Chemical Projects Scale Up: How to go from Laboratory to Commercial

By Joe M. Bonem

Chemical Projects Scale Up: How to Go from Laboratory to Commercial covers the chemical engineering steps necessary for taking a laboratory development into the commercial world. The book includes the problems associated with scale up, equipment sizing considerations, thermal characteristics associated with scale up, safety areas to consider, recycling considerations, operability reviews and economic viability. In addition to the process design aspects of commercializing the laboratory development, consideration is given to the utilization of a development in an existing plant.

• Explains how heat removal for exothermic reactions can be scaled up
• Outlines how a reactor can be sized from batch kinetic data
• Discusses how the plant performance of a new catalyst can be evaluated
• Presents how the economics of a new product/process can be developed
• Discusses the necessary evaluation of recycling in commercial plants

• Language: English
• Publisher: Elsevier Science
• Release date: May 31, 2018
• ISBN: 9780128137284

Joe M. Bonem

Mr. Bonem’s highly productive five-decade career has included over three decades in Polymers manufacturing and process development with Exxon Chemical as well as 20 years in consulting. He is available for consulting in his areas of expertise. These areas include all phases of chemical engineering including Technology Transfer and Assimilation, Process Development and Scaleup, Project Basis Development and Process Design, Plant Performance Improvements and Safety Assessment of New and Existing Technology. Mr. Bonem is experienced in the development and mentoring of young engineers, and has extensive experience in working in foreign countries and cultures. He also has experience serving as an expert witness.

Book preview

Chemical Projects Scale Up: How to go from Laboratory to Commercial

Joe M. Bonem

Table of Contents

Cover

Title page

Copyright

Introduction

1: Potential Problems With Scale-up

Abstract

Equipment Related

Mode Related

Theoretical Considerations

Thermal Characteristics

Safety Considerations

Recycle Considerations

Regulatory Requirements

Project Focus Considerations

Take Home Message

2: Equipment Design Considerations

Abstract

Introduction

Reactor Scale-up

Laboratory Batch Reactor to Larger Batch Reactor (Pilot Plant or Commercial)

Laboratory Batch Reactor to a Commercial Continuous Stirred Tank Reactor

Laboratory Batch Reactor to a Commercial Tubular Reactor

Laboratory Tubular Reactor to a Commercial Tubular Reactor

Reactor Scale-up Example

Summary of Considerations for Reactor Scale-up

Supplier’s Scale-ups

Volatile Removal Scale-up

Example Problem 2-2

Summary of Key Points for Scale-up of Volatiles Removal Equipment

Other Scale-ups Using the Same Techniques

Solid–Liquid Separation

Example Problem 2-3

3: Developing Commercial Process Flow Sheets

Abstract

4: Thermal Characteristics for Reactor Scale-up

Abstract

5: Safety Considerations

Abstract

Use of New Chemicals

Change in Delivery Mode for Chemicals

Impact of a New Development on Shared Facilities

Reaction By-Products That Might be Produced

Storage and Shipping Considerations

Step-Out Designs

6: Recycle Considerations

Abstract

Why Have a Recycle System in a Pilot Plant?

Impurity Buildup Considerations

7: Supplier’s Equipment Scale-up

Abstract

Agitator and Mixer Scale-up

Indirect Heated Dryer

Summary of Working With Suppliers of Specialty Equipment

8: Sustainability

Abstract

Long-Term Changes in Existing Technology

Long-Term Availability and Cost of Feeds and Catalysts

Long-Term Availability and Cost of Utilities

Disposition of Waste and By-Product Streams

Operability and Maintainability of Process Facilities

Summary

9: Project Evaluation Using CAPEX and OPEX Inputs

Abstract

Introduction

CAPEX and OPEX

Project Timing and Early Design Calculations

10: Emerging Technology Contingency (ETC)

Abstract

Application

Contributors/Reviewers

11: Other Uses of Study Designs

Abstract

Identifying High Cost Parts of CAPEX and OPEX

Identifying Areas Where Unusual or Special Equipment Is Required

Identifying Areas for Future Development Work

Identifying the Size-limiting Equipment

Identifying Areas Where There Is a Need for Consultants

Summary

12: Scaling Up to Larger Commercial Sizes

Abstract

Summary

13: Defining and Mitigating Risks

Abstract

Techniques for Definition and Mitigation of Risk

Required Manpower Resources

Reasonable Schedules

Cooperative Team Spirit and Culture

14: Typical Cases Studies

Abstract

Successful Case Studies

Unsuccessful Case Studies

Production of an Inorganic Catalyst

Development of a New Polymerization Platform

Utilization of a New and Improved Catalyst in a Gas Phase Polymerization Process

Inadequate Reactor Scale-up

Utilization of a New and Improved Stabilizer

The Less Than Perfect Selection of a Diluent

Epilogue: Final Words and Acknowledgments

Index

Copyright

Elsevier

Radarweg 29, PO Box 211, 1000 AE Amsterdam, Netherlands

The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, United Kingdom

50 Hampshire Street, 5th Floor, Cambridge, MA 02139, United States

Copyright © 2018 Elsevier Inc. All rights reserved.

No part of this publication may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopying, recording, or any information storage and retrieval system, without permission in writing from the publisher. Details on how to seek permission, further information about the Publisher’s permissions policies and our arrangements with organizations such as the Copyright Clearance Center and the Copyright Licensing Agency, can be found at our website: www.elsevier.com/permissions.

This book and the individual contributions contained in it are protected under copyright by the Publisher (other than as may be noted herein).

Notices

Knowledge and best practice in this field are constantly changing. As new research and experience broaden our understanding, changes in research methods, professional practices, or medical treatment may become necessary.

Practitioners and researchers must always rely on their own experience and knowledge in evaluating and using any information, methods, compounds, or experiments described herein. In using such information or methods they should be mindful of their own safety and the safety of others, including parties for whom they have a professional responsibility.

To the fullest extent of the law, neither the Publisher nor the authors, contributors, or editors, assume any liability for any injury and/or damage to persons or property as a matter of products liability, negligence or otherwise, or from any use or operation of any methods, products, instructions, or ideas contained in the material herein.

Library of Congress Cataloging-in-Publication Data

A catalog record for this book is available from the Library of Congress

British Library Cataloguing-in-Publication Data

A catalogue record for this book is available from the British Library

ISBN: 978-0-12-813610-2

For information on all Elsevier publications visit our website at https://www.elsevier.com/books-and-journals

Publisher: Susan Dennis

Acquisition Editor: Kostas KI Marinakis

Editorial Project Manager: Emily Thomson

Production Project Manager: Maria Bernard

Designer: Victoria Pearson

Typeset by Thomson Digital

Introduction

When one considers writing a book, there are two questions that must be answered—The first question is Is there a need for such a book? Tied up in this question is Who is the audience and what is their experience level? The second question is What knowledge do I have that would allow me to write such a book?

For this book, the answer to the first question is that one of the desires of industrial research, as well as academic research is to convert a discovery into a viable useful product. Essentially all research and/or development work is done with the goal to eventually commercialize the product or process so that it may:

• Create increased profits or turn a money-losing venture into one that makes a profit by a new process, process modification, or new catalyst.

• Create a new chemical or modification of an existing chemical that can increase company profitability.

• Create a pharmaceutical drug, which can extend life, cure diseases, or make life more comfortable.

With these goals in mind, the idea of a book began to evolve. The title is self-explanatory. It is basically a book that describes how we get there from here. The job of getting there is often assigned to a chemical engineer with in-depth knowledge of research or in-depth knowledge of plant operations and/or process design. However, it is likely that they will have only limited knowledge with taking a discovery from the laboratory to commercial operation. On one hand, this is not a book for experts who are seeking a new and exotic way to scale up an unusual reactor design. The audience for this book is the inexperienced engineer. He could be an engineer who is not experienced in either research or plant engineering or who has minimal experience in both, such as a new college graduate. On the other hand, the book also provides insight of value to either a researcher with no plant engineering experience or a plant engineer/process designer with no research experience. The audience for the book might have a need to understand the basics in one of the following:

• Reactor scale-up using simplified the first-order kinetics.

• The inherent risks in increasing size of a reactor where an exothermic reaction is being conducted.

• How does one organize for a successful scale-up.

In addition, the book provides techniques to understand how suppliers of specialized equipment, such as agitators, dryers, or centrifuges scale up from their pilot plant data. Although one might think that the primary purpose of such a book is technical, it is important to know at an early stage of any development whether a successful scale-up will produce an economically successful project. The book includes chapters that discuss how a project can be evaluated at an early point in the research phase. The book also includes several examples of successful and unsuccessful scale-up projects. The means to develop successful development teams are also discussed.

The techniques and approaches discussed in this book were developed based on many years of experience in heavy industry—the oil refining and petrochemical business. Although creating a new pharmaceutical drug was mentioned as a goal of going from the laboratory to commercial production, some might question whether these techniques apply to the pharmaceutical business. The development of a commercial process to produce a laboratory-based product is often done with a goal to reduce the cost of manufacturing the product. With the pressure on the pharmaceutical industry today to reduce the cost of their products, it would seem that cost reduction is a high priority. As a general rule, the cost of a product can be reduced when the mode of producing the chemical is changed from batch to continuous and when the scale of production is increased. That is what this book is about: Going from batch bench-scale operations to commercial size continuous operation.

Terminology is always important when attempting to communicate concepts. As this book developed, I became aware that there were certain concepts that were second nature to me that I needed to explain. The terminology is described in the following paragraphs.

Batch operations are those that are conducted by adding reactants to a vessel and keeping the vessel at a specific temperature for a period of time. During this period of time, there will be no flow of material into or out of the vessel. The vessel contents are then removed, and the reactants and products are separated. These batch operations are normally reactions or extractions, but they could be any unit operation. The art of cooking is filled with batch operations. On the other hand, continuous operations are those where reactants are always going into the vessel and material is always flowing out. Thus while the average particle in a continuous reactor may have the same residence time as that in a batch reactor, there will be some that have much shorter residence times and some with much longer residence times. Most operations in refineries and chemical plants are continuous.

The distinction among bench scale, pilot plant, and commercial size often is based on production capacity. Bench scale has to do with operations (normally batch operations) that are conducted on such a small scale that they can be done on the laboratory counter (bench) or fume hood. They are generally operated only during normal office hours. Pilot plant operations are generally continuous and conducted in facilities that are separate from the laboratory. A typical pilot plant might be housed in a separate building with a DCS (Digital Control System), be a scaled down version of the commercial plant and produce 50–500 lbs/h of product. The pilot plant will often operate full time (24 h a day and 7 days a week). Some of the equipment might be batch. The commercial plant is very similar to the pilot plant except essentially all facilities will be continuous.

In writing this book, it was necessary to define a starting point and an ending point for the project that is being commercialized. I have defined these points as described below:

• The starting point is the point where a single individual or small group working in a laboratory seems to have made a discovery significant enough that additional resources are assigned to the project. At this point in project development, the research is advanced to the point that a process designer is assigned at least part time to the project. The process designer will be a chemical engineer who has designed commercial plants and/or solved operating plant problems. This process designer will have two functions: he will help uncover other areas of research that must be completed to allow a firm process design to be developed; he will also be involved in developing a study design and cost estimate to allow an economic evaluation of the project. This aspect of project development is often overlooked. However, the development of the study design at an early point allows for the modification of the design as the project progresses, as well as development of the economics along the way. It is conceivable that one of these economic evaluations might cause the project development to look unattractive. This will normally bring cries of foul. We should have waited until we developed more data to make this evaluation. However, it is likely that a good study design and economic evaluation will determine the feasibility of the project no matter how much additional data are required. Chapter 9 describes the study design in more detail.

• The true ending point is when the plant, plant modification, or new catalyst/chemical utilization has been successfully implemented. When one considers what is meant by a successful startup or successful utilization of a new chemical or catalyst a definition of this state of success is required. The successful completion of a project (new plant or new catalyst) is defined as the point where the project is either meeting the economic projections or a clear path is available for reaching this point in three to six months. This book deals with the initial steps of a new development through the initiation of detailed design. However, The last three steps in this implementation process (detailed engineering design, construction, and plant startup) have been described thoroughly by others. Thus, they receive only minimal attention in this book. Therefore, I have defined the ending point for a project that consists of construction of a new plant or existing plant physical modification as the completion of the front-end engineering work. At this point, all the aspects of scale-up and chemical engineering design will be essentially finished and a detailed engineering design will have been initiated. For the case where a new catalyst/chemical is being utilized, the end point is when the chemical is successfully utilized in the commercial plant.

The second question deals with the question of having sufficient knowledge to write such a book. In answering this question, I reviewed my career. My career progressed through several stages of learning what chemical engineering was all about. These stages of learning, in addition to the academic world, consisted of time spent doing conceptual process design (including scale-up), process evaluation based on conceptual design, detailed process design, serving as an owner’s representative during detailed engineering, and facilities startup. Along the way, I made four observations:

• I wanted to stay in technical work rather than progress as a manager.

• The technical work was of interest if it was challenging and provided value added for my clients or the company that I was working for.

• The commercialization of technology is potentially one of the more challenging aspects of chemical engineering. Unfortunately, it is an area that often is treated superficially. I learned first-hand the risk of failing to peel back layers of the onion when considering a new technology development. As layers of the onion are peeled back, more and more questions, which need to be considered, are uncovered.

• I also learned that a pragmatic solution based on theoretically correct relationships is much better than a beautiful theoretically correct solution that does not work because of its complexity. Thus, there are some in the chemical engineering field, who will look at this book and consider it overly simplified. The primary defense against this charge is that the concepts given here have been proven to work. In addition to the practicality of the approaches described herein, they have the advantage of being easily understood. An engineer or chemist working in today’s industrial environment rarely has time to fully understand a complicated approach. This is particularly true when the marginal benefit of the complicated approach is minimal. Lord Ernest Rutherford once proclaimed A theory that you cannot explain to a bartender is probably no good.

The goal of this book is to provide a package of information to allow one to visualize how a technology development can flow from the laboratory to commercial operation and to show how simple concepts can be used to scale-up from laboratory bench scale or pilot plant data to a commercial plant. Fig. I.1 presents a very simplified sketch of the technology development process. Fig. I.1 only shows the development of the process or new raw material along with product development as single lines. More detail for process development is given in Fig. 9.1. In addition, the product development is an important step and must be completed in synchronization with the process development.

Figure I.1   Parallel paths of commercial development.

(Concept of need to combine process development with product development. May not apply to all development projects).

The approach proposed in this book works whether the new technology is simple or complicated. The new technology may seem to be a simple replacement that does not require what might be considered an elaborate stepwise procedure. On first pass, it might seem that most of the details shown later in this book can be omitted. For example, if a new additive is proposed to replace one that is not performing well, it might seem that some or most of the proposed steps can be eliminated. As trivial as this may sound, all the steps suggested in this book will be applicable. In contrast, the new technology may well be the development of a new process to replace an out of date process or a new process to make a new product. The new process/new product is obviously a much more complicated sounding development. But, the same process described in this book is applicable regardless how complicated or simple the innovation is. As a personal example, I found out the hard way when assigned to a project to make a simple change in an additive that in the process industry, no change is simple. This failure is described in Chapter 14.

It is my hope that this book will be helpful to new engineers working in all phases of research (chemicals, oil production, refinery, pharmaceuticals…….) and for those responsible for commercialization of new technology. The book will also be of importance to the laboratory chemist that is developing a new technology or the experienced plant engineer assigned to the project who has no research experience.

Commercialization of new technology is often referred to as scale-up. While this term has the connotation of larger equipment, it can also be applied to new technology associated with a chemical or catalyst change. Regardless of a successful laboratory product or process demonstration, there will almost always be a step to expand the production of a product or use of a chemical/catalyst from laboratory size quantities to commercial sized quantities. This step is referred to as scale-up. In addition, this term is often used to address the additional steps that must be added to the laboratory demonstration to allow commercialization. For example, a process demonstrated in the laboratory using reagent grade feedstock will likely require a step in the scaled-up process to purify the commercially available feedstock. The term scale-up is well known in the chemical/refining, food, and pharmaceutical industries. A second term that is often used is scale-up ratio. This is generally the ratio of commercial production to that in the pilot plant or laboratory. The scale-up ratio can also be associated with the ratio of equipment capacities or sizes, which may be slightly different than the production scale-up ratio. There may be multiple scale-ups involved in going from laboratory production and/or a laboratory process to a fully commercial venture. These scale-ups can consist of:

• Scaling up from bench scale equipment to pilot plan equipment.

• Scaling up from bench scale equipment to commercial size equipment.

• Scaling up from pilot plant equipment to commercial size equipment.

• Scaling up from a small commercial size plant to a large commercial plant.

• Scaling up a single piece of equipment, such as an indirect heated dryer or extruder from pilot plant size to commercial size equipment.

• Scaling up from bench scale studies to use a new catalyst in either a pilot plant or commercial plant.

Each of these scale-up steps requires an outlay of money and also involves some risk, when considering scale-up to commercial plants the outlay of money and resources will be significant. In addition, the building of a commercial plant often involves a commitment to supplying product to a customer, at a specified time. Thus, the importance of the scale-up becomes obvious.

When considering the current chemical engineering academic environment and the wide diversity of chemical engineering education and employment opportunities, the areas of process design, process scale-up, and commercial development are often overlooked. This leaves the chemical engineer assigned to a new technology development struggling with how to proceed on this important step. When considering that the transfer of technology from the laboratory to commercial operation often fails, the question of Why did it fail? is of value. Given the importance of scale-up, the risks of an improper scale-up can be classified into eight categories shown below:

• Equipment related: Scale-up would always involve larger equipment and possibly a change in equipment design, such as from a jacketed vessel to an exchanger pump-around loop.

• Mode related: A typical scale-up may well involve a change in equipment mode, such as a change from a batch reactor to a continuous reactor.

• Theoretical considerations: While theoretical conclusions and considerations have generally been the regime of the laboratory chemists, the scale-up should consider if it is possible that anything is missed or erroneous conclusions have been drawn. This will also be a good time to consider simplified kinetic relationships and their possible relationships to the scale-up. An example of a failed scale-up associated with inadequate considerations of theory is given in Chapter 14.

• Thermal characteristics: Scale-up of a reactor or other vessel where heat transfer is occurring will always require consideration due to the potential reduced area to volume ratio as the reactor is scaled up.

• Safety considerations: While safety is always a consideration, it is more so as the equipment size is increased. Larger equipment will contain more potential energy and more toxic chemical in the contingency associated for a containment failure.

• Recycle considerations: Several factors require that recycle facilities be included in commercial facilities where it may not be as important in laboratory or pilot plant facilities.

• Regulatory requirements: This area might include products, process, and by-product disposal.

• Project focus considerations: The project team must maintain focus on the development and the economic aspects of the process.

These failure modes are covered in more detail in various chapters in the book.

The available literature deals with both scale-up from a unit operations standpoint and an approval process as separate entities. Dealing with scale-up from a unit operations approach has to do with how data and equipment from a laboratory bench scale or a pilot plant can be used to design a larger facility. The approval process is that process where permission and funding are granted for taking the next step in the process development process. It usually occurs at a point where significantly increased