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Automated Process Control Autoclave Engineers Erie, PA USA Improving Polymerization Catalyst Research 3 rd Automated Process Control Autoclave Engineers Erie, PA USA Improving Polymerization Catalyst Research 3 rd Eurokin Workshop - San Donato, Milanese September 2000 www. Autoclave. Engineers. com

Presentation Overview z Available hardware for Gas-Solid catalyst research z Available hardware for Gas-Liquid-Solid Presentation Overview z Available hardware for Gas-Solid catalyst research z Available hardware for Gas-Liquid-Solid catalyst research z Range of Automatic Controls and Instrumentation available as accessories z Case Study 1: Automated polymerization synthesis compared to a manual system. z Case Study 2: Automated, closed system polymer synthesis compared to a manual system.

Gas-Solid Reaction Equipment BTRS Jr. ®/ BTRS 900 Gas-Solid Reaction Equipment BTRS Jr. ®/ BTRS 900

Gas-Solid Reaction Equipment Berty Reactor / Caldwell Gas-Solid Reaction Equipment Berty Reactor / Caldwell

Gas-Liquid-Solid Reaction Equipment Gas-Liquid-Solid Reaction Equipment

Gas-Liquid-Solid Reaction Equipment Gas-Liquid-Solid Reaction Equipment

Range of Control Systems Ê Manual Ë Open-loop with display Ì Closed-loop with display Range of Control Systems Ê Manual Ë Open-loop with display Ì Closed-loop with display Í Closed-loop with analog retransmission Î Closed-loop with computer control ý Remote Manipulation of variables, real-time trending, data logging, etc. . » Closed-loop with Custom computer control system ý Full computer control, batch automation, data logging, alarm interlocks, etc. . l Each level of sophistication reduces variations. l Case studies demonstrate improvement between Levels 3 and 6.

Case Study 1 z. Albemarle Corp. - Baton Rouge, LA z. Application: Sample Preparation Case Study 1 z. Albemarle Corp. - Baton Rouge, LA z. Application: Sample Preparation for QC of Catalyst z. Objective: Comparisons between lots of catalyst. z. Problem: Poor Reproducibility z. Strategy: Process Automation

Mechanical System Case Study 1 Mechanical System Case Study 1

Control System Case Study 1 Control System Case Study 1

Case Study 1: Results z. Catalyst yield variation drops from +/20% to +/- 7% Case Study 1: Results z. Catalyst yield variation drops from +/20% to +/- 7% z. Rapidly Implemented z. Productivity Improved

Case Study 2 z WR Grace Columbia, S. C. U. S. A. z Application: Case Study 2 z WR Grace Columbia, S. C. U. S. A. z Application: Polymerization Research-Multistation Synthesis z Objectives: y 1. Improve reproducibility for statistical analysis. y 2. Eliminate environmental contamination. z Problem: System error approx. @ size of experimental effect z Strategy: Process Automation, Closed System

Mechanical System Case Study 2 Mechanical System Case Study 2

Control System Case Study 2 Control System Case Study 2

Case Study 2: Results z. Undisclosed Improvement in reproducibility. z. Benefit such that a Case Study 2: Results z. Undisclosed Improvement in reproducibility. z. Benefit such that a two additional, four reactor systems, were purchased.

Conclusions z. Consider Process Automation to improve the ratio of experimental effect (signal) to Conclusions z. Consider Process Automation to improve the ratio of experimental effect (signal) to system error (noise).

Acknowledgements z. Albemarle Corporation y. Glen Mc. Clelland y. Jamie Strickler z. Cryovac Division Acknowledgements z. Albemarle Corporation y. Glen Mc. Clelland y. Jamie Strickler z. Cryovac Division of Sealed Air y. Paul Hughes y. Nate Miranda z. Autoclave Engineers y. Steven Simon and Tim Porco