稀土石膏母液循环法制备硫酸钙晶须及其晶型转换和性能研究  

Preparation of calcium sulphate whiskers by recycling method of rare earth gypsum mother liquor and study of their crystal transformation and properties

作　　者：卢琪 皮雯静 吴锦绣[1,2,3] 张一鸣 柳召刚 胡艳宏[1,2,3] 张晓伟 李健飞[1,2,3] Lu Qi;Pi Wenjing;Wu Jinxiu;Zhang Yiming;Liu Zhaogang;Hu Yanhong;Zhang Xiaowei;Li Jianfei(College of Rare Earth Industry,Inner Mongolia University of Science and Technology,Baotou 014010;Key Laboratory of Green Extraction and Efficient Utilization of Light Rare Earth Resources,Ministry of Education,Inner Mongolia University of Science and Technology,Baotou 014010;Key Laboratory of Wet Metallurgy of Rare Earths and Application of Light Rare Earths,Inner Mongolia Autonomous Region,Baotou 014010)

机构地区：[1]内蒙古科技大学稀土产业学院(稀土工程技术学院),包头014010 [2]轻稀土资源绿色提取与高效利用教育部重点实验室,包头014010 [3]内蒙古自治区稀土湿法冶金与轻稀土应用重点实验室,包头014010

出　　处：《化工新型材料》2025年第1期278-285,共8页New Chemical Materials

基　　金：国家自然科学基金(51965053);内蒙古自然科学基金项目(2022LHMS05022);内蒙古自治区直属高校基本科研业务费(内财教规[2022]11号No.242和No.311);内蒙古自治区一流学科科研专项项目(YLXKZX-NKD-042)。

摘　　要：以稀土冶金过程产生的废渣(稀土石膏)为原料,采用微波法制备硫酸钙晶须,随后探讨母液循环对硫酸钙晶须制备及其晶型转化的影响,明确了硫酸钙晶须晶型转换条件,最后探究硫酸钙的性能。通过X射线衍射仪(XRD)、扫描电子显微镜(SEM)、热重-差热分析仪(TG)、傅里叶红外光谱仪(FT-IR)和原子力-拉曼光谱仪和荧光光谱仪(F-4600)等仪器对硫酸钙晶须的结构、形貌和性能进行表征和分析。结果表明:母液循环3次后,晶须的形貌和晶体结构稳定,平均长度为92.4μm,长径比为13.7,可见母液循环方案可行。循环后的产物通过调控干燥温度进行烘干,在80℃、90℃和420℃下分别制备出二水、半水和无水硫酸钙晶须,3种硫酸钙晶须均具有吸收紫外光和发射蓝光的性能,其中半水硫酸钙晶须的发光性能最好。固废与母液循环提高了废渣和废液处理过程中的资源利用效率,减少了对环境的不良影响。通过对硫酸钙晶须晶型的调控并赋予硫酸钙晶须发光特性,为探究硫酸钙晶须应用领域提供新方向,同时为稀土冶金的清洁化生产提供了新思路。In the article,calcium sulfate whiskers were prepared by microwave method using the waste slag(rare earth gypsum)generated from the rare earth metallurgical process as the raw material.Then the effect of mother liquor circulation on the preparation of calcium sulfate whiskers and their crystal transformation was explored.The crystal transformation conditions of calcium sulfate whiskers were clarified.Finally,the properties of calcium sulfate were investigated.The structure,morphology and properties of calcium sulfate whiskers were characterized and analyzed by X-ray diffractometer(XRD),scanning electron microscope(SEM),thermogravimetric-differential calorimetric analyzer(TG),Fourier-transform infrared spectrometry(FT-IR),and atomic force-Raman and fluorescence spectrometry(F-4600).The results showed that the morphology and crystal structure of the whiskers were stable with an average length of 92.4μm and an aspect ratio of 13.7 after three cycles of the mother liquor,indicating that the mother liquor recycling scheme was feasible.The recycled products were dried by regulating the drying temperature,and dihydrate,hemihydrate and anhydrous calcium sulfate whiskers were prepared at 80℃,90℃and 420℃,respectively.All three prepared calcium sulfate whiskers had the performance of absorbing UV light and emitting blue light,among which the hemihydrate calcium sulfate whiskers had the best luminescence performance.The recycling of solid waste and mother liquor improved the resource utilization efficiency in the process of waste residue and waste liquid treatment,and reduced the adverse impact on the environment.By regulating the crystal shape of calcium sulfate whiskers and endowing them with luminescent properties,new directions for exploring the application fields of calcium sulfate whiskers were provided,and at the same time,new ideas for the clean production of rare earth metallurgy were offered.

关 键 词：固废处理 硫酸钙晶须 微波法 母液循环 晶型调控 

分 类 号：TQ132.3[化学工程—无机化工]