IPR By: Supervised By: Institute t for Polymer Research, Department tof fchemical Engineering University of Waterloo
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1 Active Site Identification and Mathematical Modeling of fp Polypropylene l Made with Ziegler-Natta Catalysts By: Ahmad Alshaiban Supervised By: Prof. João B.P. Soares Institute t for Polymer Research, Department tof fchemical Engineering i University of Waterloo 1
2 OUTLINE OBJECTIVES INTRODUCTION Saudi Basic Industries Corporation SABIC Polypropylene py Facts & Figures Polypropylene Structure MODEL & RESULTS Population Balance and Method of Moments: Model Results: Steady State vs. Dynamic CSTR s Solutions Monte Carlo Approach: Model Results CURRENT & FUTURE WORK CONCLUSION 2
3 OBJECTIVES Develop mathematical models for the steady-state and dynamic simulation of propylene polymerization with Ziegler-Natta Ntt catalysts tl t in industrial id tilreactors using different modeling approaches: population balances and method of moments and the Monte Carlo techniques Describe, for the first time, site transformation by electron donors, with a mathematical model and quantify its effect on polymer chain microstructure 3
4 INTRODUCTION SABIC is the world s fourth largest producer of polyolefins. It is the world s third largest producer of polyethylene and the fifth largest producer of polypropylene. Overall polypropylene demand is forecasted to grow globally at a rate of 5.8% in timeframe Source: Alberta - Polypropylene Market Study CMAI (Sep. 2004) 4
5 INTRODUCTION Propylene Polypropylene py Commercial PP Isotactic Atactic Syndiotactic i 5
6 Z-N NMultiple l Site Catalyst t 110 Face Mg +2 Cl 100 Face Highly isotactic Low isotactic Atactic Ti Mg Cl Vacancy Polymer 6
7 Reaction Mechanism: Site Transformation: Propagation: Ti Atactic Mg Electron Donor D D Cl Vacancy Ti + Ti Highly isotactic Polymer Termination: Ti + H H Ti H + 7
8 Species Classification Blocks Stereo-Blocks Pure Atactic Pure Isotactic 8
9 Single Site Steady State Simulation Results 9
10 Steady State Solution for One Site Type: R P1 /R P2 = 1, R P1 /R T1 =1364, R P2 /R T2 =1364 Effect of Changing the Electron Donor Concentration 1/2 No Donor 50.00% Pure Isotactic Stereo-Blocks 0.00% Pure Atactic 0.00% No Donor 0.00% 00% 0.00% 0.00% 0.00% % 50.00% 00% 1 block 2 blocks 3 blocks 4 blocks 5 blocks 6 blocks Normal [Do] 6.04% 7.19% 86.77% Pure Isotactic Pure Atactic Stereo-Blocks 2 [Do] 2.26% 90.91% Pure Isotactic Stereo-Blocks 6.83% Pure Atactic Normal [Do] 1.13% 13% 2 [Do] 1.80% 0.07% 07% 0.05% 4.93% 0.02% 0.01% 6.00% 0.00% 0.00% 92.81% 1 block 2 blocks 3 blocks 4 blocks 5 blocks 6 blocks 93.17% 1 block 2 blocks 3 blocks 4 blocks 5 blocks 6 blocks M n (g/mol) 57,000 57,000 57,000 M w (g/mol) 114, , , PDI
11 Steady State Solution for One Site Type: R P1 /R P2 = 1, R P1 /R T1 =1364, R P2 /R T2 =1364 Effect of Changing the Electron Donor Concentration 2/2 Normal [Do] 6.04% 7.19% 86.77% Pure Isotactic Pure Atactic Stereo-Blocks 2 [Do] 2.26% 90.91% Pure Isotactic Stereo-Blocks 6.83% Pure Atactic Normal [Do] 1.13% 13% 2[Do] 1.80% 007% 0.07% 0.05% 4.93% 0.01% 0.02% 6.00% 0.00% 0.00% 92.81% 1 block 2 blocks 3 blocks 4 blocks 5 blocks 6 blocks 93.17% 1 block 2 blocks 3 blocks 4 blocks 5 blocks 6 blocks 1/2 [Do] 13.38% Pure Isotactic Stereo-Blocks 7.02% 79.60% Pure Atactic 1/2 [Do] 0.64% 0.03% 03% 6.34% 0.00% 0.00% 92.98% 1 block 2 blocks 3 blocks 4 blocks 5 blocks 6 blocks M n (g/mol) 57,000 57,000 57,000 M w (g/mol) 114, , , PDI
12 Steady State Solution for One Site Type Block s Properties and Their Weight Distribution End Iso End Ata i Mn Mw PD Mn Mw PD 1 56, , ,000 92, , , , , , , , , , , , , , , , , , , , , i = Weight % by Block 0.00% 1.04% 3.10% 2.90% 6.04% 0.00% 0.08% 08% 0.00% 0.01% 0.03% 0.03% 86.77% 1 end Iso 1 end Ata 2 end Iso 2 end Ata 3 end Iso 3 end Ata 4 end Iso 4 end Ata 5 end Iso 5 end Ata 6 end Iso 6 end Ata 12
13 Steady State Solution for One Site Type Effect of Changing the Donor Type Donor A Donor B Donor C Pure Isotactic Stereo-Blocks Donor A 6.04% 92.81% 7.19% 86.77% 95.10% 1.25% 3.64% 22.38% 11.74% 65.87% Pure Atactic Pure Isotactic Pure Atactic Pure Isotactic Pure Atactic Stereo-Blocks Stereo-Blocks 1.13% 0.94% 1.21% 0.05% Donor B 0.02% Donor C 0.10% 0.01% 0.01% 0.01% 6.00% 0.00% 2.68% 0.00% 10.43% 0.00% 1 Block 2 Blocks 3 Blocks 4 Blocks 5 Blocks 6 Blocks 96.36% 1 Block 2 Blocks 3 Blocks 4 Blocks 5 Blocks 6 Blocks 88.26% 1 Block 2 Blocks 3 Blocks 4 Blocks 5 Blocks 6 Blocks K + / K A K / K A M n g/mol 57,000 57,000 57,000 M w g/mol 114, , ,000 PDI
14 Steady State Solution for One Site Type Normal [H2] 604% 6.04% 7.19% 86.77% Pure Isotactic Pure Atactic Stereo-Blocks Effect of Changing the Hydrogen Concentration 2 [H2] 1/2 [H2] 7.45% 88.65% 3.90% Pure Isotactic Pure Atactic Stereo-Blocks 4.28% 12.70% Normal [H2] 1.13% 0.05% 2 [H2] 0.33% 0.01% 1/2 [H2] 3.33% 0.25% 6.00% 0.01% 356% 3.56% 0.00% 008% 0.08% 0.00% 0.00% 9.04% 0.01% 92.81% 1 Block 2 Blocks 3 Blocks 4 Blocks 5 Blocks 6 Blocks 96.10% 1 Block 2 Blocks 3 Blocks 4 Blocks 5 Blocks 6 Blocks 83.01% Pure Isotactic Pure Atactic Stereo-Blocks 87.29% 1 Block 2 Blocks 3 Blocks 4 Blocks 5 Blocks 6 Blocks M n M w R P1 /R T1 =1364, R P2 /R T2 =1364 R P1 /R T1 =682, R P2 /R T2 =682 R P1 /R T1 =2727, R P2 /R T2 =2727 g/mol 57,000 29, ,000 g/mol 114,000 58, , PDI
15 Multiple Sites Steady State Simulation Results 15
16 Summary Results for a 4-Site Model of Propylene Polymerization Site Overall Mass % Mass % Mass % Mass % Mass % Pure Isotactic 98.22% 100 % 100 % 93.40% 86.47% Pure Atactic 0.30% 0.0 % 0.0 % 2.84% 0.88% Stereo-Blocks 1.48% 0.0 % 0.0 % 3.76% 12.64% Block weight %: Single-state stereospecific sites Two-state sites 1 block 97.98% 100 % 100 % 96.24% 87.35% 2 blocks 1.44% 0.0 % 0.0 % 3.24% 7.89% 3 blocks 0.52% 0.0 % 0.0 % 0.50% 4.25% 4 blocks 0.04% 0.0 % 0.0 % 0.01% 0.35% 5 blocks 0.01% 0.0 % 0.0 % 0.00% 0.14% 6 blocks 0.00% 0.0 % 0.0 % 0.00% 0.01% M n (g/mol) 52,081 62, ,316 7, ,523 M w (g/mol) 231, , ,595 16, ,055 PDI R P1 /R P R P1 /R T R P2 /R T
17 Single Site Dynamic Simulation Results 17
18 Dynamic Solution Simulation Effect of Donor, Hydrogen, & Monomer Concentrations on Molecular Weight eight (g/mol) Molecular W x 10 M w M n 4 Overall : Molecular l Weights vs. Time Normal Conditions 2 [Do] 2 [H 2 ] 2 [M] Time "Sec" " x
19 Isotactic Mass % Atactic 10 Stereoblocks Dynamic Solution Simulation Effect of Donor, Hydrogen, & Monomer Concentrations on Tacticity Normal Conditions Overall: Mass % vs. Time 2 [Do] 2 [H 2 ] 2 [M] Time "Sec" x 10 4 Isotactic Stereoblocks Atactic 19
20 Dynamic Solution Simulation Molecular Weights by Block Number Molecular Weigh ht (g/mol) 3.5 x 10 5 Normal Condition : Molecular Weights % vs. Time Mn Block 1 Mn Block 2 3 Mn Block 3 Mn Block Mn Block 5 Mn Block 6 Mw Block 1 2 Mw Block 2 Mw Block 3 Mw Block Mw Block 5 Mw Block Time "Sec" 20
21 Multiple Sites Dynamic Simulation Results 21
22 Molecular Weigh ht (g/mol) Dynamic Solution Simulation for a 4-Site Model Molecular Weight & Polydispersity Index 4.5 x 105 Overall : Molecular Weight % vs. Time Mn Overall 4 Mw Overall Mn Mw 1 Mn 3 2 Mw Mn 3 Mw 2 3 Mn Mw PDI 5 Overall : PDI vs. Time PDI Overall 4.5 PDI 1 PDI 2 PDI 3 4 PDI Time "Sec" Time "Sec"" 22
23 Monte Carlo Simulation P = p R p + R p R tr + R tf P = tr R p R tr tf Ptf = + Rtr + Rtf Rp + Rtr + Rtf R Can have the whole distribution ib i 23
24 Monte Carlo Approach r = Chain Length r = r + 1 Yes Start i= 1:2 (Two States) P p1 + P tr1 + P tf1 = 1 P pi, P tri, P tfi P p2 + P tr2 + P tf2 = 1 r = 0 Rand r = r + 1 No Rand d< P t Yes p2? State = 1? Rand d< P p1? No Rand < No No Rand < P p2 +P tr2 P p1 +P tr1 Yes State = 1 State = 2 Yes No Save chain information Save chain information Yes Another No No Another Yes End chain? chain? 24
25 Monte Carlo Approach Donor Effect: P p1 + P tr1 + P tf1 = 1 P p2 + P tr2 + P tf2 = 1 R tf = k + Do P tf = R p II [ P ][ Do] r + R tf R tr + R tf Donor Type Donor Concentration 25
26 Chain Length vs. Weight Normal [Do] ion Weight Fract M n = 57,078 M w = 113,650 PDI = 1.99 ^ Normal Do Overall Pure Isotactic Pure Atactic Setreo Blocks Chain Length 26
27 Chain Length vs. Weight 1/2 [Do] Weight Frac ction Overall Pure Isotactic Pure Atactic Setreo Blocks Weight Frac ction M n = 57,213 M w = 115,780 PDI = 2.02 ½ ^ Do Overall Pure Isotactic Pure Atactic Setreo Blocks Chain Length Chain Length
28 Chain Length vs. Weight 2 [Do] Weight Frac ction Overall Pure Isotactic Pure Atactic Setreo Blocks ction Weight Fra M n = 56,990 M w = 114,540 PDI = ^ Do Overall Pure Isotactic Pure Atactic Setreo Blocks Chain Length Chain Length 28
29 CURRENT & FUTURE WORK Add additional features to the Monte Carlo code such as number of defects per chain and end group determination Use the microstructural information obtained by simulation to predict polypropylene l fractionation with the temperature t rising elution fractionation (TREF) and the nuclear magnetic resonance ( 13 C NMR) Plan for the parameter estimation for some known commercial catalyst / donor systems. 29
30 CONCLUSION The model is able to predict the polypropylene properties taking in consideration site transformation in the presence of the electron donor. The model is able to predict the tacticity during propylene polymerization which could enhance and used as a tool for the process control. The model will be used for parameter estimation for some commercial catalyst /electron donor systems. The microstructural information obtained by simulation can be used to predict polypropylene py fractionation with the temperature rising elution fractionation (TREF). 30
31 THE END THANK YOU 31
32 Steady State vs. Dynamic Solution Simulations Mass % Steady State Dynamic Error % Pure Isotactic Pure Atactic 6.07% Stereo-Blocks 7.20% By Block %: 86.73% 86.68% -0.1% 6.10% 7.22% 0.5% 0.2% 1 block 92.81% 92.81% 0.0% 2 blocks 6.00% 6.00% 0.0% 3 blocks 1.13% 1.13% 0.0% 4 blocks 0.05% 0.05% 0.0% 5 blocks 0.01% 0.01% 0.0% 6 blocks 0.00% 0.00% 0.0% M n (g/mol) 57,270 57, % M w (g/mol) 114, , % PDI % 32
33 Steady State vs. Dynamic Solution Simulations Steady State Dynamic Error % i Mn Mw PD Mn Mw PD Mn Mw PD 1 55, , , , % 0.00% 0.00% 2 102, , , , % 00% 0.00% 00% 0.00% 00% 3 157, , , , % 0.00% 0.00% 4 204, , , , % 0.00% 0.00% 5 259, , , , % 0.00% 0.00% 6 306, , , , % 0.00% 0.00% Steady State Dynamic Error % Mn Mw PD Mn Mw PD Mn Mw PD Iso-Segments 56, , , , % -0.02% -0.03% Ata-Segments 46,274 92, ,271 92, % 0.01% 0.00% Total Segments 55, , , , % -0.08% 0.01% 33
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