Department of Chemical Engineering, Auburn University

CHEN 4470, Spring 2008

DESIGN OF A SODIUM METHYLATE PRODUCTION PROCESS

Background Sodium Methylate (NaOCH3) is a catalyst used in the production of biodiesel from triglycerides, such as soybean oil, rapeseed (canola) oil or animal fats. Sodium Methylate is typically sold as a solution with Methanol. The overall objective of this project is to design a grass-roots facility capable of producing a total of 60,000 metric tons per year of a 30wt% NaOCH3/70wt% Methanol solution. Sodium Methylate can be manufactured by the direct reaction of Sodium Hydroxide (NaOH) with Methanol (CH3OH), as follows: NaOH + Sodium Hydroxide CH3OH Methanol NaOCH3 + Sodium Methylate H2 O Water

This reaction is carried out in a reactive distillation column. In this system, a 50% Sodium Hydroxide solution in water is fed to the top of the column and methanol vapor is fed to the bottom. As the reaction occurs, the Sodium Methylate/Methanol solution is collected at the bottom of the column. The column is fed an excess of Methanol vapor to strip the water out of the product. It is critical to keep water out of the final product. The flow diagram below shows the basic configuration of the process. Questions marks indicate decisions to be made during process design.
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T=? P= ? T=? P= ?

50% NaOH Soln.

T=? P= ?

T=? P= ?

?
Fresh MeOH Supply Waste Water

Reaction Column

Methanol Column

NaOCH3 Prod. Soln.

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Department of Chemical Engineering, Auburn University

CHEN 4470, Spring 2008

Operating temperatures and pressures must be determined during process design. Additional equipment such as utility systems, pumps, surge vessels and storage tanks should be added as required. The column overhead product will contain methanol and water. This mixture must be separated so the methanol can be recycled to the reaction column. The second column is an ordinary distillation column designed to separate the Methanol/Water solution. The overhead product is to be Methanol containing no more that 500 ppm of water. The bottom product is to be waste water. In order to avoid a hazardous waste classification, the Methanol content in the waste water must be less than 1000 ppm. Additional design requirements for this process are given in the following section. Design Requirements In order for the Sodium Methylate reaction to proceed to completion, 3 minutes of residence time are needed on each tray. Consider this requirement when selecting a tray type for the reactive distillation column. Using the given kinetic parameters below, calculate the conversion per tray, and then calculate the total number of trays to achieve 100% conversion. The column diameter will have to be determined in conjunction with the hydraulic requirements of the column. Aspen Plus can be used to carry out this optimization. Be sure to justify the number of trays and column diameter you select. There is no specific residence time requirement for the Methanol/Water column. The NaOCH3 reaction is an equilibrium reaction. The following kinetic data shown in the screen print below are available for use with Aspen Plus:

Because of the methanol recycle, the two columns required for this process are coupled with regard to energy and operating pressure. The operating pressure at the top of the reactive distillation column should be close to atmospheric pressure. Carefully consider pressure drop in the two columns and interconnected piping to determine the pressure at the top and bottom of each column. Remember, the residence time requirement in the column will affect the pressure drop! The pressure in the Methanol/Water column will be higher than in the reactive distillation column. This means that you will have to raise the pressure of the reactive distillation column distillate to get it in to the Methanol/Water column. This can be accomplished using a compressor, or by
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Department of Chemical Engineering, Auburn University

CHEN 4470, Spring 2008

condensing the distillate and using a pump. Consider the impact on capital cost and energy cost when making this decision. Propose a control strategy for these coupled columns. What variables will you control? What variables will you chose as fixed setpoints? What measured values will your strategy require? Describe how control fluctuations in one column will affect the other. Are there any special requirements for unsteady state conditions, such as start-up or shut-down? Is any additional equipment required to achieve good control, such as hold-up tanks, or heat exchangers? How do your equipment choices affect your control strategy (ie, with regard to the pressure considerations described above)? Your Methanol supplier has informed you that fresh Methanol contains at least 1000 ppm of water! Based on this information, carefully consider where you will feed the fresh Methanol to the system. Remember, we want to keep water out of the Sodium Methylate Product, so the Methanol used to strip water must be dry, ie, containing less than 500 ppm of water. NOTE: The property model you select is important! Try to find actual VLE Data for the Methanol/Water mixture and justify the property method you decide to use. Dont forget, NaOCH3 is an electrolyte! The relationship between number of trays and reflux ratio is extremely important for this system. Be sure to determine both the minimum reflux ratio and the minimum number of theoretical trays to guide your decision regarding the number of trays you select for the Methanol/Water column. Be sure to justify your choice for number of trays based on the results of these calculations! HINT: Aspen can be used for carrying out these calculations. The energy costs for this product are high, therefore, finding ways to reduce the energy requirements are important. A thermal pinch analysis is a good place to start, but this is not the whole story. The equipment design and the interaction between the two columns will greatly affect the energy requirement. Apply your engineering judgment and the tools of process optimization to minimize the energy usage of this process. Quantify how much energy your design will save versus a non-optimal (but still operational!) design. Since the biodiesel market is new in the US, some volatility in demand is expected, especially in the first few year of operation. Therefore you must design your plant for a 50% turndown. How does this affect your control strategy? How will this affect your choice for condenser and reboiler type for the columns? What about energy efficiency? Is it better to run at 50% production rates, or only run the plant half the time during times of low demand? HINT: Consider both fixed and variable costs in addressing this question! Finally, this system uses raw materials that are hazardous and/or flammable. Describe your safety concept for this process. What are the process risks and how can those risks be mitigated? How will you set design pressures and temperatures for your process equipment? Can the principles of inherently safe process design be used to reduce the hazards of this process? The project will incorporate a wide range of aspects related to chemical process and product design, e.g. flowsheet synthesis and simulation, heat and mass integration for resource conservation, process optimization, process economics, and also environmental, health and safety related issues. In the following some information is given about the progress reports that need to be submitted during the course of this design project. It must be emphasized that the items listed below are suggested main topics for the content of the reports, they are NOT meant as a complete check list. This is an open-ended design project so the project may go in many directions, which are not listed.

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Department of Chemical Engineering, Auburn University

CHEN 4470, Spring 2008

Progress Report No. 1 Thursday January 31, 2008 Review literature on production, market and economics of biodiesel, NaOCH3 and MeOH Describe governing chemical/physical principles in each process including phase behavior Identify the principal process units necessary to achieve the desired products Prepare a Process Flow Diagram for the NaOCH3 process Prepare detailed material balance based on flowsheet (full capacity and turndown cases) Prepare preliminary energy balance for flowsheet (full capacity and turndown cases) Prepare an economic analysis based on the preliminary flowsheet and mass/energy balances Progress Report No. 2 Tuesday March 4, 2008 Use ASPEN Plus to develop a rigorous process model of the NaOCH3 process Simulate and optimize Reactive Distillation Column Determine number of trays based on kinetics and hydraulics Determine column diameter Determine reboiler and condenser type Determine reflux ratio and condenser/reboiler duty Determine feed location for NaOH and MeOH Simulate and optimize Methanol/Water Column Calculate number of trays and reflux ratio Determine reboiler and condenser type Determine optimum feed location Determine operating pressures for coupled columns Recommend means of coupling columns Progress Report No. 3 Thursday April 3, 2008 Prepare final energy balance for flowsheet (full capacity and turndown cases) Complete the control strategy and include on Process Flow Diagram Propose a safety concept including inherently safe design considerations Complete the energy assessment, including thermal pinch analysis Review literature for separation and process improvement techniques that can be used to further improve the overall process performance Final Report Thursday April 17, 2008 Complete the economic analysis including all process options Complete the detailed environmental, health and safety analysis of the suggested design Report results from individual team assignment Combine the results from all progress reports into one coherent and comprehensive report Individual Team Assignments March 3-7, 2008 Each team will be assigned an individual open ended problem to investigate. These problems will be assigned the second week of March and must be reported in the final report as well as the oral presentation. Below is a list of possible projects. Additional Open Ended Projects Consider the impacts if two grades of NaOCH3 are required a 25% Solution and 30% Solution in Methanol. How can this requirement be met and how does it affect the project economics? How does this affect the product storage requirements? What additional equipment is required? How is the control concept affected by this requirement? How will you manage inventory and prevent contamination?
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Department of Chemical Engineering, Auburn University

CHEN 4470, Spring 2008

Complete an environmental assessment using the WAR Algorithm to determine environmental impacts of your process decisions. Consider the Global Warming Potential of the process and how a carbon tax would impact your design choices. Consider how the process to manufacture NaOCH3 affects the overall carbon footprint of the biodiesel process. How does the NaOCH3 based biodiesel process compare in terms of carbon footprint to other biodiesel manufacturing processes? Consider an alternate case where no cooling tower water is available. Determine whether a system that relies on air cooled heat exchangers for process cooling is more cost effective than including a new cooling tower in the process scope. Determine the surface area and fan speed requirements for the air cooled exchanger option. What are the advantages and disadvantages of this alternate? How does the weather affect the operation and control of this process? Conduct a risk assessment for the NaOCH3 process. Develop hazard scenarios, including likelihoods and consequences. Make recommendation for safeguards to mitigate the risks you discover. How do the economic impacts of the safeguards compare with making the process inherently safer in the conceptual design phase? Consider in detail the choice of property method in the ASPEN Plus simulation. Compare the results using at least three different property methods and determine the impact on the estimated project cost. Quantify the economic risk based on uncertainty in the property method and include this contingency in your final economic assessment. Determine other sources of project risk and attempt to quantify them in your final estimate.

Oral Presentation Last Week of Classes, April 24-25, 2008 The oral presentations of the proposed designs are tentatively scheduled for the last week of classes, i.e. April 28-30, however depending on availability of the external reviewers it may be rescheduled. More information will follow later. Background Literature The references listed here do not represent a complete list. They serve as a basis for obtaining further information through quoted papers and reports. Furthermore the teams are strongly encouraged to use novel sources of information such as the World Wide Web. Process Description Kirk-Othmer Encyclopedia of Chemical Technology Perry and Green, Perrys Chemical Engineers Handbook Ullmanns Encyclopedia of Industrial Chemistry BASF European Patent EP 1242345 B (2004) Process Design Biegler, Grossmann and Westerberg, Systematic Methods of Chemical Process Design Douglas, Conceptual Design of Chemical Processes Seider, Seader and Lewin, Process and Product Design Principles Smith, Chemical Process Design Process Economics Coulson and Richardson, Chemical Engineering Design by R.K. Sinnott Peters, Timmerhaus and West, Plant Design and Economics for Chemical Engineers

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Department of Chemical Engineering, Auburn University

CHEN 4470, Spring 2008

A Few Words of Wisdom Remember that this is an open-ended project, i.e. you can take the project in almost any direction you find interesting. However you will need to state your reasons for turning the focus on a specific part. During the different stages of the project it will become necessary to make assumptions in order to solve the problems. ALWAYS state your assumptions and the reasons for making them. There are many aspects of this project that can be worked on simultaneously. Use your time and efforts wisely so you do not waste valuable time waiting on help just because you are stuck on one part of the project. The instructor is there to help you, so use him.

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