摘要
在低温条件下,硫代硫酸钠与固体碘反应,经重结晶制得高纯二水合连四硫酸钠,并用XRD和IR对其结构进行了表征。结果表明,最佳制备条件为:氧化剂碘要比计量比稍过量一点,反应温度在10℃以下,至少需要重结晶1次;XRD图表明,该工艺制备的产品XRD图与标准图谱基本一致;IR图谱表明,连四硫酸钠中所含杂质硫代硫酸盐对红外图谱有较大的影响,硫代硫酸盐含量越低,在1238~1090 cm^(-1)区间内的吸收峰越少,曲线越平滑。
The high purity of sodium tetrathionate dihydrate was prepared by the reaction between iodine and sodium thiosulphate at low temperature.It was recrystallized from a cool aqueous solution by the addition of ethanol.Its structure was characterized by XRD and IR.Based on the experiment results,the best preparation method is that the addition of oxidant iodine was slightly excessive than the stoichiometric ratio,the reaction temperature was below 10℃,and the recrystallization was required at least once.The XRD pattern showed that the XRD diagram of the products prepared by this process was basically consistent with the standard diagram of sodium tetrathionate dehydrate.The IR spectra showed that the impurity thiosulphate in the product had a great impact on the infrared spectra.The content of thiosulfate becomes lower along with the less absorption peak in the wave range of 1238~1090 cm^(-1),as well as the smoother the curve.
作者
刘红梅
谷芳芳
王保金
李炳华
杜荣光
陈勉彬
LIU Hong-mei;GU Fang-fang;WANG Bao-jin;LI Bing-hua;DU Rong-guang;CHEN Mian-bin(Guangzhou Chemical Reagent Factory,Guangzhou 510288,China;Guangdong Guangshi Reagent Technology Co.,Ltd,Zhaoqing 526238,China)
出处
《化学试剂》
CAS
北大核心
2023年第2期161-165,共5页
Chemical Reagents
关键词
连四硫酸钠
高纯度
制备
表征
sodium tetrathionate dihydrate
high purity
preparation
characterization
