化工进展2018，Vol.37Issue(1)：406-413,8.DOI:10.16085/j.issn.1000-6613.2017-0782
氯硅烷中痕量磷杂质的检测方法及应用
Determination method and application of trace amounts of phosphorus in chlorosilanes
摘要
Abstract
Phosphorus impurities in the chlorosilane mixture was difficult to be separated due to their similar boiling points. The adsorbents of 13X zeolite(13X) and 13X zeolite modified with CuCl2 (Cu-13X)compared with adsorbents of metal oxide were prepared to adsorb trace PCl3in this study. The Ultraviolet-visible spectroscopy(UV-vis)was used to determine the content of trace phosphorus in the chlorosilanes. The effects of the composition of the hydrolysate and the phase state of the raw materials on the determination of phosphorus impurity content with UV-vis were investigated based on the analysis of the contents of phosphorus in water and in the chlorosilanes. Besides, the breakthrough curves at 20℃were investigated to determine the performance of the adsorbents of 13X and Cu-13X. The results showed that the pre-treatment phase state of chlorosilanes samples with the high purity nitrogen used as carrier gas is gas phase when they were passed into the high-purity water and the determined mass fraction of phosphorus in chlorosilanes varied between 0.0003 and 0.03. The adsorption performance of Cu-13X was enhanced after modified with CuCl2. When the volume of the mixture solution increased to 120mL in the breakthrough experiment process,the removal efficiency of the complexation adsorbents for PCl3was still greater than about 80%,whereas the adsorption capacity of the 13X zeolite disappeared due to complete breakthrough when the volume of the mixture solution was 20mL.关键词
氯硅烷/三氯化磷/水解/共沸(混合)物/吸附/沸石Key words
chlorosilanes/phosphorus trichloride/hydrolysis/azeotrope/adsorption/zeolite分类
化学化工引用本文复制引用
刘帅峰,黄国强..氯硅烷中痕量磷杂质的检测方法及应用[J].化工进展,2018,37(1):406-413,8.基金项目
国家自然科学基金项目(21676197). （21676197）
