Modeling and Parameter Estimation of Interpenetrating

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1 Modeling and Parameter Estimation of Interpenetrating Polymer Network Process EWO Spring Meeting March, 2009 Weijie Lin Advisors: Lorenz T. Biegler, Annette Jacobson Department of Chemical Engineering, Carnegie Mellon University, it Pittsburgh, PA 15213

2 Interpenetrating Polymer Network Process Monomer Initiator Polymerization reactor Seed particle Monomer droplet Aqueous media Seed Polymer A Monomer B Fig 1. Seed Polymerization Process 2

3 Overview Objective: Tool: 3

4 Previous Work Review New Model ldevelopment Semi batch suspension polymerization (SSP) Seeded emulsion polymerization (SEP) Supported Catalyst Polymerization(SCP) Components Continuous Water, phase Monomer Water Water soluble initiator (+ Inert hydrocarbon diluents ) Water Dispersed phase Reaction sites Monomer/Polymer droplets, Suspension agent, Oil soluble initiator Monomer droplets, Latex particles, Emulsifier Monomer/Polymer Droplets Latex particles Formed polymer particles with catalysts sites Surface of the catalysts supporter Seed polymerization (SP) Monomer droplets, Seed particles, Suspension agent, Oil soluble initiator Seed particles Kinetics Similar to bulk Compartmentalisation Heterogeneous Heterogeneous Particle evolution Coalescence/breakup Homogeneous and micellar nucleation Growing polymer layers around Growing new polymer active sites penetrating the seeds Tab 1. Special Features of IPN particle growth 4

5 Single Particle Modeling Particle growth mechanism Intra particle diffusion Dynamics of the kinetics Reaction Media Skin shell Based on mass conservation law External mass transfer Collision absorption assumption Internal mass transfer Fick s first law approximation Growing Growing shell polymer seed Fig 3. Reaction-Zone-Divided Model Structure Local reaction rate 5

6 New Improvement (1) Modeling Particle growth Partial molar Volume model Partial molar properties of j Concentration dependent approximation Shell volume representation Initial condition estimation Initial conversion / molecular weight 13 system parameters + 2/process initial condition 6

7 Parameter Ranking and Subset Selection (1) Parameter Ranking Subset selection [Lund,B; Foss,B, Automatic 2008, 44(1), ] 7

8 Parameter Ranking and Subset Selection (2) Multi-response se sensitivity s coefficient c e matrix 3 types of measurements Molecular weight Conversion ratio Particle size 3 grades of products 19 model parameters 8

9 Parameter Ranking and Subset Selection (3) Tab 2: Result of Parameter Selection and Estimation Combine the parameter ranking information with the simultaneous estimation strategy 9

10 New Estimation Results Fig 4. Fitting results for Three Grades of Products 10

11 New Improvement (2) Kinetics of Multi polymer System Networking reactions Key Concern of the Model: Model complexity Multiple reaction probability distributions from model sources Highly nonlinear structure Difficulties for efficient optimization 11

12 Possible Reactions in IPN System I* Grafting Intermolecular transfer Inter radical generation Possible growing and networking Network β scission Fig 5. Schematic Representation of the Nonlinear Reactions in the IPN System Free radical on chain B Free radical on chain hi A Grafted polymer Crosslinked polymer 12

13 Nonlinear Polymer Molecular Weight Cl Calculation lti Numerical fractionation Unableto model chain Instantaneous MWD method random scission Discrete weighted residuals Approximation functions of molecular weight distribution Monte Carlo simulation Difficult to optimization Double moment method Population balance approach Has not applied for polymer composite system 13

14 Decompose the Nonlinear Structure Separate representation for two polymers = + = + 14

15 Statistical and Sectional Grid Approach (1) analogy to Chain combination / breakup Particle breakup /aggregation Sectional grid approach Fixed pivot technique (Number and mass are preserved by set f(v) to zeroth and first properties) 15

16 Statistical and Sectional Grid Approach (2) Chain random scission: 16

17 Statistical and Sectional Grid Approach (3) Chain combination: 17

18 Statistical and Sectional Grid Approach (4) Nonlinear chain structure is recovered by statistical assemblage Position independent assumption Network fraction is classified by crosslinked chain length New model capabilities i Gel fraction / Gel composition Branching frequency Joint molecular weight distribution 18

19 Summary Single particle model has been improved in modeling particle growth Consistent agreement was observed in all studied cases Parameter ranking and subset selection are implemented for parameter estimation Kinetics of polymer composite is under study. More efficient modeling approach is proposed for further research 19

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