液相氧化-喷雾干燥法制备高纯超细二氧化锡颗粒

Preparation of high purity ultrafine tin dioxide particles by liquid oxidation⁃spray drying method

为了减少反应中氮氧化物(NO_(x))排放对环境造成的影响,提高二氧化锡产品纯度、减小粒径,以金属锡粒和稀硝酸为原料,采用液相硝酸氧化法与喷雾干燥工艺结合制备高纯超细二氧化锡颗粒。考察锡源类型、硝酸浓度及滴加速度、反应温度及煅烧温度等参数对产物的影响,并利用X射线衍射仪、电感耦合等离子体发射光谱仪、扫描电子显微镜、激光粒度仪、比表面积分析仪等对所制备的偏锡酸(H_(2)SnO_(3))和二氧化锡进行结构和性能表征。结果表明:以锡粒为锡源、硝酸质量分数为25%、滴加速度为30 m L/min、反应温度为80℃,经喷雾干燥工艺处理,再经950℃煅烧,最终制得纯度为99.997%、D_(50)为1.15μm、D_(90)为2.44μm、比表面积为3.86 m^(2)/g的二氧化锡,该产品在屏幕显示技术领域有重要应用,可用于制备氧化铟锡粉体材料(ITO)。

To reduce the impact of nitrogen oxides(NO_(x))emissions on the environment in the reaction,improve the purity of tin dioxide(SnO_(2)) products,and reduce the particle size,the metal tin particles and dilute nitric acid were used as raw materials,and the liquid phase nitric acid oxidation method and spray drying in combination with the process were used.To pre⁃pare high⁃purity ultra⁃fine SnO_(2) particles.The influence of parameters such as tin source type,nitric acid concentration and dropping rate reaction temperature and calcination temperature on the product were investigated.The structure and proper⁃ties of the prepared metastannic acid(H_(2)SnO_(3)) and SnO_(2) were characterized by X-ray diffractometer inductively coupled plas⁃ma emission spectrometer scanning electron microscope laser particle size analyzer and specific surface area analyzer.The results showed that using tin particles as the tin source,nitric acid mass concentration of 25%,adding speed of 30 mL/min,reaction temperature of 80℃,after spray drying process,and then 950℃calcination,the final purity of SnO_(2) was 99.997%,D_(50) was 1.15μm,D_(90) was 2.44μm,with a specific surface area of 3.86 m^(2)/g.This products had important applications in the field of screen display technology and could be used to prepare indium tin oxide powder materials(ITO).