Kinetic Modeling of Batch Slurry Reactions
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1 Kinetic Modeling of Batch Slurry Reactions Paul J. Gemperline 1, Mary Ellen McNalley 2, Ron Hoffman 2, Chun Hsieh 1, David Joiner 1, Julien Billeter 1 (1), (2) DuPont Crop Protection June 27, 2012 XIII Chemometrics in Analytical Chemistry Budapest, Hungary 1
2 Overall project goal develop monitoring technique for batch processes involving slurries Extend kinetic modeling approach to a prototypical slurry reaction at DuPont: sulfonylurea coupling reaction for monitoring purposes Make optical measurements in light-scattering medium Modify kinetic models to include: Dissolution of starting material A & flow-in of reagent B Nucleation and crystallization of product, P Develop empirical models for dissolution, nucleation and crystallization Kinetic models with reagent flow-in impose strict mass balance 2
3 Isothermal model with flow-in reagents r = k C C r r 1 1 = k C SA I = k C C W ASA AA AA r = k C C AA dc AA C AAin C AA = r1 r3 r4 + F V dc I C I = r1 r2 FAA V dc SA C V AA SA Batch 1 = r1 FAA spectra dcw CW = r3 FAA V dc ASAA C ASAA = r4 FAA V dc HA C HA = r2 + 2r3 + r4 F V dv = FAA = Est. conc x Est. pure spectra AA 3
4 Slurries A dynamic system of crystalline material suspended in a liquid medium Common Examples Production of pharmaceuticals Production of fine chemicals Biological absorption of pharmaceuticals Dynamic processes Dissolution of starting materials Nucleation and crystal growth of products Crystal products Often desire specific properties Size distribution, lattice form, etc. Relative rates determine properties Factors governing process rates Temperature Rate of stirring Crystal surface area Attrition Agglomeration 4
5 Challenges Optical Methods in Slurries Linear response is needed for kinetic modeling and self-modeling curve resolution Reflectance measurements include both light scattering and light absorption signals Mathematical resolution of the two is needed to estimate solid fraction and dissolved fraction Effective path length is dependent on Number density of light scattering particles Particle size distribution Wavelength ATR measurements for light absorption (dissolved fraction) 5
6 Project 1: modeling of dissolution of salicylic acid r = k( c c) sat n Develop a kinetic model for the dissolution of salicylic acid in a solvent mixture (52% ethanol, 48% water), based on a power law equation simpler system, easily controlled help gain understanding about kinetic of dissolution and crystallization in general Precisely controlled conditions will facilitate model validation Optimize the rate constant (k) and the exponent (n) of the power law equation Salicylic acid M.W g mol -1 pka 2.97 Monoclinic 6
7 Laboratory scale batch reactors Batch Titration Reactor 7
8 Laboratory scale batch reactors Batch Titration Reactor 8
9 Dissolution of salicylic acid Saturated Supersaturated Undersaturated Addition 1 Addition 2 Addition 3 Addition 4 Seeding Dilution 2 Dilution 4 Dilution 6 Dilution 1 Dilution 3 Dilution 5 9
10 Simplifying Assumptions Crystallization Rate high theory model Φ MW k = η s s c g r c r ( sat ) 3d sφv low theory model c c sat c r = k ( c c ) g c r d d = Dissolution Rate 2MWsk d s d d ( c sat sat c) r = m k ( c c) n Assumptions: Well-mixed slurries, the length of crystals, solid density, effectiveness factor, molecular weight of the solid, surface factor and volumetric shape factor do not change significantly in these experiments. Blandin, A. et. al., Chemical Engineering Journal, 2001, 81, Bhattacharya A. Chemical Engineering and Processing, 2007, 46,
11 Model batch ( ) Hessian UV-vis range used:: nm, NIR range used: 1100 nm Fitted ATR & NIR PLS est. of undissolved mass 3 4 Initial Conditions: Dissolution rate constant (kd) = L n-1 /(mol n-1 min) Crystallization rate constant (kc) = L n-1 /(mol n-1 min) Order parameter (n) = Order parameter (g) = Total SA mass added (mt) = g Concentration (c0) = (mol/l) Saturation limit (csat) = Initial volume (v0) = 22.7 ml Correction factor (cf) = 15 Optimized Parameters: Dissolution rate constant (kd) = L n-1 /(mol n-1 min) Crystallization rate constant (kc) = L n-1 /(mol n-1 min) Order parameter (n) = Order parameter (g) = Saturation limit (csat) = (mol/l) Correction factor (cf) = Sum of Square (SSQ) =
12 Experiment 2 Reaction of Salicylic Acid to form Acetylsalicylic Acid (Aspirin) Simple, well understood reaction to test modeling ability Process includes: Dissolution 4 Primary Reactions Crystallization 12
13 Reaction Mechanisms Catalyzed Reaction k1 SA + AA ASA + HA k2 ASA + AA ASAA + Water Addition k3 ASAA + H 2 O ASA + k4 AA + H 2O 2HA HA HA 13
14 Time (min) 14
15 15
16 Addition of Solid SA 16
17 Addition of Water 17
18 Onset of Crystallization 18
19 Begin Cooling Ramp 19
20 20
21 Saturation and Supersaturation Considered relative to equilibrium solubility Super-saturation Driving force of nucleation and crystal growth Metastable Generated by Cooling Anti-solvent addition Solvent evaporation 21
22 Differential Equations d[sa] solid = r d d[asaa] = r 2 dv [ASAA] V d[sa] = r d r 1 dv [SA] V d[asa] = r 1 r 2 + r 3 r c dv [ASA] V d[aa] = r 1 r 2 r 4 dv [AA] V d[h 2 O] = r 3 r 4 + f [H 2O] in V dv [H 2 O] V d[ha] = r 1 + r 2 + r 3 + r 4 dv [HA] V d[asa] solid = r c 22
23 Differential Equations d[sa] solid = r d d[asaa] = r 2 dv [ASAA] V d[sa] = r d r 1 dv [SA] V d[asa] = r 1 r 2 + r 3 r c dv [ASA] V d[aa] = r 1 r 2 r 4 dv [AA] V d[h 2 O] = r 3 r 4 + f [H 2O] in V dv [H 2 O] V d[ha] = r 1 + r 2 + r 3 + r 4 dv [HA] V d[asa] solid = r c 23
24 Concentration Profile of Active Species 24
25 Concentration Profiles of All Species 25
26 Validation of ASA Concentration Profiles by HPLC Preliminary results 26
27 Project 3: modeling of sulfonylurea coupling reaction Develop a combined kinetic model for the reaction, dissolution and crystallization for the slurry-based sulfonylurea coupling reaction. Use NIR diffuse reflectance spectroscopy 3 and kinetic model for monitoring purpose, and to perform endpoint and fault detections. Use High Performance Liquid Chromatography (HPLC) samples taken from the reaction mixture to validate kinetic models Barrett P., Smith B. et al. (2005). Organic Process Research & Development 9:
28 Sulfonyl Urea Coupling Reaction + CMBSI A4098 T6376 benzoic acid 2- [(Isocyanato)sulfonyl]- methyl ester 2-amino-4-methoxy- 6-methyl-1,3,5- triazine metsulfuron methyl 28
29 Apparatus setup at DuPont Sampling valve Overhead stirrer NIR reflectance probe Oil bath Thermocouple Peristaltic Pump Balance Recirculation tube 29
30 Sample batch slurry system Disappearance of NIR overtone band corresponds to consumption of starting material 30
31 Sulfonylurea coupling reaction (NIR) /07/22 Wavelength vs log (1/R) (Overall) log (1/R) At 2010 nm Wavelength (nm) 31
32 Modeling the Coupling Reaction 32
33 Coupling Reaction - Kinetic Fitting Results Concentration 33
34 Acknowledgements This research was supported by the National Science Foundation (NSF) under Grant Number CHE for Grant Opportunities for Academic Liaison with Industry (GOALI) This research was also sponsored by E.I. DuPont de Nemours and Co., Inc., Crop Protection Products and Engineering Technologies GOALI Principal Investigators (PIs) Dr. Mary Ellen McNally (Dupont) Dr. Ron Hoffman (Dupont) Dr. Paul Gemperline (ECU) Dr. Julien Billeter Chun Hsieh Chad Adkins Ethan Chiappisi Kristian Scott Dr. Liguo Song (UT) Dr. David S. Cho Dr. Frank Chambers (OSU) Consultant Dr. Kelsey Cook (NSF) 34
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