湿法磷酸副产氟硅酸钙制备纳米硫酸钙实验研究  

Preparation of nano calcium sulfate from by-product calcium fluosilicate in wet-process phosphoric acid production

作　　者：隋岩峰 石劲鹏 杨帆 李会勇 SUI Yanfeng;SHI Jinpeng;YANG Fan;LI Huiyong(State Key Laboratory of Efficient Utilization of Medium and Low Grade Phosphate Rock and Its Associated Resources,Guiyang 550002,China;Wengfu Institute of Technology,Guiyang 550014,China)

机构地区：[1]中低品位磷矿及其共伴生资源高效利用国家重点实验室,贵州贵阳550002 [2]瓮福技术研究院,贵州贵阳550014

出　　处：《生态产业科学与磷氟工程》2025年第1期14-18,共5页Eco-industry Science & Phosphorus Fluorine Engineering

基　　金：中低品位磷矿及其共伴生资源高效利用国家重点实验室开放课题“磷矿伴生资源氟、镁、钙多元素协同回收关键技术研究”(WFKF(2023)003);贵州省科技计划项目(黔科合中引地[2023]004)。

摘　　要：以湿法磷酸副产氟硅酸钙和硫酸为原料,以十二烷基苯磺酸钠和乙二醇为表面活性剂制备纳米硫酸钙,反应生成的气体去生产无水氟化氢和四氟化硅产品。考察反应温度、反应时间、硫酸用量、乙二醇用量以及煅烧温度对纳米硫酸钙收率的影响。实验结果表明,制备纳米硫酸钙最佳工艺条件如下:反应温度为90℃,反应时间为90 min,硫酸与氟硅酸钙摩尔比为1.03,十二烷基苯磺酸钠、乙二醇与氟硅酸钙的质量比分别为0.01、0.02,煅烧温度为600℃。最佳工艺条件下可制得粒径90 nm、纯度99.0%~99.5%的纳米硫酸钙产品,回收氟资源的同时,有效解决了硫酸钙污染、堆放问题。Nano calcium sulfate is prepared using by-product calcium fluorosilicate in wet-process phosphoric acid production and sulfuric acid as raw materials,sodium dodecyl benzenesulfonate and glycol as surfactants.The gas produced by the reaction is used to produce anhydrous hydrogen fluoride and silicon tetrafluoride products.The effects of reaction temperature,reaction time,amount of sulfuric acid,amount of glycol and calcining temperature on yield of nano calcium sulfate products are investigated.The results show that the optimal reaction conditions are as follows:Reaction temperature is 90℃,reaction time is 90 min,the mole ratio of sulfuric acid and calcium fluorosilicate is 1.03,the mass ratio of sodium dodecyl benzenesulfonate and glycol to calcium fluorosilicate are 0.01 and 0.02 respectively,and the calcination temperature is 600℃.Under the optimal process conditions,nano calcium sulfate products with particle size of 90 nm and purity of 99.0% to 99.5% can be produced,effectively solving the problems of calcium sulfate pollution and stacking while recovering fluorine resources.

关 键 词：湿法磷酸 氟硅酸钙 纳米硫酸钙 制备 

分 类 号：TQ132.32[化学工程—无机化工] TB383[一般工业技术—材料科学与工程]