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Phi-TEC II | Bench-top, low phi-factor, adiabatic calorimeter

The Phi-TEC II is an adiabatic calorimeter, which supports the use of low Phi-factor test cells. This allows for manufacturing plant conditions to be fully replicated on a lab-scale thus allowing thermal runaway risks to be simulated and assessed. Utilizing low-Phi factor cells means that the runaway rate is not tempered by the test equipment, and subsequently, the measured rate of pressure increase and final temperature (T_end) – along with the calculated Time to Maximum Rate (TMR_d) and adiabatic temperature rise (∆T_ad,d) – are representative of what would be expected to occur during a production-scale incident

The impact of different operating scenarios can be explored using the Phi-TEC II, and the data generated can be utilized to determine appropriate safety controls for the manufacturing plant, such as:

Emergency and evaporation cooling
Quenching
Controlled depressurization
Vent sizing (in accordance with DIERS methodology)

Thus, the Phi-TEC II enables hazards to be fully evaluated, enabling their mitigation prior to scale-up.

High Phi-Factor Test Cell Catalog

Process Safety and Scale Up Specifications

Process Safety and Scale Up (Mandarin)

Process Safety and Scale Up Brochure

Applications

Hazard and Operability Assessment

Plant-scale parameters from the laboratory

The Phi-TEC II is a more advanced type of adiabatic calorimeter, which supports the use of low Phi factor test cells. This capability means that very little of the heat produced during a reaction or thermal runaway is consumed in warming the test cell. As a result, the runaway rate is not tempered.

The measured rate of pressure increase and final temperature (T_end), along with the calculated Time to Maximum Rate (TMR) and adiabatic temperature rise (ΔT_ad), are representative of what would be expected to occur during a manufacturing scale incident. Thus, the Phi-TEC II enables the hazards to be fully evaluated and explored, facilitating their mitigation prior to scale-up.

Safety by design

The data generated by the Phi-TEC II can be used to directly compare the impact of different operating scenarios. From this, the necessary safety controls for the manufacturing plant can be selected. Examples of these are:

Emergency and evaporation cooling
Quenching
Controlled depressurization
Vent sizing (in accordance with DIERS methodology)

Features and Options

Test Cells Types and Volumes

Thin-walled, 10ml to 110 ml, low Phi-factor test cells.
Also compatible with standard ARC-type high Phi-factor test cells, up to 10 ml volume.

Temperature Control

Ambient to 500°C.

High Pressure and Vacuum Systems

Pressure range 1 to 137 bar.

Sampling Systems

Optional: gas sampling.

Reagent Addition

Optional: High-pressure liquid feed pump for dosing of a critical ingredient at a controlled rate to the reaction vessel.
Optional: High-pressure injector for rapid addition of a critical ingredient to the test cell, replicating plant-scale conditions.

Stirring available

Indirect agitation with magnetic stirrer bar as standard; fixed stirring rate of 300 rpm.
Optional: Direct overhead stirring available for metal test cells for effective agitation of highly viscous samples.

Intelligent Software Control and Analysis

Control software enables regular data logging, multi-step recipes, parameter control, and feedback loops.
Customizable standard plans allow for easy running of the system with automated heating, detection of gas generation, and safety steps
Optional: High data rate acquisition available for characterizing extremely fast reactions (up to 10 000 Hz).
Optional: Bespoke testing methods.

Safety Features

Automatic, user-configurable, event monitoring and shutdown procedures if a safety condition is exceeded to ensure user safety.
Automatic hardware and software fail-safes are installed on every system.

Publications

The following are a list of some technical publications which highlight the use of the equipment.

Effects of typical additives on the thermal stability of ammonium peroxydisulfate

Mingju Jing, Yingnan Zhang, Jianpeng Wang, Juncheng Jiang Chi-Min Shu and Bin Zhang

06-Jan-2023

https://www.sciencedirect.com/science/article/abs/pii/S0950423023000049(Subscription or purchase maybe required for full access)

Thermal stability evaluation of tert-butyl peroxybenzoate mixed with impurities

Yilin Zhao, Nengcheng Zhou, Min Hua, Xiuxia Guo, Wenxing Zhang, Huichun Jiang, Xuhai Pan & Juncheng Jiang

02-Nov-2022

https://www.tandfonline.com/doi/abs/10.1080/00986445.2022.2126769(Subscription or purchase maybe required for full access)

Analysis of thermal hazards of tert-butylperoxy-2-ethylhexyl carbonate by calorimetric technique

Juan Zhou Chen-Ye Wei Min Hua, Xu-Hai Pan, Xin-Miao Liang, An-Dong Yu, Cyril G. Suetor and Jun-Cheng Jiang

06-Mar-2021

https://link.springer.com/article/10.1007/s10973-021-10619-3(Subscription or purchase maybe required for full access)

Analysis of thermal hazards of tertbutylperoxy2ethylhexyl carbonate by calorimetric technique

Juan Zhou, Chen-Ye Wei, Min Hua, Xu-Hai Pan, Xin-Miao Liang, An-Dong Yu, Cyril G. Suetor & Jun-Cheng Jiang

06-Mar-2021

https://doi.org/10.1007/s10973-021-10619-3(Subscription or purchase maybe required for full access)

Zero-Order Versus Intrinsic Kinetics for the Determination of the Time to Maximum Rate under Adiabatic Conditions (TMRad): Application to the Decomposition of Hydrogen Peroxide

Lamiae Vernières-Hassimi, Amine Dakkoune, Lokmane Abdelouahed, Lionel Estel, and Sébastien Leveneur

24-Jun-2017

https://doi.org/10.1021/acs.iecr.7b01291(Subscription or purchase maybe required for full access)

Experimental sensitivity analysis of the runaway severity of Dicumyl peroxide decomposition using adiabatic calorimetry

Olga J. Reyes Valdesa, Valeria Casson Moreno, Simon P. Waldram, Luc N. Véchot, M. Sam Mannan

10-Oct-2015

https://doi.org/10.1016/j.tca.2015.07.016(Subscription or purchase maybe required for full access)

Calorimetric studies on the thermal stability of methyl ethyl ketone peroxide (MEKP) formulations

Stephen R.Graham, Robert Hodgson, Luc Vechota, M.Iqbal Essa

01-Nov-2011

https://doi.org/10.1016/j.psep.2011.08.005(Subscription or purchase maybe required for full access)

Simple Procedure for Optimally Scaling-up Fine Chemical Processes. I. Practical Tools

Francesco Maestri, Sabrina Copelli, Renato Rota*, Lucia Gigante, Angelo Lunghi, and Paolo Cardillo

12-Jan-2009

https://doi.org/10.1021/ie800465d(Subscription or purchase maybe required for full access)

Safe and Productive Operation of Homogeneous Semibatch Reactors. II. The Nitration of N-(2-Phenoxyphenyl) Methane Sulfonamide

Francesco Maestri, Leonardo Re Dionigi, Renato Rota, Lucia Gigante, Angelo Lunghi, and Paolo Cardillo

31-Oct-2006

https://doi.org/10.1021/ie060262v(Subscription or purchase maybe required for full access)

Different scale experimental techniques to approach the problem of substances generated in the loss of control of chemical systems: a study on ethyl diazoacetate decomposition

Katia Marsanich, Federica Barontini, Valerio Cozzani, Alain Creemers, Ronald Kerstend

01-Jan-2004

https://doi.org/10.1016/j.jlp.2003.08.012(Subscription or purchase maybe required for full access)

Calorimetric Approach and Simulation for Scale-Up of a Friedel−Crafts Reaction

Lucia Gigante, Angelo Lunghi, Simone Martinelli, Paolo Cardillo, Luca Picello, Roberto Bortolaso, Marco Galvagni, and Renato Rota

06-Nov-2003

https://doi.org/10.1021/op030043a(Subscription or purchase maybe required for full access)

Thermal Stability: A Review of Methods and Interpretation of Data

Stephen M. Rowe

12-Oct-2002

https://doi.org/10.1021/op025569u(Subscription or purchase maybe required for full access)

The Use of Adiabatic Calorimetry for the Process Analysis and Safety Evaluation in Free Radical Polymerization

G. Maschio, J. A. Feliu, J. Ligthart, I. Ferrara & C. Bassani

01-Oct-1999

https://doi.org/10.1023/A:1010137217005(Subscription or purchase maybe required for full access)

Some Reaction Safety Aspects of Ruthenium-Catalyzed Allylic Oxidations of Δ-5-Steroids in the Pilot Plant

Michael Harre, Reinhard Haufe, Klaus Nickisch, Peter Weinig, Hilmar Weinmann, William A. Kinney, and Xuehai Zhang

24-Feb-1998

https://doi.org/10.1021/op9700587(Subscription or purchase maybe required for full access)

Downloads

The following are a list of available downloads.

High Phi-Factor Test Cell Catalog

Process Safety and Scale Up Specifications

Process Safety and Scale Up (Mandarin)

Process Safety and Scale Up Brochure

Phi-TEC II | Bench-top, low phi-factor, adiabatic calorimeter