H - Acid Caustic Fusion Stage

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Information about H - Acid Caustic Fusion Stage
Technology

Published on March 11, 2014

Author: GerardBHawkins

Source: slideshare.net

Description

H - Acid Caustic Fusion Stage
CONTENTS
0 INTRODUCTION
1 DESIGN INFORMATION
1.1 Reactor Type
1.2 Temperature Range
1.3 Pressure Range
1.4 Chemical System
2 BACKGROUND
3 KINETICS AND MECHANISM
4 MAXIMUM YIELD AND IMPLICATIONS FOR REACTOR DESIGN
5 USE OF DESIGN MODEL FOR START-UP AND MANUFACTURING MONITORING
6 BIBLIOGRAPHY
FIGURES
1 FUSION MODEL OUTLINE MECHANISM AND KINETIC SCHEME
2 TEST RUN OPTIMIZATION OF HEATING TIME 3600 kg/h STEAM

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com GBH Enterprises, Ltd. Process Engineering Guide: GBHE-PEG-RXT-813 H - Acid Caustic Fusion Stage Process Disclaimer Information contained in this publication or as otherwise supplied to Users is believed to be accurate and correct at time of going to press, and is given in good faith, but it is for the User to satisfy itself of the suitability of the information for its own particular purpose. GBHE gives no warranty as to the fitness of this information for any particular purpose and any implied warranty or condition (statutory or otherwise) is excluded except to the extent that exclusion is prevented by law. GBHE accepts no liability resulting from reliance on this information. Freedom under Patent, Copyright and Designs cannot be assumed.

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com Process Engineering Guide: H - Acid Caustic Fusion Stage CONTENTS 0 INTRODUCTION 1 DESIGN INFORMATION 1.1 Reactor Type 1.2 Temperature Range 1.3 Pressure Range 1.4 Chemical System 2 BACKGROUND 3 KINETICS AND MECHANISM 4 MAXIMUM YIELD AND IMPLICATIONS FOR REACTOR DESIGN 5 USE OF DESIGN MODEL FOR START-UP AND MANUFACTURING MONITORING 6 BIBLIOGRAPHY FIGURES 1 FUSION MODEL OUTLINE MECHANISM AND KINETIC SCHEME 2 TEST RUN OPTIMISATION OF HEATING TIME 3600 kg/h STEAM

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 0 INTRODUCTION This document supersedes previous GBHE Report; Process Engineering Design Guide GBHE-PEG-RXT-818. 1 DESIGN INFORMATION 1.1 Reactor Type Batch autoclave, optimized heating/cooling cycle. 1.2 Temperature Range 120°C to approximately 220°C. 1.3 Pressure Range 1 to 23 bar. 1.4 Chemical System Series and parallel complex reaction scheme, homogeneous, non-catalytic 2 BACKGROUND H-Acid (4 amino 5 hydroxy - 2, 7 naphthalene disulfonic acid) is an important intermediate in dyestuffs manufacture. It is produced by the ''caustic fusion'' of Koch Acid (4 amino - 2, 5, 7 naphthalene trisulfonic acid) traditionally in batch autoclaves. Since the desired reaction involves the replacement of one of three SO3H groups by an OH, not surprisingly isomer byproducts are obtained. In addition the amino group itself undergoes substitution. The major reactions are shown schematically in Figure 1 (the traditional shorthand notation S = SO3H being adopted).

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com For etymological consistency the kinetic modelers christened the tarry residues "Ghost Acid" (that portion of the starting materials whose useful life has departed). Process and laboratory experience showed that yield was crucially affected by variations in the time/temperature history of the batch. The emergence of analytical techniques in the 1960s made analysis of process intermediates possible and as a consequence elucidation of kinetic data became a distinct probability. This case study summarizes the work carried out aimed at both optimizing existing manufacturing facilities and designing new plant. The technology described has been incorporated into a European Plants. 3 KINETICS AND MECHANISM Since the reaction is carried out in the presence of excess caustic soda the scheme of Figure 1 is most simply represented by a set of pseudo first order mass action kinetic equations. This simple model was subsequently found to fit the experimental data within the accuracy of that data. From isothermal laboratory fusions at different temperature levels the activation energies and pre-exponential factors were determined. In terms of H-Acid yield, only reactions I, II and III (see Figure 1) are of direct interest for further modeling. Mass balances on Koch and H-Acids may be written:

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 4 MAXIMUM YIELD AND IMPLICATIONS FOR REACTOR DESIGN An unconstrained optimization on the kinetic Equations (1) and (2) showed that a maximum yield of some 84% was achievable under (unreal) conditions of rapid heat-up and instantaneous quench. Since this figure was over 10% higher than current manufacturing attainments in heat transfer limited autoclaves the margin for improvement was considerable. Clearly the nearest approach to the desired temperature profile predicted by the unconstrained optimization would be approximated in a jacketed plug flow reactor. Pilot plant experiments on such a reactor system were unsuccessful due to a variety of mechanical details rendering operation hazardous. A compromise approach was investigated whereby extra heat transfer surface (in the form of coils) for rapid heating and pressure let down for flash evaporative rapid cooling in a batch autoclave was adopted. A mathematical model incorporating the heat transfer phenomena was constructed around which optimization of temperature profile (by Rosenbrock) was introduced. With the limitation of jacket heating/cooling on the existing process plant only small increases in overall yield proved possible. For new autoclave designs incorporating coils, yields as high as 81.5% were predicted at cycle times much shorter than current plant practice. With finite steam supply the optimization reduced to the single variable of change-over from heating to cooling. This permitted the Rosenbrock technique to be replaced by a simple Fibonacci search (Ref. [1]). Laboratory checks on the predicted profiles gave yield figures within 0.1% of the model's predicted yields. As a design tool the mathematical model was refined to incorporate corrosion data, programmed cooling (to avoid stress cracking) and fitted with digital plotter output (see example in Figure 2).

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 5 USE OF DESIGN MODEL FOR START-UP AND MANUFACTURING MONITORING Under start-up and indeed routine manufacturing operations various mishaps are likely to make strict adherence to the temperature profiles impossible. The most likely cause of such problems will be "hiccoughs" in the steam supply. The complexity of the model lies with reproducing the reactor environment and optimization routines rather than the simple kinetic equations. In principle the latter can be incorporated into the process control computer scheme to predict the H-Acid yield pattern developing in time as a consequence of the achieved time temperature sequence for a particular batch. In new manufacturing plant this will be done and used as a production management tool. 6 BIBLIOGRAPHY [1] Gill P E, Murray W & Wright M H, Practical Optimization, Academic Press (1981), London, pp 89 - 90.

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com FIGURE 2 TEST RUN OPTIMIZATION OF HEATING TIME 3600 kg/h STEAM

Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com

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