Analysing Phenol-Formaldehyde Resin Reaction For Safe Process Scale Up
|
|
- Denis Neal
- 6 years ago
- Views:
Transcription
1 SYMPOSIUM SERIES NO 16 HAZARDS IChemE Analysing Phenol-Formaldehyde Resin Reaction For Safe Process Scale Up David Dale, Process Safety Manager, SciMed/Fauske and Associates, Unit B4, The Embankment Business Park, Vale Road, Stockport, Cheshire. SK4 3GN. The production of phenolic resins is an old but still very active industry with uses today including heat shields, abrasives, coatings, composites, felt-bonding, laminates, moulding and many others. Over the years much safety work has been done characterising the process safety aspects of these challenging but industrially important phenol-formaldehyde reactions. Two types of phenol-formaldehyde resins, namely Novolac and Resole, can be formed depending on the formaldehyde to phenol ratio. In this paper we will briefly discuss various calorimetry techniques (differential scanning, reaction and adiabatic), what data each can provide, and then show how they can be used in conjunction with each other to fully characterise the energies involved in a generic Resole recipe. The obtaining of such thermal data is an essential part of the process if we are to make informed decisions about safe scale up and due to the magnitude of these heat releases we will show how important it is to control the intended heat of reaction and also the latent crosslinking energy that is liberated should the reaction runaway. Having obtained this data we will then demonstrate by the use of simple calculations what these energies mean for safe scale up strategies and discuss and present options for how this may be achieved based on typical plant set ups utilising options such as traditional jacket or reflux (condenser) control, addition control, temperature and pressure staging. A real life example will also be used to aid this discussion and hopefully this paper will give an appreciation for the challenges faced by phenol formaldehyde resin manufacturers and how various calorimetry techniques are essential in providing an insight into process performance, understanding how to prevent runway reactions and providing the data to necessary to design protective relief systems. Introduction Producing phenolic resin is a very old but still active industry. Von Bayer first reported the polycondensation of phenol with aldehydes in In 192 Blumer had the first industrial process producing shellac from a phenol formaldehyde reaction. Baekeland made the first thermosetting plastic in 199. Today phenolic resins see a wide variety of uses such as ablation (heat shields), abrasives, coatings (can lining), composites, felt-bonding, foams, foundry (casting), friction, laminating (PCB), molding, proppants (fracking), refractory, rubber, substrate saturation (paper) and wood bonding (plywood, particle board). There are two types of phenol formaldehyde resins. When the formaldehyde to phenol ratio is less than 1 a Novolac resin is formed. These resin reactions are acid catalysed, react to completion and the resulting product requires a separate crosslinking agent (typically hexamine) to produce the final resin. A Resole resin is formed when the formaldehyde to phenol ratio is greater than 1 (typically 1 to 3). These reactions are based catalysed and intentionally not reacted to completion. The Resole product carries pendent methylene hydroxy moieties (not stable in acid) that allow the resin to be self-crosslinking at higher temperatures. It is these reactive groups that make the Resole version of this chemistry particularly hazardous due to this latent but elevated temperature activated reactivity. Figure 1: Schematic of Resin Types In this paper we demonstrate the use of Reaction Calorimetry, Differential Scanning Calorimetry (DSC), and Adiabatic Calorimetry to characterise the energies involved in a generic Resole recipe. Our example generic recipe has a formaldehyde to phenol ratio of 2.2 and is 31% wt phenol, 21% water, 4% catalyst (5% aq. sodium hydroxide) with the aldehyde source being 5% aq. formaldehyde (44% wt). Figure 2 shows the normalized (W/kg phenol) heat flux profile for a batch reaction at 5 C of this recipe initiated by a 1 minute addition of the catalyst. Figure 3 shows an expanded plot where the addition of the catalyst is clearly visible. Phenol is a weak acid while 5% sodium hydroxide is a strong base so the formation of sodium phenolate (the active species in the polycondensation) is a rapid and complete reaction. The sloped appearance of the heat flow profile during the catalyst 1
2 (g), (W/kg phenol) ( C), (%) (g), (W/kg phenol) ( C), (%) SYMPOSIUM SERIES NO 16 HAZARDS IChemE addition is due to the growing rate of the polycondensation reaction underlying the addition limited kinetics of the phenolcaustic reaction (square-wave response). The area under the heat flow profile curve represents the total heat of our batch reaction and integrating yields a normalized heat of reaction of -92 kj/kg phenol. Dividing the total heat by the thermal mass (mass x heat capacity) calculates the theoretical temperature rise under adiabatic conditions due to the intended heat of reaction. For this recipe the calculated adiabatic temperature rise was +91 C. Phenol Formaldehyde Batch at 5 C Figure 2: Normalised Profile for Batch Reaction at 5 C Phenol Formaldehyde Batch at 5 C (expanded) Figure 3: Normalised (Expanded) Profile for Batch Reaction at 5 C. So here just from the intended heat of reaction we see a large adiabatic potential, as from 5 C a loss of cooling scenario could result in a temperature rise to 141 C where the vapour pressure of water would be 54 psig. If we take the reaction product from the batch reaction at 5 C and look at it in the DSC we see the scan shown in Figure 4. 2
3 (W/g) (W/g) SYMPOSIUM SERIES NO 16 HAZARDS IChemE.5 Size: 9.1 mg Method: 2 C/min C C C 32.6 J/g Temperature ( C) Figure 4: DSC Of Reaction Product Mixture In the DSC scan we see the latent crosslinking energy from the pendent methylene hydroxy groups in the Resole reaction mass. Taking the integrated energy from the scan, 32.6 J/g, and dividing by the heat capacity of the reaction mass tested (3.1 J/g C) we calculate an additional +98 C adiabatic temperature rise potential. Adding this higher temperature activated energy to our previous intended reaction energy totals a temperature rise +189 C! To confirm that the intended heat of reaction under loss of cooling conditions can raise the temperature of the reaction to a temperature where the latent crosslinking energy can be realized, adiabatic calorimetry is needed. Figure 5 shows the same recipe run in the Fauske VSP2 adiabatic calorimeter. Thermosetting Catalyst add Intended Reaction Figure 5: Adiabatic VSP test Trace on Generic Reaction Mixture In the VSP2 the reaction is initiated by injection of the catalyst at 5 C and proceeds under adiabatic conditions. Indeed the VSP2 trace shows the intended reaction heat does carry the system into the temperature range where the crosslinking reaction occurs and further temperature rise is realized. Though not covered in this paper, the temperature rise rate and pressure rise rate data from such an experiment can be used to design a proper vent size for plant reactor for this process. The information gathered and illustrated by these three instruments definitively shows how important it is to control the intended heat of reaction in this Resole phenol formaldehyde resin process. Not only is there plenty of intended reaction energy to deal with but there is also latent crosslinking energy waiting to be liberated should the reaction runaway. While these reaction are easy to control in a laboratory reaction calorimeter via jacket cooling, to answer the question how easy is it to control with scale we can now look at some simple calculations to show how these thermal challenges offered by the phenol formaldehyde process can be handled with scale. Normally in batch equipment one would rely on jacket cooling to remove the reaction heat and control temperature. If we scale our phenol formaldehyde batch process to 2 kg of phenol and run it in a 12, litre (diameter 2.2 m) the stirred volume for our generic recipe would be 35 litres corresponding to a heat transfer area of 9 m 2 (A). If the tank was glass 3
4 (g), (W/kg phenol) ( C), (%) SYMPOSIUM SERIES NO 16 HAZARDS IChemE lined steel, a typical heat transfer coefficient (U) would be ~3 W/m 2 K. Assuming a maximum temperature difference between the reactor and jacket (ΔT) of 5 C, our maximum cooling capacity would be UAΔT = 3 x 9 x 5 = 135, W. For the 2 kg phenol batch size the normalized cooling capacity is 67.5 W/kg phenol. However, practitioners of phenol formaldehyde processes universally cool their processes through the use of oversized condensers and reflux of water most of the time under various levels of vacuum. Data from an industrial plant showed the cooling capacity of their condenser to be 38.4 K BTU/min. This cooling capacity would be the equivalent of condensing 176 kg water/hr or converting to our current unit of choice, 675,236 W. Normalizing to our 2 kg batch size yields 338 W/kg phenol. Figure 6 shows the expanded plot of our 5 C batch reaction though this time with the normalized cooling capacities for the glass line steel jacketed reactor and that provided by the previously mentioned reflux condenser presented as horizontal dotted lines. Also shown are similar lines for a Hastelloy reactor (U = 5 W/m 2 K), and a stainless steel reactor (U = 1 W/m 2 K). Please note that all the values for the heat transfer coefficient are at the upper end of the performance range for each material of construction. Certainly jacket fouling and choice of heat transfer fluid can affect these assumed U values, as well. 5 Phenol Formaldehyde Batch at 5 C (expanded) Q-Condenser Q-SS Q-Hast Q-GLS Q - GLS Q - Hast. Q - SS Q - Condenser 3 2 Figure 6: Batch at 5 C showing heat flow versus time overlaid with various cooling capacity scenarios One can easily see that jacket cooling in either the glass lined steel reactor or Hastelloy reactor is inadequate as a significant portion of the heat flux profile exceeds the cooling capacity line. One can see that jacket cooling in a stainless steel vessel is close to having enough cooling capacity and possibly with a slightly longer catalyst addition it may well have been enough. Even with cooling by reflux the cooling capacity line is just shy of completely surpassing the peak heat rate of this batch process. So what other options are available for scale up of these types of processes? If one is fortunate enough to have aqueous formaldehyde as the aldehyde source then running the process semi-batch with a controlled addition of formaldehyde will help. Figure 7 shows an expanded plot of a semi-batch version of our generic phenol formaldehyde recipe. Here the initial rate corresponded to a 4 hour addition of 37% aq. formaldehyde to the precharged phenol, water and catalyst. 4
5 True (W/kg), Reaction Mass (kg) Tr ( C), (%) (W/kg phenol), Formaldehyde Add (g) ( C), (%) SYMPOSIUM SERIES NO 16 HAZARDS IChemE Phenol Formaldehyde Semi-Batch - Formaldehyde Addition 7 C (expanded) Q-Condenser Q-SS Q-Hast Q-GLS 35 1 Dosing Mass Formaldehyde Dosing Mass Q - GLS Q - Hast Q - SS Q - Condenser Figure 7 :Semi- Batch plot for generic recipe After 3 minutes the addition rate was doubled then the addition rate increased again to three times the original rate then slowed to 1.5 times the original rate through the end of the addition. One can see addition limited kinetics (square-wave pattern) for the initial addition rate and double that rate but accumulation begins when the original rate was tripled. More important is to notice that the controlled addition of formaldehyde, at least at the initial 4 hour rate, brings the stainless steel, Hastelloy and even the glass lined steel reactor jacket cooling into play. Reflux cooling provides plenty of cooling capacity margin for the semi-batch process. But not all phenol formaldehyde recipes use aqueous formaldehyde as the aldehyde source thus allowing for semi-batch operation, and there is no guarantee that the semi-batch process makes the same material as its batch counterpart. Also water is a necessary burden in phenol formaldehyde processing. While it is convenient to have during the main reaction, before end use water will be stripped off to concentrate the resin before final thermosetting. This costs cycle time and generates waste needing disposal. One answer to using less water is to use paraformaldehyde, a polymer of formaldehyde which is a solid thus avoiding the water that comes along with using aq. formaldehyde. Being a solid though, paraformaldehyde is batch loaded. Figure 8 shows a different recipe where the paraformaldehyde is present in a ~2:1 ratio versus aqueous formaldehyde, more phenol and overall less water than our generic recipe. This run was carried out batch at 7 C with a ten minute catalyst addition. Batch at 7 C Q-Condenser True Q - Condenser (2K kg) 2 2 Figure 8: Reaction using paraformaldehyde at 7 C 5
6 (W/kg Phenol) Reaction Temperature ( C), (%) SYMPOSIUM SERIES NO 16 HAZARDS IChemE For comparative purposes this recipe has a normalized heat of reaction of -943 kj/kg phenol and an adiabatic temperature rise of +143 C. Also shown on the plot is the 338 W/kg phenol reflux cooling capacity line and we can clearly see that this recipe could not be safely run, in this manner, at the 2 kg scale. So how might you scale a specific recipe that does not lend itself to controlled addition of one of the components? Staging of temperature, catalyst and even vacuum can be done to help keep the rate in check. Figure 9 shows an actual plant process whereby the temperature and catalyst addition is staged. Plant Mimic Run, 37 C to 67 C, Catalyst Add in Thirds Q-Condenser (1x) ZXReactor Temperature Q-Condenser (3.2 x) Experiment Time (hr.) Q-Condenser (1X) Q - Condenser (3.2X) Tr % Conv. Figure 9: Laboratory Run of Actual Plant Process To mimic the plant process a background temperature ramp was performed adding the catalyst in thirds at appropriate times corresponding to the points where they establish and confirm temperature control. The three vertical spikes are the catalyst addition points and were done so in the lab much faster than the actual catalyst would be added in the plant. Notice the initial endotherm at the start where there is significant undissolved paraformaldehyde going into solution with reaction which helps offset exothermic reaction heat at the lower temperatures. By the time the last third of the catalyst is added 35% of the reaction has been completed and throughout the entire process reflux cooling is more than adequate, at least for the current batch-size (1X). Also shown is the normalized cooling capacity line if this recipe were to be scaled up by a factor of 3.2 (3.2X). Here you can see that by the second catalyst addition the reaction rate exceeds the 3.2X condenser cooling capacity. Based on this data it was decided not to scale this process up to the larger batch size. Possible changes to enable safe plant scale up, include controlled addition of the aqueous formaldehyde portion of the recipe and/or switching out some or all of the paraformaldehyde for aqueous formaldehyde, provided equivalent material can be made with the new recipe. Summary In summary we hope this paper has given an appreciation for the challenges faced by phenol formaldehyde resin manufacturers. In particular, that reaction calorimetry provides a vital window into process performance and helps gather the data necessary to understand how to prevent a runaway reaction together with simple heat rate scale up calculations. Thermal screening and adiabatic calorimetry are key to understanding the total upset scenario and provides the data necessary to design a relief system to protect the vessel in case of runaway. 6
THE USE OF DEWAR CALORIMETRY IN THE ASSESSMENT OF CHEMICAL REACTION HAZARDS
THE USE OF DEWAR CALORIMETRY IN THE ASSESSMENT OF CHEMICAL REACTION HAZARDS R.L. ROGERS* Dewar Calorimetry is one of the simplest and most useful techniques used in the assessment of chemical reaction
More informationIMPROVED ADIABATIC CALORIMETRY IN THE PHI-TEC APPARATUS USING AUTOMATED ON-LINE HEAT LOSS COMPENSATION
# 27 IChemE IMPROVED ADIABATIC CALORIMETRY IN THE PHI-TEC APPARATUS USING AUTOMATED ON-LINE HEAT LOSS COMPENSATION B Kubascikova, D.G. Tee and S.P. Waldram HEL Ltd, 5 Moxon Street, Barnet, Hertfordshire,
More informationA COMPARISON OF DSC AND RADEX FOR THE INVESTIGATION OF SAFETY PARAMETERS FOR INHOMOGENEOUS SYSTEMS
A COMPARISON OF DSC AND RADEX FOR THE INVESTIGATION OF SAFETY PARAMETERS FOR INHOMOGENEOUS SYSTEMS Markus Luginbuehl 1 and Ian Priestley 2 1 Syngenta Crop Protection, Switzerland; Tel: þ41 62 8685464,
More informationTHE VERSATILE VSP2: A TOOL FOR ADIABATIC THERMAL ANALYSIS AND VENT SIZING APPLICATIONS
THE VERSATILE VSP2: A TOOL FOR ADIABATIC THERMAL ANALYSIS AND VENT SIZING APPLICATIONS Charles F. Askonas, Dr. James P. Burelbach, and Dr. Joseph C. Leung Fauske and Associates, Inc. 16W070 W. 83 rd Street
More informationRUNAWAY REACTIONS Experimental Characterization and Vent Sizing
RUNAWAY REACTIONS Experimental Characterization and Vent Sizing Ron Darby Professor of Chemical Engineering Texas A&M University College Station, TX 77843-3122 (979) 845-3301 r-darby@tamu.edu ARSST CALORIMETER
More informationReaction Calorimetry as a Tool for Thermal Risk Assessment and Improvement of Safe Scalable Chemical Processes
Reaction Calorimetry as a Tool for Thermal Risk Assessment and Improvement of Safe Scalable Chemical Processes Kamala Jyotsna G, Sindhanur Srikanth, Vinay Ratnaparkhi, and Rakeshwar Bandichhora * Research
More informationROBUST CHEMICAL REACTIVITY PROGRAM PREVENTS POTENTIAL TANK EXPLOSION
ROBUST CHEMICAL REACTIVITY PROGRAM PREVENTS POTENTIAL TANK EXPLOSION John C. Wincek, CSP, Croda, Inc., USA A 41.6 m 3 storage tank and connected gauge tank last used to store dimethyl sulfate (DMS), was
More informationFIRE PROTECTION MEASURES FOR VESSELS CONTAINING REACTIVE CHEMICALS
FIRE PROTECTION MEASURES FOR VESSELS CONTAINING REACTIVE CHEMICALS J A Hare 1,3, L Cusco 1, D C Kerr 1 and M D Bishopp 2 1 Health and Safety Laboratory, Process Safety Section 2 Health and Safety Executive,
More informationEffect of curing time on phenolic resins using latent acid catalyst
International Journal of ChemTech Research CODEN (USA): IJCRGG ISSN: 0974-4290 Vol.9, No.01 pp 30-37, 2016 Effect of curing time on phenolic resins using latent acid catalyst G.N.Manikandan*, K.Bogeshwaran
More informationCalorimetry Guide. Safety by Design What do we Learn from Reaction Calorimetry?
Calorimetry Guide What do we Learn from Reaction Calorimetry? Developing new compounds and transferring them to manufacturing requires an understanding of the chemical route, process and all its parameters.
More informationAn Alternative Way to Determine the Self-Accelerating Decomposition Temperature by Using the Adiabatic Heat- Pressure Accumulation Test
139 A publication of CHEMICAL ENGINEERING TRANSACTIONS VOL. 48, 2016 Guest Editors: Eddy de Rademaeker, Peter Schmelzer Copyright 2016, AIDIC Servizi S.r.l., ISBN 978-88-95608-39-6; ISSN 2283-9216 The
More informationVISIMIX TURBULENT. TACKLING SAFETY PROBLEMS OF STIRRED REACTORS AT THE DESIGN STAGE.
VISIMIX TURBULENT. TACKLING SAFETY PROBLEMS OF STIRRED REACTORS AT THE DESIGN STAGE. This example demonstrates usage of the VisiMix software to provide an Inherently Safer Design of the process based on
More informationInvestigation of adiabatic batch reactor
Investigation of adiabatic batch reactor Introduction The theory of chemical reactors is summarized in instructions to Investigation of chemical reactors. If a reactor operates adiabatically then no heat
More informationChemical Reaction Engineering Prof. JayantModak Department of Chemical Engineering Indian Institute of Science, Bangalore
Chemical Reaction Engineering Prof. JayantModak Department of Chemical Engineering Indian Institute of Science, Bangalore Module No. #05 Lecture No. #29 Non Isothermal Reactor Operation Let us continue
More informationAGrignard reaction, in which a reactant, A, is coupled with phenyl magnesium chloride, is used to
DEVELOPMENT OF AN EFFICIENT AND SAFE PROCESS FOR A GRIGNARD REACTION VIA REACTION CALORIMETRY H. Ferguson and Y. M. Puga The Dow Chemical Co., Inc. Engineering Sciences/Market Development A paper from
More informationAn Introduction to Reaction Calorimetry
An Introduction to Reaction Calorimetry Syrris A brief history Driven by Productizing Science Founded in 2001 to address the challenges faced by the pharmaceutical industry Syrris is the longest established
More informationIncorporation of Reaction Chemicals Testing Data in Reactivity Hazard Evaluation. Ken First Dow Chemical Company Midland, MI
Incorporation of Reaction Chemicals Testing Data in Reactivity Hazard Evaluation Ken First Dow Chemical Company Midland, MI Reactivity Hazard Screening Evaluation Evaluation of reactivity hazards involves
More informationDR JASBIR SINGH Hazard Evaluation Laboratory Limited, Borehamwood, Herts, England
SAFE DISPOSAL OF REACTIVE CHEMICALS FOLLOWING EMERGENCY VENTING DR JASBIR SINGH Hazard Evaluation Laboratory Limited, Borehamwood, Herts, England This paper will discuss the technical issues that must
More informationDrum Burst due to Runaway Reaction and the Limits of MOC
805 A publication of CHEMICAL ENGINEERING TRANSACTIONS VOL. 48, 2016 Guest Editors: Eddy de Rademaeker, Peter Schmelzer Copyright 2016, AIDIC Servizi S.r.l., ISBN 978-88-95608-39-6; ISSN 2283-9216 The
More informationThermochemistry: Calorimetry and Hess s Law
Thermochemistry: Calorimetry and Hess s Law Some chemical reactions are endothermic and proceed with absorption of heat while others are exothermic and proceed with an evolution of heat. The magnitude
More informationWORKBOOK FOR CHEMICAL REACTOR RELIEF SYSTEM SIZING ANNEX 10 NOMENCLATURE A cross-sectional flow area of relief system (m 2 ) A actual actual cross-sectional area of safety valve nozzle (m 2 ) A approx
More informationThermal Safety Software (TSS) series
Thermal Safety Software (TSS) series the analog-free methodology and software for reaction hazard assessment of Chemical Processes and Products. TSS is the integrated system which covers the entire spectrum
More informationExperiment 14 - Heats of Reactions
Experiment 14 - Heats of Reactions If a chemical reaction is carried out inside a calorimeter, the heat evolved or absorbed by the reaction can be determined. A calorimeter is an insulated container, and
More informationCHAPTER 4 THERMAL HAZARD ASSESSMENT OF FIREWORKS MIXTURE USING ACCELERATING RATE CALORIMETER (ARC)
68 CHAPTER 4 THERMAL HAZARD ASSESSMENT OF FIREWORKS MIXTURE USING ACCELERATING RATE CALORIMETER (ARC) 4.1 INTRODUCTION Accelerating Rate Calorimeter (ARC) is one of the versatile experimental tools available
More informationnot to be republished NCERT MOST of the reactions are carried out at atmospheric pressure, hence THERMOCHEMICAL MEASUREMENT UNIT-3
UNIT-3 THERMOCHEMICAL MEASUREMENT MOST of the reactions are carried out at atmospheric pressure, hence heat changes noted for these reactions are enthalpy changes. Enthalpy changes are directly related
More informationSynergy of the combined application of thermal analysis and rheology in monitoring and characterizing changing processes in materials
Synergy of the combined application of thermal analysis and rheology in monitoring and characterizing changing processes in materials by A. Franck, W. Kunze, TA Instruments Germany Keywordss: synergy,
More informationThermochemistry. Chapter Energy Storage and Reference. 4.2 Chemical Rxns. 4.3 Hess s law Overview
Chapter 4 Thermochemistry 4.1 Energy Storage and Reference Thermochemistry is the study of the energy released when the atomic-level associations are changed. A chemical reaction (rxn) is one where these
More informationMOST of the reactions are carried out at atmospheric pressure, hence
MOST of the reactions are carried out at atmospheric pressure, hence heat changes noted for these reactions are enthalpy changes. Enthalpy changes are directly related to the temperature changes by the
More informationOptimization of a Nitration Reaction
CBC-PROCOS S.p.A. - Research and Development Laboratory - Calorimetry Optimization of a Nitration Reaction Alessandro Barozza*, Paolo Paissoni, Jacopo Roletto barozza@procos.it Giornata di Studio sullo
More informationThermochemistry. Chapter Energy Storage and Reference. 4.2 Chemical Rxns. 4.3 Hess s law Overview
Chapter 4 Thermochemistry 4.1 Energy Storage and Reference Thermochemistry is the study of the energy released when the atomic-level associations are changed. A chemical reaction (rxn) is one where these
More informationCoflore Agitated Cell Reactor
Coflore Agitated Cell Reactor Coflore ACR The Coflore ACR is a lab flow reactor developed by AM Technology for studying chemistry in flow and developing scalable continuous processes. Its flexible design
More informationExperiment #12. Enthalpy of Neutralization
Experiment #12. Enthalpy of Neutralization Introduction In the course of most physical processes and chemical reactions there is a change in energy. In chemistry what is normally measured is ΔH (enthalpy
More informationChemical Reaction Engineering Prof. Jayant Modak Department of Chemical Engineering Indian Institute of Science, Bangalore
Chemical Reaction Engineering Prof. Jayant Modak Department of Chemical Engineering Indian Institute of Science, Bangalore Lecture No. #40 Problem solving: Reactor Design Friends, this is our last session
More informationApplications of the Micro Reaction Calorimeter
Applications of the Micro Reaction Calorimeter Power-compensation method. Versatility Automated sample addition, repeated or timed. Wide temperature range Pressure measurement Stirring Highly sensitive
More informationcalorimeter heat flow calorimetry, power compensation calorimetry
calorimeter heat flow calorimetry, power compensation calorimetry Atlas simply does it all What is the Atlas Reaction Calorimeter? The Atlas Reaction Calorimeter accurately measures the power and enthalpy
More informationTHE FUTURE OF THE CHEMISTRY: CONTINUOUS FLOW REACTIONS BASEL 2016
THE FUTURE OF THE CHEMISTRY: CONTINUOUS FLOW REACTIONS BASEL 2016 CHEMICAL PLANT CONTINUOUS FLOW REACTOR The continuous flow reactor is a safe system, running chemical reactions in reduced volume with
More informationThe THT micro reaction calorimeter μrc
The THT micro reaction calorimeter μrc Titration calorimetry isothermal calorimetry and scanning calorimetry - all in one instrument CHEMICAL APPLICATIONS BROCHURE Introduction and reaction kinetics The
More informationThe THT micro reaction calorimeter RC
The THT micro reaction calorimeter RC Titration calorimetry isothermal calorimetry and scanning calorimetry - all in one instrument C H E M I C A L A P P L I C A T I O N S B R O C H U R E Introduction
More informationHow to Use Kinetic Modeling Analysis To Predict Profile Part Failure
Tips and Techniques Reprinted From: PLASTICS TECHNOLOGY Magazine How to Use Kinetic Modeling Analysis To Predict Profile Part Failure Real-world project demonstrates how kinetic modeling can help estimate
More informationLecture (9) Reactor Sizing. Figure (1). Information needed to predict what a reactor can do.
Lecture (9) Reactor Sizing 1.Introduction Chemical kinetics is the study of chemical reaction rates and reaction mechanisms. The study of chemical reaction engineering (CRE) combines the study of chemical
More informationMultiMax Application Note
MultiMax Application Note Investigation of an Imine Formation 1. Introduction Today s Research and Development world demands faster results to be able to deliver more products on time. Automation techniques
More informationPilot Plant Reactive Chemistry Incidents: Case Studies and Prevention
Pilot Plant Reactive Chemistry Incidents: Case Studies and Prevention Dennis C. Hendershot Albert I. Ness Rohm and Haas Company Engineering Division Croydon, PA, USA For presentation at the American Institute
More informationTECHNICAL UPDATE. Ricon Resins Peroxide Curing Data and Use as a Reactive Plasticizer in Polyphenylene Ether Based CCL and PWB
TARGET MARKETS/ APPLICATIONS Copper clad laminate (CCL) and printed wiring [Circuit] boards (PWB) Structural composites Radomes Aerospace applications ADDITIONAL INFO SDS /TDS: Ricon 100, 154, 157, 184,
More informationIntroduction 1. DSC scan 5-bromo-2-aminopyridine..3. DSC scan 5-bromo-2-nitropyridine...4
SUPPORTING INFORMATION Introduction 1 DSC scan 5-bromo-2-aminopyridine..3 DSC scan 5-bromo-2-nitropyridine.....4 Oxidant mixture. Adiabatic test stability, glass cell and Hastelloy C22 test cell 5 Hastelloy
More informationMicro Reaction Calorimeter
C3 Prozess- und Analysentechnik GmbH Produktinformation µrc Micro Reaction Calorimeter Tel. (089) 45 60 06 70 info@c3-analysentechnik.de www.c3-analysentechnik.de The THT micro reaction calorimeter µrc
More informationTHE SOLVENT EFFECTS ON GRIGNARD REACTION
THE SOLVENT EFFECTS ON GRIGNARD REACTION Mieko Kumasaki, Takaaki Mizutani, and Yasuhiro Fujimoto National Institute of Occupational Safety and Health, 1-4-6, Umezono, Kiyose, Tokyo, 204-0024, Japan; e-mail:
More information4 th Edition Chapter 9
Insert Page 547A 4 th Edition Chapter 9 In summary, if any one of the following three things had not occurred the explosion would not have happened. 1. Tripled production 2. Heat exchanger failure for
More informationI. CHEM. E. SYMPOSIUM SERIES NO. 68
ADIABATIC CALORIMETRY AND SIKAREX TECHNIQUE L. Hub* The suitability of adiabatic calorimetry for safety investigations, the specific requirements on the experimental set-up and the problems of correct
More informationThe Integration of Process Safety into a Chemical Reaction Engineering Course: Kinetic Modeling of the T2 Incident
The Integration of Process Safety into a Chemical Reaction Engineering Course: Kinetic Modeling of the T2 Incident Ronald J. Willey, a H. Scott Fogler b, and Michael B. Cutlip c a Department of Chemical
More informationTHE STORAGE, HANDLING AND PROCESSING OF DANGEROUS SUBSTANCES
THE STORAGE, HANDLING AND PROCESSING OF DANGEROUS SUBSTANCES LEARNING OUTCOMES On completion of this element, you should be able to demonstrate understanding of the content through the application of knowledge
More informationDevelopment of an organometallic flow chemistry. reaction at pilot plant scale for the manufacture of
Supporting Information Development of an organometallic flow chemistry reaction at pilot plant scale for the manufacture of verubecestat David A. Thaisrivongs*, John R. Naber*, Nicholas J. Rogus, and Glenn
More informationINCIDENT DURING NITRATION IN A BATCH REACTOR. K DIXON-JACKSON C.CHEM MRSC MSc*
INCIDENT DURING NITRATION IN A BATCH REACTOR K DIXON-JACKSON C.CHEM MRSC MSc* During routine production of a nitro diazo species a serious thermal incident occurred. Due to agitation stoppage a slow deflagration
More informationgskin Application Note: Calorimetry
1 / 7 gskin Application Note: Calorimetry Direct and precise calorimetric measurements with the gskin Sensor The gskin Heat Flux Sensor enables direct and highly precise measurements of reaction enthalpies
More informationThe Essential Elements of a Successful Reactive Chemicals Program
A publication of CHEMICAL ENGINEERING TRANSACTIONS VOL. 26, 2012 Guest Editors: Valerio Cozzani, Eddy De Rademaeker Copyright 2012, AIDIC Servizi S.r.l., ISBN 978-88-95608-17-4; ISSN 1974-9791 The Italian
More informationAnalysis of Synthesis of General-Purpose Phenolic Resin and Its Curing Mechanism
Advances in Petroleum Exploration and Development Vol. 10, No. 2, 2015, pp. 135-139 DOI:10.3968/8047 ISSN 1925-542X [Print] ISSN 1925-5438 [Online] www.cscanada.net www.cscanada.org Analysis of Synthesis
More informationTypes of Chemical Reactors. Nasir Hussain Production and Operations Engineer PARCO Oil Refinery
Types of Chemical Reactors Nasir Hussain Production and Operations Engineer PARCO Oil Refinery Introduction Reactor is the heart of Chemical Process. A vessel designed to contain chemical reactions is
More informationCHEMICAL REACTION ENGINEERING LAB
CHEMICAL REACTION ENGINEERING LAB EQUIPMENTS 1.CHEMICAL REACTORS SERVICE UNIT The chemical reactors service unit consists of a moulded ABS plinth which is used as a mounting for the chemical reactor to
More informationPRODUCTION OF URANOUS NITRATE WITH HYDRAZINE NITRATE AS REDUCING AGENT IN PRESENCE OF ADAMS CATALYST FOR URANIUM RECONVERSION PURPOSES
PRODUCTION OF URANOUS NITRATE WITH HYDRAZINE NITRATE AS REDUCING AGENT IN PRESENCE OF ADAMS CATALYST FOR URANIUM RECONVERSION PURPOSES Abstract: K.S. Rao, K Kumaraguru & P.M. Gandhi. Fuel Reprocessing
More informationLABOTRON EXTRACTION & SYNTHESIS 2450 MHz
LABOTRON EXTRACTION & SYNTHESIS 2450 MHz The LABOTRON TM series is the generic name for a ground breaking range of integrated reactor and microwave transmission systems especially designed to carry out
More informationStructure of the chemical industry
CEE-Lectures on Industrial Chemistry Lecture 1. Crystallization as an example of an industrial process (ex. of Ind. Inorg. Chemistry) Fundamentals (solubility (thermodynamics), kinetics, principle) Process
More informationHeat Transfer in Polymers
Industrial Advisory Group Heat Transfer in Polymers Chris Brown Date: October 16 th 2003 Introduction: why heat transfer in polymers? To help enhance productivity Faster heat transfer means better equipment
More informationWorking with Hazardous Chemicals
A Publication of Reliable Methods for the Preparation of Organic Compounds Working with Hazardous Chemicals The procedures in Organic Syntheses are intended for use only by persons with proper training
More informationCOMBUSTION OF FUEL 12:57:42
COMBUSTION OF FUEL The burning of fuel in presence of air is known as combustion. It is a chemical reaction taking place between fuel and oxygen at temperature above ignition temperature. Heat is released
More informationAPPLICATIONS OF THERMAL ANALYSIS IN POLYMER AND COMPOSITES CHARACTERIZATION. Wei Xie TA Instruments
APPLICATIONS OF THERMAL ANALYSIS IN POLYMER AND COMPOSITES CHARACTERIZATION Wei Xie TA Instruments Abstract Thermal Analysis is the generic name for a series of measurement techniques traditionally used
More informationMonitoring Emulsion Polymerization by Raman Spectroscopy
An Executive Summary Monitoring Emulsion Polymerization by Raman Spectroscopy Why process analytical matters to process development R&D. Serena Stephenson, PhD Senior R&D Analytical Manager Kishori Deshpande,
More informationHess' Law: Calorimetry
Exercise 9 Page 1 Illinois Central College CHEMISTRY 130 Name: Hess' Law: Calorimetry Objectives The objectives of this experiment are to... - measure the heats of reaction for two chemical reactions.
More informationJust a reminder that everything you do related to lab should be entered directly into your lab notebook. Calorimetry
Just a reminder that everything you do related to lab should be entered directly into your lab notebook. Objectives: Calorimetry After completing this lab, you should be able to: - Assemble items of common
More information3.2 Calorimetry and Enthalpy
3.2 Calorimetry and Enthalpy Heat Capacity Specific heat capacity (c) is the quantity of thermal energy required to raise the temperature of 1 g of a substance by 1 C. The SI units for specific heat capacity
More informationReal-Time Feasibility of Nonlinear Predictive Control for Semi-batch Reactors
European Symposium on Computer Arded Aided Process Engineering 15 L. Puigjaner and A. Espuña (Editors) 2005 Elsevier Science B.V. All rights reserved. Real-Time Feasibility of Nonlinear Predictive Control
More informationEXPERIMENT 9 ENTHALPY OF REACTION HESS S LAW
EXPERIMENT 9 ENTHALPY OF REACTION HESS S LAW INTRODUCTION Chemical changes are generally accompanied by energy changes; energy is absorbed or evolved, usually as heat. Breaking chemical bonds in reactants
More informationKinetics and Safety Analysis of Peracetic Acid
559 A publication of CHEMICAL ENGINEERING TRANSACTIONS VOL. 48, 216 Guest Editors: Eddy de Rademaeker, Peter Schmelzer Copyright 216, AIDIC Servizi S.r.l., ISBN 978-88-9568-39-6; ISSN 2283-9216 The Italian
More informationTEPZZ Z 4A_T EP A1 (19) (11) EP A1 (12) EUROPEAN PATENT APPLICATION. (43) Date of publication: Bulletin 2017/35
(19) TEPZZ Z 4A_T (11) EP 3 211 024 A1 (12) EUROPEAN PATENT APPLICATION (43) Date of publication:.08.17 Bulletin 17/3 (21) Application number: 171768.0 (22) Date of filing: 28.03.13 (1) Int Cl.: C08H 7/00
More informationHigh Pressure Chemistry. Hydrogenation & Catalysis Tools.
High Pressure Chemistry Hydrogenation & Catalysis Tools www.helgroup.com HYDROGENATION AND CATALYSIS Product Selection Guide HEL Group s top quality high pressure reactors and systems offer innovative,
More informationCHEMISTRY 135 General Chemistry II. Energy of Phase Changes [1]
CHEMISTRY 135 General Chemistry II Energy of Phase Changes [1] Water at its triple point, where 3 phases coexist, looks unfamiliar a bit like boiling water and ice. [2] Coexistence of two phases, such
More informationICHEME SYMPOSIUM SERIES NO Zeneca Specialties, P.O. Box 42, Hexagon House, Blackley, Manchester, M9 8ZS
ABNORMAL OCCURRENCE: IRON REDUCTION PJ DUGGAN Zeneca Specialties, P.O. Box 42, Hexagon House, Blackley, Manchester, M9 8ZS An abnormal occurrence during a telescoped iron reduction resulted in over-pressurisation
More informationVOCs Emissions and Structural Changes of Polypropylene During Multiple Melt Processing
VOCs Emissions and Structural Changes of Polypropylene During Multiple Melt Processing Q. Xiang, M. Xanthos*, S. Mitra and S. H. Patel* Department of Chemical Engineering, Chemistry and Environmental Science
More informationDevelopment and validation of a simple and cost effective procedure for scaling-up hazardous chemical processes
Development and validation of a simple and cost effective procedure for scaling-up hazardous chemical processes Copelli S., Maestri F., Rota R. Politecnico di Milano - Dipartimento di Chimica, Materiali
More informationRedox for Main Polymerization of
AS SEEN IN Paint Coatings Industry Globally Serving Liquid and Powder Manufacturers and Formulators Redox for Main Polymerization of Emulsion Polymers By Paul Fithian and Mike O Shaughnessy, BruggemanChemical
More informationAt approximately 10:42 a.m. on. Under a 1997 Memorandum of. Columbus, Ohio Sept. 10, Accident Investigation CASE STUDY
United States Environmental Protection Agency Office of Solid Waste and Emergency Response (5104) HOW TO PREVENT RUNAWAY REACTIONS EPA 550-F99-004 August 1999 www.epa.gov/ceppo/ CASE STUDY: PHENOL-FORMALDEHYDE
More informationChemistry CP Lab: Additivity of Heats of Reaction (Hess Law)
Chemistry CP Lab: Additivity of Heats of Reaction (Hess Law) Name: Date: The formation or destruction of chemical bonds is always accompanied by an energy exchange between the reactant molecules and the
More informationRelease Liners: The Most Important Trash You ll Ever Buy. by Charles Sheeran
Release Liners: The Most Important Trash You ll Ever Buy. by Charles Sheeran MPI Release 37 East Street, Winchester, MA 01890 Phone: 888-MPI-8088 Fax: 781-729-9093 www.mpirelease.com Abstract If you ve
More informationThermal Hazard Analysis of Methyl Ethyl Ketone Peroxide
Thermal Hazard Analysis of Methyl Ethyl Ketone Peroxide Ron-Hsin Chang, Chi-Min Shu and Po-Yin Yeh Process Safety and Disaster Prevention Laboratory, Department of Environmental and Safety Engineering,
More informationLecture 25: Manufacture of Maleic Anhydride and DDT
Lecture 25: Manufacture of Maleic Anhydride and DDT 25.1 Introduction - In this last lecture for the petrochemicals module, we demonstrate the process technology for Maleic anhydride and DDT. - Maleic
More informationSupporting Information. Flow Grignard and Lithiation: Screening Tools and Development of Continuous Processes
for: Flow Grignard and Lithiation: Screening Tools and Development of Continuous Processes for a Benzyl Alcohol Starting Material Michael E. Kopach, *, Kevin P. Cole, Patrick M. Pollock, Martin D. Johnson,
More informationExperiment 15: Exploring the World of Polymers
1 Experiment 15: Exploring the World of Polymers bjective: In this experiment, you will explore a class of chemical compounds known as polymers. You will synthesize and modify polymers, test their properties
More informationHeat. Heat Terminology 04/12/2017. System Definitions. System Definitions
System Definitions Heat Physical Science 20 Ms. Hayduk Heat Terminology System: the part of the universe being studied (big Earth, or small one atom) Surroundings: the part of the universe outside the
More informationADDITIONAL RESOURCES. Duration of resource: 21 Minutes. Year of Production: Stock code: VEA12052
ADDITIONAL RESOURCES Chemical changes occur around us, and inside us, all the time. When chemical reactions happen, one or more new substances are formed and energy is either given off or absorbed in the
More informationSpecific Heat. Power Supply Beaker Beam Balance Conecting wires ice. Assembly
Specific Heat Objectives a. To measure the specific heat capacity of water b. To measure the specific heat capacity of aluminium c. To measure the heat of fusion of ice (Optional) Apparatus Required Power
More informationSpecific Heat. Power Supply Beaker Beam Balance Conecting wires ice. Assembly
Specific Heat Objectives a. To measure the specific heat capacity of water b. To measure the specific heat capacity of aluminium c. To measure the heat of fusion of ice (Optional) Apparatus Required Power
More informationAppendix to Section 3: Space Shuttle Tile Thermal Protection System. MAE 5420 Compressible Fluids 1
Appendix to Section 3: Space Shuttle Tile Thermal Protection System 1 Temperature Versus Heat (1) Often the concepts of heat and temperature are thought to be the same, but they are not. Temperature is
More informationExpt 10: Friedel-Crafts Alkylation of p-xylene
Expt 10: Friedel-Crafts Alkylation of p-xylene INTRODUCTION The Friedel-Crafts alkylation reaction is one of the most useful methods for adding alkyl substituents to an aromatic ring. Mechanistically,
More informationProcess Safety. Process Safety and Hazard Assessment Avoiding Incidents in the Lab and in the Plant
Process Safety Process Safety and Hazard Assessment Avoiding Incidents in the Lab and in the Plant Process Safety Process Safety and Hazard Assessment From Early Development to Manufacturing The importance
More informationThermal Decomposition Behavior of di-tert-butyl Peroxide Measured with Differential Adiabatic Calorimeter
835 A publication of VOL. 31, 213 CHEMICAL ENGINEERING TRANSACTIONS Guest Editors: Eddy De Rademaeker, Bruno Fabiano, Simberto Senni Buratti Copyright 213, AIDIC Servizi S.r.l., ISBN 978-88-9568-22-8;
More informationLiquid Polybutadienes and Derivatives
Liquid Polybutadienes and Derivatives Coatings & Colorants Product Range Our polyoils and derivatives are stereospecific, lowviscosity and unsaponifiable liquid polybutadienes having a high 1.4-cis double
More informationEnfield Public Schools. Advanced (AP/UCONN) Chemistry (0297) Curriculum Writers: Patrick Smith William Schultz
Enfield Public Schools Advanced (AP/UCONN) Chemistry (0297) Curriculum Writers: Patrick Smith William Schultz November 2007 Lab Safety 1. Basic safety rules must be followed in the Advanced Chemistry laboratory.
More informationFreezing point depression (Item No.: P )
Freezing point depression (Item No.: P3021101) Curricular Relevance Area of Expertise: Chemistry Education Level: University Topic: General Chemistry Subtopic: Solutions and Mixtures Experiment: Freezing
More informationExperiment 7 Can You Slow It Down?
Experiment 7 Can You Slow It Down? OUTCOMES After completing this experiment, the student should be able to: tell which factors influence the reaction rate and how they influence the rate. change the temperature
More informationCHEMISTRY Scientific Inquiry
Chemistry Overview The standards for chemistry establish scientific inquiry skills and core content for all chemistry courses in South Carolina schools. In chemistry, students acquire a fundamental knowledge
More informationAP Chemistry Lab #10- Hand Warmer Design Challenge (Big Idea 5) Figure 1
www.pedersenscience.com AP Chemistry Lab #10- Hand Warmer Design Challenge (Big Idea 5) 5.A.2: The process of kinetic energy transfer at the particulate scale is referred to in this course as heat transfer,
More informationPLANNING PROTECTION MEASURES AGAINST RUNAWAY REACTIONS USING CRITICALITY CLASSES
PLANNING PROTECTION MEASURES AGAINST RUNAWAY REACTIONS USING CRITICALITY CLASSES Francis Stoessel Swiss Institute for the Promotion of Safety & Security, Schwarzwaldallee 215; WRO-1093.3.35, CH-4002 Basel;
More information