Novel Process for the Treatment of Wastewaters from the Microelectronics Industry IWC 13-34

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1 Novel Process for the Treatment of Wastewaters from the Microelectronics Industry IWC Authors: Temple Ballard 1, Nabin Chowdhury 2, Bruno Heiniger 4, Denise Horner 2, Antonio Lau 1, Sunil Mehta 2, Barbara Schilling 3, Rich Ubaldi 1, John Williamson 2 Key Words: wastewater, treatment, microelectronics, biological, activated sludge, ozone, advanced oxidation process. Abstract Infilco Degremont, Inc. has developed an innovative process to treat wastewaters generated by the microelectronics industry. These highstrength wastewaters contain many organic and inorganic compounds, such as tetramethylammonium hydroxide ((CH 3 ) 4 NOH, TMAH), monoethylamine (C 2 H 5 ONH 2, MEA), dimethyl sulfoxide ((CH 3 ) 2 SO, DMSO), hydrofluoric acid (HF) and others. Based on fundamental biological and physical/chemical treatment principles, this novel process consists of three stages: (1) aerobic biodegradation (i.e., activated sludge) of the organics and organic nitrogen compounds into ammonia-nitrogen and carbon dioxide, (2) chemical oxidation of ammonia into nitrates via ozonation, and (3) post-anoxic biological denitrification of the nitrates into nitrogen gas. This process generates an effluent with >98% removal of the Total Organic Carbon (TOC), >99% degradation of TMAH into ammonia-nitrogen and carbon dioxide and >95% removal of the Total Nitrogen. (activated sludge and ozonation) and to generate design parameters for a full-scale treatment system. This patent-pending treatment system currently marketed as MICROGREEN and can be easily integrated into existing wastewater treatment units at semiconductor manufacturing facilities. This demonstrated technology provides a robust and cost-effective alternate technology to the microelectronics industry. 1 Infilco Degremont, Inc., 8007 Discovery Drive, Richmond, VA Degremont North America R&D Laboratory, Ashland, VA Ozonia North America, Leonia, NJ Degremont Technologies R&D Laboratory, Duebendorf, Switzerland This paper describes bench-scale and pilot studies that were conducted to validate this combined biological and physical/chemical treatment process

2 1. Introduction The semiconductor and electronic components manufacturing industry is one of the fastest growing industrial sectors in North America, Europe, Asia and Australia. The semiconductor industry in North America experienced a 61% annual growth in There are more than 250 fabrication units in the US, in addition to 400 units worldwide. The semiconductor industry spends approximately $1 billion per year for water and wastewater treatment systems and services (Reference 1). The semiconductor and electronic component manufacturing plants typically generate high-strength wastewaters containing tetramethylammonium hydroxide (TMAH, (CH 3 ) 4 NOH) and many other organic and inorganic compounds. TMAH is recognized as a poisonous, corrosive, slow to biodegrade and eutrophic to aquatic environments. The recently observed growth of the semiconductor industry and the stringent regulations imposed on industrial and municipal discharges require innovative solutions to treat these wastewaters. There are few technology options available in the market that provide a complete green sustainable solution for treatment of semiconductor wastewaters. For example, physicochemical treatment methods include catalytic oxidation and photocatalysis as well as ion-exchange resins for TMAH recovery. On the biological treatment area, there are reports that use a 2-stage anoxic-aerobic activated sludge process, anoxic-aerobicmembrane bioreactors (MBR), up-flow anaerobic sludge blanket reactors (UASB) and sequencing batch reactors (SBR). Few studies achieved high destruction of organic matter (i.e., >90% Chemical Oxygen Demand (COD) removal), however, nitrogen removal was limited to <70% Total Nitrogen (TN) (References 2 to 5). This paper discusses the results from pilot studies that were conducted using a high strength semiconductor wastewater to achieve a high removal rate of organic matter (i.e., >98% Total Organic Carbon (TOC) removal), a high degradation of TMAH (i.e., >98% conversion of TMAH) as well as a high removal of Total Nitrogen (i.e., >95% TN removal) from the wastewater. 2. Novel Semiconductor Wastewater Treatment Process The objectives of this study were to develop a sustainable and costeffective process to treat high strength wastewater from the semiconductor manufacturing process and achieve the following process performance targets: >98% conversion of the organic nitrogen compound TMAH >98% removal of organics (TOC) >95% removal of Total Nitrogen (TN) A combination of biological degradation and advanced oxidation processes was employed in the treatment of the semiconductor wastewater. The process described in this paper is illustrated in Figure 1 below.

3 Figure 1. MICROGREEN Wastewater Treatment Process The individual treatment processes have the following functions: An Aerobic Reactor is used to oxidize and convert the organic nitrogen compound TMAH into ammonia and carbon dioxide as well as biological oxidation of other organics into CO 2. A simplified reaction can be represented as follows: Organics + Microorganisms + O 2 -- CO 2 (gas) + H 2 O + Biomass TMAH + Microorganisms + O NH 3 + CO 2 (gas) + H 2 O + Biomass An Advanced Oxidation Process follows to convert the ammonia generated in the Aerobic Reactor into nitrates. A simplified reaction can be represented as follows: NH 3 + Organics + Ozone ---- NO 3 + CO 2 A Post- Anoxic Reactor is used to denitrify the nitrate into nitrogen gas. A simplified reaction can be represented as follows: NO 3 (nitrates) + Carbon Source + Microorganisms ---- N 2 (gas) + CO 2 + H 2 O + Alkalinity + Biomass

4 3. Methodology The semiconductor wastewater was obtained from a major chip manufacturing facility. Water quality parameters (alkalinity, COD, BOD, TOC, MLSS, MLVSS, NH 4 -N, NO 3 -N, TKN, PO 4 -P and Total P) were analyzed following Standard Methods for Water and Wastewater Analysis (Reference 6). Reactor ph, temperature, Dissolved Oxygen (DO) and Oxidation Reduction Potential (ORP) were monitored using a multimeter (HQ40d, HACH). TMAH analysis was outsourced to a commercial analytical laboratory. Table 1 below shows the characteristics of the wastewater used in this study. Table 1: Semiconductor Wastewater Characteristics Parameter Value ph >12 Conductivity (ms/cm) 75 TMAH (mg/l) 23,000 TOC (mg/l) 17,561 Total Nitrogen (mg/l) 4,675 COD (mg/l) No test method available The wastewater was initially diluted at 1:6 with deionized water. The essential micro/macro nutrients (metals, alkalinity and orthophosphate) were added for proper microbial metabolism. Influent ph was also adjusted to 7±0.1 using concentrated hydrochloric acid (HCl, 37%). The external carbon source used for the post-anoxic reactor was MicroC The biological reactors were inoculated with return activated sludge from Henrico municipal WWTP located in Richmond, VA. The AOP process consisted in the addition of ozone at a controlled ph>8. 4. Results and Discussion The wastewater stream was treated using an activated sludge process configured with aerobic and anoxic bioreactors, and an AOP system utilizing ozone. The AOP system was integrated within the treatment loop as shown in Figure 1. The purpose of the AOP system was to oxidize ammonia into nitrates using ozone at a controlled ph. The raw wastewater was initially diluted at 1:6 with deionized water to avoid chemical toxicity to the biological processes. Table 2 shows the Influent, Aerobic Reactor Effluent, AOP Effluent and the Final Effluent characteristics from this pilot study.

5 Table 2: Influent and Effluent Wastewater Characteristics Influent Aerobic Effluent AOP Effluent Anoxic Effluent Final Effluent Removal TOC (mg/l) 2, >98% NH 4 -N (mg/l) NO 3 -N (mg/l) <0.4 < <0.4 < NO 2 -N (mg/l) <0.5 <0.5 <0.5 <0.5 < TKN (mg/l) >95% TMAH (mg/l) 3,933 < >99% The organic matter was degraded in the Aerobic Reactor resulting in 98% removal of the TOC. As the organic nitrogen compounds were being biologically degraded to carbon dioxide and water, the nitrogen component was also being oxidized to ammonia-nitrogen as shown by the increase in NH 4 -N from 7 mg/l to 689 mg/l in the effluent of the Aerobic Reactor. The AOP treatment system used ozone at a controlled ph to oxidize most of the ammonia into nitrates as shown in the appearance of 613 mg/l NO 3 -N. This concentration of nitrates was subsequently biologically denitrified to <0.4 mg/l in the Anoxic Reactor. Even though the influent TMAH concentration was approximately 4,000 mg/l, no toxicity and/or inhibition of the biological treatment was observed over the experimental period. Figures 2 and 3 below show the Total Organic Carbon (TOC) and Total Nitrogen (TN) performance curves throughout the experiment.

6 Figure 2. Influent and Effluent Total Organic Carbon (TOC) Concentration Figure 3. Influent and Effluent Total Nitrogen (TN) Concentration Figures 4 and 5 show the conversion of ~ 500 mg/l of ammonia to nitrates as the wastewater was oxidized with an ozone dose of 5-6 g/l.

7 Figure 4. Conversion of Ammonia to Nitrate via Ozonation Figure 5. Nitrates Formation during Oxidation of Ammonia with Ozone

8 5. Conclusions An innovative patent-pending process consisting of aerobic biodegradation of TMAH followed by advanced oxidation treatment and biological denitrification provides a complete solution for semiconductor industry wastewaters to meet stringent regulatory requirements. This process can achieve the following performance requirements: >99% TMAH degradation >98% Total Organic Carbon (TOC) removal >95% Total Nitrogen (TN) removal The Aerobic Reactor biological treatment step was responsible for the degradation of organics and conversion of the organic nitrogen component into ammonia. The Advanced Oxidation step utilizing ozone was used to convert ammonia (NH 4 -N) into nitrates (NO 3 -N). Finally, the post-anoxic biological denitrification step was used to convert the nitrates from the AOP treated effluent into nitrogen gas. 3. Lei, C.N., et al., Biological Treatment of Thin-Film Transistor Liquid Crystal Display (TFT-LCD) Wastewater, Water Science Technology, 58 (5), (2008). 4. Lei, Chin-Nan, et. al., Biological Treatment of Thin- Film Transistor Liquid Crystal Display (TFT-LCD) Wastewater using Aerobic and Anoxic/Oxic Sequencing Batch Reactors, Chemosphere, 81, (2010). 5. Whang, L.M., et. al., Microbial Ecology and Performance of Nitrifying Bacteria in an Aerobic Membrane Bioreactor Treating Thin-Film Transistor Liquid Crystal Display Wastewater, Water Science Technology, 58, 12 (2008). 6. Standard Methods for the Examination of Water and Wastewaters APHA. 6. References 1. American Water Intelligence, Hu, Tai-Ho, et. al., Biological Treatment of TMAH (tetramethylammonium hydroxide) in a Full-Scale RFT- LCD Wastewater Treatment Plant, Bioresource Technology, 113, (2012).

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