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A Solution for Microelectronics Manufacturing Wastewater Treatment Nabin Chowdhury 1 , Denise Horner 1 , Temple Ballard 2 , Barbara Schilling 3 1 SUEZ/Degremont North American Research and Development Center; 2 SUEZ Treatment Solutions, Richmond, VA; 3 SUEZ treatment Solutions, Leonia, NJ. VWEA, Charlottesville, VA March 8, 2016
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A Solution for Microelectronics Manufacturing Wastewater Treatment

Nabin Chowdhury1, Denise Horner1, Temple Ballard2, Barbara

Schilling3

1 SUEZ/Degremont North American Research and Development Center;2SUEZ Treatment Solutions, Richmond, VA;

3SUEZ treatment Solutions, Leonia, NJ.

VWEA, Charlottesville, VA – March 8, 2016

2 I

Outline

Context

Drivers

Objectives

Process Development

Waste Characteristics

Biodegradability Test

Processes Selection

Experimental Results

Biodegradability Test

Waste Stream #1

Waste Stream #2

Findings

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment3 I

Context

Microelectronics manufacturing is one of the fastest growing

industries

A typical semiconductor

manufacturing facility

consumes 6.7 MGD water

Manufacturing process uses

toxic and recalcitrant chemicals

Industries are looking for water

reuse technologies.

(American Water Intelligence, 2012).

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment4 I

Chemicals/Contaminants

Parameter Concentration (mg/L)

Tetra-methyl ammonium hydroxide (TMAH) 5,000-60,000

Di-methyl sulfoxide <2000

Glycerol 5,000-66,000

Pyrazole 50-2,000

N-methyl pyrrolidone (NMP) 0-23,000

Triethanolamine (TEA) 0-10,000

Ethylene glycol (EG) 0-10,000

Morpholinopropylamine 0-3,000

Formaldehyde 60-700

Acetone 100-200

Methanol 300-400

Methyl methacrylate 600-700

Calcium fluoride 700-800

Potassium hydroxide 50-1000

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment5 I

Drivers

Increased pollutants loading limits POTWs’ ability to treat industrial

discharges

Difficult to treat complex water matrix

Corrosive, alkaline wastewater (pH ~12)

Toxic and persistent organic compounds

Inhibitory to biological processes

Limited information on pilot/full scale demonstration of >95% TOC and

TN removal from high strength microelectronics WW.

(e.g. TMAH).

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment6 I

Objectives

Develop a sustainable solution for microelectronics WW treatment

Investigate biodegradability of toxic substances (e.g. TMAH)

Evaluate nitrification and denitrification options

Achieve >98% TMAH degradation, >95% TOC and TN removal

Develop design, operational and kinetic parameters.

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment7 I

Waste Characteristics

Waste stream #1: Organic rich combined waste

Waste stream #2: Segregated waste (TMAH only)

ParameterWaste Stream

#1

Waste Stream

#2

pH >12 >12

TMAH (mg/L) 49,762 23,000

TOC (mg/L) 79,528 17,561

TN (mg/L) 9,311 4,675

COD (mg/L) 174,024 n/a

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment8 I

TOC, TKN Correlation with TMAH

R² = 0.999R² = 0.990

0

100

200

300

400

500

600

0 50 100 150 200 250 300

TMA

H (m

g/L)

TKN, TOC (mg/L)

TOC

TKN R² = 0.9992

R² = 0.9903

0

50

100

150

200

250

300

0 50 100 150 200 250 300

Ana

lyti

cal (

mg/

L)

Theoretical (mg/L)

TOC TKN COD

Analytical correlations:

TOC/TMAH = 0.527

TKN/TMAH = 0.154

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment9 I

TMAH Biodegradation

0

40

80

120

160

200

0 20 40 60 80

Ox

yg

en

Up

tak

e,

mg

Time (hour)

Oxygen Uptake

Activated Sludge

Acativated sludgeTMAH 35 mg/L

Acclimated sludge

Acclimated sludgeTMAH 35 mg/L

Acclimated sludgeTMAH 70 mg/L

Respirometer testing: biodegradation of

TMAH using AS and acclimated biomass

OU for degradation of TOC/TMAH and

formation of ammonia-nitrogen

0

10

20

30

40

50

0 20 40 60 80

Con

cen

trat

ion,

mg/

L

Time (hour)

TOC Degradation

Activated sludge TMAH 35 mg/L

Acclimated sludge TMAH 35 mg/L

Acclimated sludge TMAH 70 mg/L

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment10 I

Waste Stream #1

Pre-Anoxic + Aerobic + Clarifier + Aerobic + Clarifier

or

Pre-Anoxic + Aerobic + Clarifier + AOP + Post-Anoxic + Clarifier

Qinf

Aerobic

Reactor

Pre

AnoxicClarifier

QeffClarifierPost

Anoxic

AOP

C source

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment11 I

Waste Stream #1: Lab-scale Test Data

Influent Anoxic Aerobic AOPPost

AnoxicEffluent Removal

COD (mg/L) 2,600 925 85 <30 n/a n/a >98%

TOC (mg/L) 1,350 450 60 <30 n/a n/a >98%

NH4-N (mg/L) 14 56 106 <1.0 n/a 3 >98%

NO3-N (mg/L) <0.4 <0.4 <0.4 97 <0.4 <0.4 n/a

TKN (mg/L) 165 141 118 33 n/a 27 >80%

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment12 I

Waste Stream #2

Aerobic + Clarifier + AOP + Post-Anoxic + Clarifier

Qeff

Aerobic ReactorClarifier Clarifier

Post

Anoxic

AOP

C source

Qinf

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment13 I

West Stream #2: Bench-scale Test Results

0%

20%

40%

60%

80%

100%

0

1,000

2,000

3,000

4,000

0 7 14 21 28 35 42 49 56 63 70 77 84 91

Inf TOC

Eff TOC

% TOC Removal

TOC

Co

nce

ntr

atio

n, m

g/L

TOC

Re

mo

ved

,%

Days

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment14 I

West Stream #2: Bench-scale Test Results

Influent TN 750 mg/L

Aerobic effluent NH4-N 670 mg/L

Effluent TN <30 mg/L

0

10

20

30

40

50

60

70

80

90

100

0

100

200

300

400

500

600

700

800

900

1000

0 7 14 21 28 35 42 49 56 63 70 77 84 91

Inf TKN

Aero Eff TKN

Aero Eff NH4-N

% TMAH Conversion

Inf NH4-N

TKN

, NH

4-N

Con

cent

rati

on, m

g/L

TMA

H C

onve

rsio

n,%

TMAH Biodegradation

Days

SampleInfluent TMAH (mg/L)

Effluent TMAH (mg/L)

% Removal

1 4,000 39 ≥99%

2 4,100 <0.5 ≥99%

3 3,700 <0.5 ≥99%

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment15 I

West Stream #2: Bench-scale Test Results

AOP: Ozonation

NH4-N NO3-N

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment16 I

West Stream #2: Bench-scale Test Results

Aerobic degradation – AOP (nitrification) – Anoxic (biological de-nitrification)

0

20

40

60

80

100

0

200

400

600

800

1000

0 7 14 21 28 35 42

Inf TN Final Eff TN

NH4-N in Bio-Effluent Bio Eff TKNs

% TN Removal

TN, N

H4-

N C

once

ntra

tion

, mg/

L

TN R

emov

ed,%

TN Performance

Days

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment17 I

West Stream #2: Bench-scale Test Results

Aerobic-AOP-Anoxic for TMAH treatment

Influent Aerobic AOP Anoxic Effluent Removal

COD (mg/L) <30 201 67 n/a n/a n/a

TOC (mg/L) 2,800 80 n/a n/a n/a >98%

NH4-N (mg/L) 7 690 8 n/a 6.4 n/a

NO3-N (mg/L) <0.4 <0.4 610 <0.4 <0.4 n/a

NO2-N (mg/L) <0.5 <0.5 <0.5 <0.5 <0.5 n/a

TKN (mg/L) 750 715 30 n/a 26 >95%

TMAH (mg/L) 4,000 n/a n/a n/a BDL >99%

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment18 I

Findings

Combination of AOP and Biological treatment provides a complete

treatment solution for microelectronics wastewater

Aerobic biodegradation of TMAH generated ammonia-nitrogen

even at TMAH of 4000 mg/L. Biological nitrification was not

observed throughout the study

Ozonation (AOP) completely nitrify ammonia-nitrogen generated

from the aerobic biodegradation of TMAH

>98% TMAH degradation, and >95% TOC and TN were achieved.

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment19 I

Acknowledgement

SUEZ / Degremont North American Research and Development Center

(DENARD), Ashland, VA

John Williamson

Keith Newton

SUEZ Treatment Solutions, Richmond, VA

Temple Ballard

Rich Ubaldi

Amit Kaldate

SUEZ Treatment Solutions, Leonia, NJ

Bruno Heiniger

March 8, 2016; A solution for Microelctronics Manufacturing WW Treatment20 I

Thank You!

Questions & Answers

Nabin Chowdhury, PhD

Sr. R&D Engineer

SUEZ / Degremont North American Research & Development Center

[email protected]

804-521-7478


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