A solvent extraction approach to recover acetic acid from mixed waste acids produced during semiconductor wafer process.

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.

Chemical extraction of arsenic from contaminated soil under subcritical conditions.

In this research, we investigated a chemical extraction process, under subcritical conditions, for arsenic (As)-contaminated soil in the vicinity of an abandoned smelting plant in South Korea. The total concentration of As in soil was 75.5 mg/kg, 68% of which was As(+III). X-ray photoelectron spectroscopy analysis showed that the possible As(+III)-bearing compounds in the soil were As(2)O(3) and R-AsOOH. At 20°C, 100 mM of NaOH could extract 26% of the As from the soil samples. In contrast, 100 mM of ethylenediaminetetraacetic acid (EDTA) and citric acid showed less than 10% extraction efficiency. However, as the temperature increased to 250 and 300°C, extraction efficiencies increased to 75-91% and 94-103%, respectively, regardless of the extraction reagent used. Control experiments with subcritical water at 300°C showed complete extraction of As from the soil. Arsenic species in the solution extracted at 300°C indicated that subcritical water oxidation may be involved in the dissolution of As(+III)-bearing minerals under given conditions. Our results suggest that subcritical water extraction/oxidation is a promising option for effective disposal of As-contaminated soil.

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

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%.