Shin Chang-Hoon, Kim Ju-Yup, Kim Jun-Young, Kim Hyun-Sang, Lee Hyang-Sook, Mohapatra Debasish, Ahn Jae-Woo, Ahn Jong-Gwan, Bae Wookeun
R&D Center, Daeil Development Co., Ltd., Ansan 425-836, Republic of Korea.
J Hazard Mater. 2009 Mar 15;162(2-3):1278-84. doi: 10.1016/j.jhazmat.2008.06.029. Epub 2008 Jun 18.
Recovery of acetic acid (HAc) from the waste etching solution discharged from silicon wafer manufacturing process has been attempted by using solvent extraction process. For this purpose 2-ethylhexyl alcohol (EHA) was used as organic solvent. In the pre-treatment stage >99% silicon and hydrofluoric acid was removed from the solution by precipitation. The synthesized product, Na(2)SiF(6) having 98.2% purity was considered of commercial grade having good market value. The waste solution containing 279 g/L acetic acid, 513 g/L nitric acid, 0.9 g/L hydrofluoric acid and 0.030 g/L silicon was used for solvent extraction study. From the batch test results equilibrium conditions for HAc recovery were optimized and found to be 4 stages of extraction at an organic:aqueous (O:A) ratio of 3, 4 stages of scrubbing and 4 stages of stripping at an O:A ratio of 1. Deionized water (DW) was used as stripping agent to elute HAc from organic phase. In the whole batch process 96.3% acetic acid recovery was achieved. Continuous operations were successfully conducted for 100 h using a mixer-settler to examine the feasibility of the extraction system for its possible commercial application. Finally, a complete process flowsheet with material balance for the separation and recovery of HAc has been proposed.
已尝试采用溶剂萃取法从硅片制造过程中排放的废蚀刻液中回收乙酸(HAc)。为此,使用2-乙基己醇(EHA)作为有机溶剂。在预处理阶段,通过沉淀从溶液中去除了>99%的硅和氢氟酸。合成产物Na₂SiF₆的纯度为98.2%,被认为是具有良好市场价值的商业级产品。含有279 g/L乙酸、513 g/L硝酸、0.9 g/L氢氟酸和0.030 g/L硅的废液用于溶剂萃取研究。根据间歇试验结果,优化了HAc回收的平衡条件,发现萃取4级,有机相:水相(O:A)比为3,洗涤4级,反萃取4级,O:A比为1。使用去离子水(DW)作为反萃取剂从有机相中洗脱HAc。在整个间歇过程中,乙酸回收率达到了96.3%。使用混合澄清器成功进行了100小时的连续操作,以检验该萃取系统用于可能的商业应用的可行性。最后,提出了一个完整的工艺流程和HAc分离回收的物料平衡。