7m MEA & 7m MEA/2m PZ Kinetics, Thermodynamics & Degradation
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1 7m MEA & 7m MEA/2m PZ Kinetics, Thermodynamics & Degradation By: Ross Dugas Marcus Hilliard Andrew Sexton Jason Davis Nidhi Mathur May 24, 2007
2 Scope of the Presentation Introduction to MEA/PZ Kinetics and Thermodynamics Apparatus Results Conclusions Oxidative Degradation Thermal Degradation
3 Why use 7m MEA/2m PZ? Faster rates kinetics Less packing Richer solutions lower energy requirements Increased capacity VLE Lower flow rates Smaller heat exchangers, pumps
4 MEA/PZ/CO 2 Primary Reactions 2 CO 2 Loading = n MEA n + CO2 2n PZ
5 Kinetics and Thermodynamics Ross Dugas Marcus Hilliard
6
7
8 Operating Conditions: 1 atm o C Equilibrium hr
9 Hilliard Jou (1995) Dugas 60C P * CO2 (kpa) C Loading (mol/mol) 7m MEA
10 Hilliard Dugas P * CO2 (kpa) C 40C Loading (mol/mol alk ) 7m MEA/2m PZ
11 CO2 Conc (m) % increase 7m MEA/2m PZ 7m MEA C P* (Pa)
12 0.01 Partial Pressure of Amine [kpa] MEA 7 m MEA/2 m PZ PZ 7 m MEA/2 m PZ 40 C Partial Pressure of CO 2 [kpa]
13 [ ] + + = T o g g G CO P k k k K CO prod l 2 * '' 2, ' g g G k k K + = = ) ( ] [ ] ([ ) ( ) ( * 2 2, , 2 * CO i CO CO l b i l i CO CO g CO CO G CO P P H k or CO CO k P P k P P K N
14 4x x C Aboudheir Laminar Jet Absorber Dugas Wetted Wall Column k g ' (mol/s. Pa. cm 2 ) 2x x C 0 7m MEA Loading (mol /mol ) CO2 amine
15 7m MEA/2m PZ 7m MEA k g ' (mol/s. Pa. cm 2 ) 1x C 60C 1x P* (Pa)
16 Kinetics and Thermodynamics Conclusions VLE measurements from Dugas, Hilliard, and Jou (1995) matched for 7m MEA over a wide range of CO 2 loadings. Dugas and Hilliard agree for 7m MEA/2m PZ. 7m MEA/2m PZ has 45% greater CO 2 capacity (40 C from Pa, molality basis). MEA and PZ volatility have been quantified. Discrepancies in Dugas and Aboudheir (2002) rate data can probably be explained by mass transfer phenomenon. 7m MEA/2m PZ shows faster rates than 7m MEA
17 Oxidative Degradation Andrew Sexton
18 Modified Low Gas Flow Apparatus O 2 CO2 100 ml / min 1400 RPM 98% O 2 / 2% CO 2 feed Saturated CO 2 / O 2 mixture VORTEXING Water Reservoir: 55 o C Amine Solution
19 Ion Chromatography Analysis Methods Dionex ICS-2500 System Anion: AS15 Ionpac Column & ASRS 4-mm 4 Suppressor Linear gradient of NaOH eluent 1.60 ml/min, 30 o C Cation: CS17 Ionpac Column & CSRS 4-4 mm Suppressor Constant methanesulfonic acid (MSA) eluent 0.40 ml/min, 40 o C
20 700 Concentration (mm) m MEA/2m PZ, 0.1 mm Fe, 5 mm Cu Formate Experiment Time (hrs)
21 40 7m MEA/2m PZ, 0.1 mm Fe, 5 mm Cu Concentration (mm) Formate Nitrate Oxalate 10 Ethylenediamine Glycolate 0 Nitrite Acetate Experiment Time (hrs)
22 Degradation Product Formation Rates (mm( mm/hr) Distinguishing Conditions 7m MEA, 250 ppm Cu 7m MEA/2m PZ, 5 ppm Fe, 250 ppm Cu 7m MEA/2m PZ, 5 ppm Fe Formate Acetate Oxalate Glycolate Nitrate Nitrite EDA Total Carbon Total Nitrogen
23 Oxidative Degradation Conclusions Confirmed formate, glycolate, oxalate as significant degradation products Discovered nitrate, nitrite, and ethylenediamine as significant products MEA/PZ relatively stable at low catalyst concentration Cu catalyzes MEA/PZ more than MEA by itself
24 Thermal Degradation Jason Davis Nidhi Mather
25 MEA/PZ Thermal Degradation Thermal degradation is a known loss mechanism for MEA and DEA at stripper conditions No literature on thermal degradation for piperazine or piperazine blend systems Less thermal degradation expected for piperazine because no alcohol group
26 Method Solutions loaded with CO 2 and placed into a set of 5x10ml stainless steel sample bombs Sample containers loaded into forced convection oven and each one removed at desired time interval Samples analyzed with GC and titration to determine the amount of MEA and piperazine remaining
27 PZ Systems (α=0.4)( 40 5m PZ GC 135 C Amine Losses (%) GC 120 C GC 11m MEA 120 C Titration 120 C Titration 135 C Time (weeks)
28 MEA/PZ Systems (α=0.4)( 50 7m MEA/2m PZ Amine Losses (%) GC 135 C Titration 135 C GC 120 C GC 11m MEA 120 C Titration 120 C 2 3 Time (weeks)
29 MEA Systems (α=( α=0.4) MEA Losses (%) m MEA Gas Chromatography 150 C 120 C 100 C Time (weeks)
30 Thermal Degradation Results Piperazine reaches equilibrium with its degradation product in a short time according to the GC results This equilibrium product comprises a large percentage of the original piperazine No losses are detected via ph titration The degradation products retain alkalinity and may be reversible back to piperazine
31 Questions? Dr. Gary Rochelle Ross Dugas
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