乙酸异戊酯共沸干燥法制备低团聚掺锑氧化锡纳米微粉

以SnCl4·5H2O和SbCl3乙醇溶液为原料,用阴离子树脂交换除氯水解法制备得到无氯离子的前驱体掺锑氢氧化锡胶体沉淀。首次对以含氧官能团为主的系列憎水有机溶剂进行了共沸干燥脱水研究,并对所得粉体团聚程度进行比较。实验发现掺锑氧化锡共沸脱水干燥效果与有机溶剂分子结构之间有密切关系,提出了选择共沸有机溶剂的3个原则,在一系列有机溶剂中选择了最符合的乙酸异戊酯进行干燥实验,与常用的正丁醇共沸溶剂进行了消除粉体团聚效果的比较。运用IR、BET、TEM、XRD等方法对掺锑氢氧化锡粉体的结构、比表面积、形貌、物相进行表征。结果表明,乙酸异戊酯溶剂是理想的共沸干燥有机溶剂,其干燥所得掺锑氢氧化锡蓬松粉体的比表面积为284.44m2/g,比用正丁醇处理的增大了22%。将乙酸异戊酯干燥所得的掺锑氢氧化锡微粉经热处理后得到了低团聚的掺锑氧化锡纳米微粉。

Preparation of Antimony-doped Tin Oxide Nano-powder with Low Agglomeration by Novel Azeotropic Drying of Iso-amyl Acetate

Sb-doped tin hydroxide colloid precipitates were synthesized with a method of anion exchange resin hydrolysis by removing chlorine , using SnCl4·5H2O and SbCl3 ethanol solution as raw materials. A series of solvents with groups containing oxygen in azeotropic distillation experiments were investigated and compared in eliminating agglomeration for the first time. It was found that the results of drying of Sb-doped tin hydroxide was closely associated with the structures of solvents and presenting three basic principles. The iso-amyl acetate was selected from a number of organic solvents following the three principles and compared with most used n-butanol solvent to treat the precipitate for preparing nonagglomerated precursor powder. The IR, BET, TEM, XRD were carried out on the dried powders of Sb-doped tin hydroxide. The results demonstrated that iso-amyl acetate is a very excellent azeotropic solvent which greatly improved the fluffy of the ob tained dried powder. The BET surface area of the dried powders, obtained with iso-amyl acetate ,was 284.44 m2/g,which increased 22% as large as that of ground dried powder treated with n-butanol. After sintering Sb-doped tin hydroxide powder dried with iso-amyl acetate, the low agglomeration antimony doped tin oxide nano-powder were obtained.