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采用溶剂萃取法从废蚀刻液中回收硝酸。

Recovery of nitric acid from waste etching solution using solvent extraction.

作者信息

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

机构信息

R&D Center, Daeil Development Co., Ltd., Ansan 425-836, Republic of Korea.

出版信息

J Hazard Mater. 2009 Apr 30;163(2-3):729-34. doi: 10.1016/j.jhazmat.2008.07.019. Epub 2008 Jul 12.

Abstract

A process was developed to recover nitric acid from the waste stream of wafer industry using solvent extraction technique. Tributyl phosphate (TBP) was selected among several extractants because of its better selectivity towards HNO(3), overall superiority in operation, favorable physical properties and economics. The waste solution containing 260 g/L CH(3)COOH, 460 g/L HNO(3), 113 g/L HF and 19.6g/L Si was used as feed solution for process optimization. In the pre-treatment stage >99% silicon and hydrofluoric acid was precipitated out as Na(2)SiF(6). Equilibrium conditions for HNO(3) recovery were optimized from the batch test results as: four stages of extraction at an organic:aqueous (O:A) ratio of 3, four stages of scrubbing at O:A ratio of 5 and five stages of stripping at an O:A ratio of 1.5. The extraction of HNO(3) was suppressed by the presence of acetic acid (HAc) in the feed solution. To examine the feasibility of the extraction system a continuous operation was carried out for 200 h using a multistage mixer-settler. The concentration of pure HNO(3) recovered was 235 g/L with a purity of 99.8%.

摘要

开发了一种利用溶剂萃取技术从晶圆行业废物流中回收硝酸的工艺。在几种萃取剂中选择了磷酸三丁酯(TBP),因为它对HNO₃具有更好的选择性,在操作上具有总体优势,物理性质良好且经济可行。含有260 g/L CH₃COOH、460 g/L HNO₃、113 g/L HF和19.6 g/L Si的废液用作工艺优化的进料溶液。在预处理阶段,>99%的硅和氢氟酸以Na₂SiF₆的形式沉淀出来。根据间歇试验结果,优化了HNO₃回收的平衡条件为:在有机相:水相(O:A)比为3的条件下进行四级萃取,在O:A比为5的条件下进行四级洗涤,在O:A比为1.5的条件下进行五级反萃。进料溶液中乙酸(HAc)的存在抑制了HNO₃的萃取。为了检验萃取系统的可行性,使用多级混合澄清器进行了200小时的连续操作。回收的纯HNO₃浓度为235 g/L,纯度为99.8%。

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