussed.The results show that C6H17N3O7 inhibitsα-CaSO4·0.5H2O growth along the c-axis.With the increase of C6H17N3O7 concentration,the morphology ofα-CaSO4·0.5H2O changes from acicular to columnar,the diameter of crystal increases from 1.5~2μm to 10~12μm and its aspect ratio reduces from 80:1~100:1 to 2:1~3:1.C6H17N3O7 prolongs induction time and phase transformation period,slows down growth rate and improves thermal stability of the crystal during CaSO4·2H2O toα-CaSO4·0.5H2O conversion.

关 键 词:柠檬酸铵 晶型控制剂 半水硫酸钙 结晶 

分 类 号:O781[理学—晶体学]

 

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