Batch Distillation Column: Executive Summary

Section AA
Evan Epstein, Stephanie Ford, Andrew Kullman, Emily Thomas, Kyle Elliott

Abstract

Biofuels are a more sustainable alternative to conventional fuels such as oil, coal, and natural gas.
The process of interest in this report, illustrated in Figure 1, uses yeast, sugar, nutrients, and
downstream processing to produce fuel grade ethanol. In industry, fuel grade ethanol is blended
with gasoline to increase the octane rating, resulting in higher quality fuel and a reduction in
non-renewable fuel usage.

Figure 1 ​Ethanol production from yeast and glucose

Water and ethanol mixtures form an azeotrope, so the separation process requires a series of
separations to achieve fuel grade ethanol concentrations. The focus of this executive summary is
to outline the feasibility of using a batch distillation column in this process. Batch distillation is
commonly used in applications demanding high product purity, but comes with the disadvantage of
requiring significantly more labor.
Rotations 1-3 have performed various analyses so the design team can determine in what capacity
the batch distillation unit will exist on the pilot plant. The rotations found that decreased heater duty
resulted in increased product purity, but decreased boilup rate. Distillate flow rate decreased with
reflux ratio, though data implying that increasing reflux ratio increases product purity were not
replicable. The rotations found that conducting a Smoker-Rose analysis yields projected
concentrations that are higher than the experimental value, but that it is relatively reliable. Rotation
3 performed an energy analysis the design team can use when optimizing the cost of their plant.
The rotations found that a single batch distillation column was unable to raise ethanol
concentrations from 50-90 mol%.
1. Introduction OMDs
The ethanol production process consists of a bioreactor unit, where ethanol is produced, and
several separation units. Since fuel grade ethanol must contain very little water, effective ethanol
purification is essential to the plant’s success. Ethanol and water form an azeotrope, one of the
required separation processes is a molecular sieve, which elevates product purity above the
ethanol-water azeotrope. The molecular sieve’s effectiveness at removing water from the solution
increases with ethanol mol% of the mixture [8]. The batch distillation column useful for preparing
the product for the molecular sieve. Achieving high purity before the sieve step can decrease
costs and increase production, and batch distillation columns are commonly used to achieve high
product purity with maximum flexibility [7]. Those savings are balanced by the costs of labor costs
or sophisticated automation equipment, and batch distillation columns’ limited inlet bulb size, which
limits production.

Increased mass transfer leads to higher product purity. In a batch distillation column, mass transfer
occurs at the theoretical trays. The number of theoretical trays is variable in batch distillation
columns; optimizing operational parameters like heater duty and reflux ratio creates more efficient
and effective distillation columns.

The research rotations have explored the effect of varying column conditions such as heater duty,
and reflux ratio. The resulting data were analyzed using:
● The Mccabe-Thiele method, which uses equilibrium data and inlet/outlet conditions to
determine the number of theoretical trays
● Smoker-Rose, which can be used by the design team to predict future distillate values.
Specifically,
● Rotation 1 and 2:
○ Established a procedure for data collection
○ Developed a python notebook for data analysis
○ Established a basis of initial fluid inlet values
○ Determined the most effective heater duty was 50%
○ Determined the feasibility of using Smoker-Rose analysis to predict distillate values
● Rotation 3:
○ Confirmed the feasibility of using Smoker-Rose analysis to predict distillate values
○ Determined the relationship between product purity and reflux ratio
○ Found parameters to minimize energy consumption and maximize product
produced
○ Created a model for energy usage at varied effective reflux ratios
These results allow the design team to make informed choices about the place of a batch
distillation unit in this process. We recommend using Smoker Rose to predict distillate results, and
carefully balancing labor and maintenance costs when considering whether to use a batch
distillation column. Two distillation columns in series, operating at R=3 should decrease operation
time and therefore labor costs as they produce high purity product. Rising labor costs might
override the benefit of the batch distillation column. If this occurs, we would recommend installing
additional trayed columns, which require less labor, and omitting the batch column entirely.

2. Experimental Approach
The test column’s physical design remained unchanged across all three rotations. Figure 5 in
Appendix A2 shows a schematic of the batch distillation column.
Summary of Methods
The initial pot solution contained 3L of 28 mol% (50% w/w) ethanol and water. A constant 50%
heater duty was applied by recommendation of Rotation II. At R=3 there exists an optimal balance
between product purity and distillate flow/production rate between 50 and 90% heater duty.
Rotation II’s data shows that a distillation run at 50% duty results in a higher ethanol product
composition over time compared to one run at 40%. It also shows that maximum duty results in
lower product ethanol composition. Rotation II’s recommendations and our interest in the effects of
varying reflux ratio caused us to apply a constant 50% heater duty. We took samples of the
instantaneous distillate and pot at total reflux. Using the sample compositions in a McCabe-Thiele
analysis determined the number of effective stages to be used in Smoker-Rose analysis. The
procedure is detailed in the Rotation II’s Appendix. We determined the energy required to obtain a
basis of 100g ethanol with calculated average product compositions and their associated
run-times. Two pot, average, and instantaneous distillate samples were taken 10 minutes apart at
R=3, 6, and 9 and compared with compositions calculated by Smoker-Rose. For samples
projected to be >70 mol% ethanol, an SRI Gas Chromatograph was used for composition
measurements. All other samples were measured using a densiometer.

3. Key Findings
Rotations 1 and 2:
- Decreased heater duty resulted in an increased number of effective stages and higher
product purity.
- As instantaneous distillate composition approached the ethanol-water azeotrope at
operation pressure, there was an increase in the number of effective stages required to
achieve desired separation.
- Lower heater duty resulted in lower boilup rate and distillate flow rate in the column. The
optimal operational parameters balanced product concentration with product flow rate, as
decreases in heater duty were found to both increase product purity and decrease product
flow rate.
- A column with a higher reflux ratio produced less product in the same amount of time.
- Smoker-Rose analysis predicts higher distillate concentration than was experimentally
obtained.
- A single batch distillation column was unable to distill a 50 mol % initial pot charge to a 90
mol % product by varying heater duty.
Rotation 3:
- The energy required to obtain a basis of 100 g of ethanol at average compositions
calculated via Smoker-Rose analysis and distillate flow rate was found to increase with
increasing reflux ratio, as shown in Figure 2 in Appendix A1.
- The relationship between average distillate composition and reflux ratio was inconclusive,
as shown in Figure 4 in Appendix A1
- The number of effective stages increased with increasing reflux ratio, as shown in Figure 3
in Appendix A1
- Smoker-Rose is a useful way to predict approximate distillate concentration

4. Significance
It is not possible to achieve 90% product purity using a single batch distillation column. The design
team would likely need to conduct further testing on what a series batch distillation process would
look like, calling into question the economic viability of batch distillation columns in this plant.
Non-continuous separation processes are highly labor intensive, and an approximately 25MM
gal/yr desired production rate would require a massive collection of batch distillation columns,
greatly increasing plant manufacturing and operating costs.
From the results reported in Table 1 and Figure 4 of Appendix A1, there is an unexpected
relationship between reflux ratio and average distillate composition. Because the number of
effective stages increases with increasing reflux ratio, Figure 3 of Appendix A1, we would expect a
better separation or greater final purity for higher reflux ratios. An inconclusive model will make
optimizing the batch distillation column for the final product difficult, so further investigation may be
required. Energy consumption analysis done in rotation 3, see Figure 2 in Appendix A1 adds that
higher reflux ratios also utilize more electricity to heat the higher return flow rate of condensate.
Table 2 in Appendix A3, shows that for the given batch distillation column, electricity costs are
insignificant compared to profit differences resulting from ethanol production. Extrapolating these
results to production batch distillation units would be worthy of future investigation by the design
team.

Smoker-Rose analysis was demonstrated to be a reliable method for predicting average distillate
compositions by rotation II. By using a second batch distillation unit with an initial charge of the
final product from the first process, 90% product purity could be reached. A reflux ratio of 3 would
be ideal to maximize the quantity of product available to separate further. The loss in product purity
is negligible compared to gains in flow rate as demonstrated by results in Table 1 in Appendix A1.

5. Rotation 3 Summary
Objectives, Milestones, and Deliverables
The three rotations aimed to find relationships between energy usage, distillate flow rate, effective
stages, and average distillate composition, as each varies with the column’s operating variables.
Rotations I and II found trends that described the relationship between heater duty, product flow
rate, and product purity. Rotation III found the energy costs indirectly associated with these
variables and those directly associated with reflux ratio. We were unable to find a conclusive
relationship between average distillate composition and reflux ratio. It has been established that
the energy required to obtain a greater amount of ethanol in the distillate product increases with
reflux ratio (Figure 3, A1).
In the production process, the economic feasibility of including one or more batch distillation
columns is dubious. Certain costs, such as operating labor, are much higher in batch processes
than they would be in continuous distillation. From a plant design perspective, synthesizing the
Rotations’ results and recommendations and performing comparative economic analyses of
different plant designs with a particular focus on the company’s labor costs ought to reveal the
efficacy of incorporating any batch distillation process.
If a batch process is determined to be viable, then it must be considered, as has been shown by
Smoker-Rose analysis, which we recommend be used for projective analyses, that 90% pure
product can only be achieved by incorporating a second batch distillation column in sequence. It
may be possible to project fairly accurate design costs based primarily on the capital cost and
operating labor of two identical batch distillation columns. Since we have found that energy costs
associated with batch production are very low relative to expected product value, they can likely be
neglected. Because operating labor is a considerable factor in any economic analysis, one big
question to answer is whether the additional labor required to operate and maintain two columns
can be optimized such that it is less than twice the amount that would be needed to operate one.
Based on our data analysis, a potentially profitable process might include two batch distillation
columns operating at R=3, which would yield the highest production rates and lowest energy costs
relative to higher ratios, effectively reducing operating time and therefore labor while keeping the
plant’s production of bioethanol higher. The trade-off in reduced operating time would be increased
time for maintenance, where labor could potentially be scaled to provide better care for equipment
and operating conditions such that the need for equipment repair and replacement and production
line interruptions could be minimized, positively influencing the plant’s productivity.*
6. References
1. Rotation 2, Batch Distillation Column Report Findings, (Takuma Okamoto, Ryan O’Hara,
Sam Ng, Zander Hall-Spicuzza)
2. Robert Perry, Don W. Green, Perry's Chemical Engineers' Handbook, 8th ed., McGraw-Hill,
2007. ISBN 0071422943
3. Distillation Column Internals. Werner Sölken 2008 - 2020.
http://www.wermac.org/equipment/distillation_part2.html
4. Calculator: Saturated Steam Table by Pressure.
https://www.tlv.com/global/US/calculator/steam-table-pressure.html
5. Water - Heat of Vaporization.
https://www.engineeringtoolbox.com/water-properties-d_1573.html?vA=94&units=C#
6. Ethanol. NIST
https://webbook.nist.gov/cgi/cbook.cgi?ID=C64175&Mask=4&Type=HVAP-FORM1&Plot=o
n#HVAP-FORM1
7. R.C. Costello.​ ​Batch vs. Continuous Distillation.​ 12 08 2016
https://rccostello.com/wordpress/distillation/batch-vs-continuous-distillation/
8. https://socratic.org/questions/what-are-the-best-methods-to-separate-an-azeotrope
Appendix
A1. Rotation III Data Summary

Avg Distillate Distillate Flow Effective Energy Usage

Reflux Ratio Initial Charge Composition [mol %] Rate (g/min) Trays [kJ]
50% by mol
3 28% by mass 0.728 4.44 9 465
50% by mol
6 28% by mass 0.706 2.96 8 708
50% by mol
9 28% by mass 0.741 1.31 7 1560
Table 1: Summary of Data Collected, Rotation III

Figure 2: Reflux ratio vs. energy required to obtain basis of 100 g Ethanol
 Figure 3: Reflux ratio vs. number of effective stages calculated via Smoker-Rose analysis

Figure 4: Reflux ratio vs. average distillate composition calculated via Smoker-Rose analysis
A2. Schematic of Process

Figure 5: Schematic of BDC test column [1]

A3. Cost Analysis

What follows is a brief cost analysis based on findings from our specific BDC unit. It should be
noted that this BDC is much smaller than what would be feasible for a processing plant and as
such the estimates here could change significantly upon scale up.

Simply put, we can calculate a cost from the value of the final product, and subtract the cost of raw
materials and electricity. Cost of operating the unit and maintenance are beyond the scope of this
analysis.

Product value is the value of what was produced from the BDC. Ethanol was expensed at $1.138
per kg and water at $1 per 1000 kg. The material cost was made similarly, as each reflux ratio
utilized a 50% initial mass charge.

Electricity cost is based on producing 100 grams at the cost of $16.8 per GJ.

Reflux Ratio Product Value [$] Material Cost [$] Electricity Cost [$] Final Profit [$]

3 13.53 2.05 0.0078 11.47

6 8.91 2.05 0.0118 6.85

9 4.02 2.05 0.0262 1.94

 Table 2: Cost analysis for data collected in rotation III

*Labor cost depends on the size of the batch distillation column and the cost of hiring, training, and
supporting operators and maintenance workers. As the rotations have not been provided with the
company’s specific profit goals, the names of equipment providers, or hiring information, Rotation
III is unable to make a more detailed analysis.