Problem statement

The ethanol purification process is pivotal for biofuel production, but scaling up production
capacity poses challenges in maintaining optimal column design and performance. One significant
concern is the occurrence of flooding and weeping within the distillation column, phenomena that
can severely compromise separation efficiency and product quality. Despite existing research
acknowledging these issues, there is a notable gap in understanding how poor column internal
specifications contribute to flooding and weeping, particularly in the context of increased
production capacity. The lack of a comprehensive analysis hinders the development of effective
strategies to prevent or mitigate these operational challenges.

Existing knowledge primarily focuses on the general impacts of flooding and weeping, but there
is insufficient insight into the specific role poor column internal specifications play in exacerbating
these issues while using design process parameters. Also, as the production capacity increases, the
potential for operational inefficiencies and product quality degradation intensifies because of
system’s susceptibility to flooding and weeping. Understanding the nuanced interplay between
inadequate internal specifications, increased production demands, and the occurrence of flooding
and weeping is crucial for refining the design and operational strategies of distillation columns.
This research aims to fill the gap by systematically investigating how poor column internal
specifications contribute to flooding and weeping during the scaling up of production capacity.

Objectives

General objective
To develop a comprehensive and precise simulation model for the ethanol purification process,
avoiding flooding and weeping while maximizing operational performance with ASPEN plus.

Specific Objectives

1. To develop an ethanol-water distillation column in ASPEN plus.

2. To study and find the optimum design specification parameters (reflux ratio and boil up
ratio) in response to the distillate (ethanol product stream, ethanol mass fraction in the
distillate column, and operating cost per hour).
3. To investigate and optimise the column hydraulics for proper simulation and industry
operations while using the optimised parameters to avoid flooding and weeping.

Significance

The significance of this research is paramount in addressing critical challenges within the ethanol
purification process, particularly as it pertains to scaling up production capacity. Ethanol, a vital
component of biofuel production, plays a pivotal role in the transition toward sustainable energy
sources. The ability to efficiently produce ethanol at an increased scale is crucial for meeting the
growing global demand for biofuels and reducing reliance on conventional fossil fuels. However,
the scalability of the ethanol purification process is hindered by the occurrence of flooding and
weeping in distillation columns.

Understanding how poor column internal specifications contribute to flooding and weeping is of
utmost importance. These phenomena not only compromise the separation efficiency of the
distillation process but also jeopardize the quality of the product. By addressing this research gap,
the study aims to provide valuable insights into the nuanced interplay between inadequate internal
specifications, heightened production demands, and the occurrence of flooding and weeping. Such
insights have direct implications for the biofuel industry, enabling engineers and designers to
optimize distillation column designs and operational strategies.

Moreover, the significance of this research extends beyond immediate practical applications. The
findings will contribute to the academic understanding of distillation column behavior under
varying operational conditions. This knowledge is essential for advancing the field of chemical
engineering and process optimization. Additionally, as the world seeks sustainable alternatives to
traditional energy sources, the research outcomes will directly contribute to the development of
more efficient and environmentally friendly biofuel production processes.

Justification

The justification for this research stems from the critical need to overcome operational challenges
in ethanol purification, a process integral to the production of biofuels. As the global demand for
sustainable energy sources continues to rise, the biofuel industry faces the imperative of increasing
production capacity. However, the scalability of ethanol purification processes is hindered by the
complex phenomena of flooding and weeping within distillation columns.

One key aspect of the justification lies in the economic implications of these challenges. The
occurrence of flooding and weeping can lead to reduced separation efficiency, lower product
quality, and increased operating costs. Addressing these issues is vital for ensuring the economic
viability of biofuel production, as inefficient processes can undermine the competitiveness of
biofuels in the energy market.

Furthermore, the environmental impact of biofuel production is closely tied to process efficiency.
Inefficient distillation processes not only contribute to higher greenhouse gas emissions but also
diminish the overall sustainability of biofuels. By investigating the role of poor column internal
specifications in flooding and weeping, this research directly aligns with the broader goal of
developing more sustainable and environmentally friendly energy solutions.

The technological advancements in the ethanol purification process are contingent upon a
comprehensive understanding of the underlying issues. This research aims to fill a critical gap in
knowledge by providing a systematic analysis of how inadequate internal specifications contribute
to flooding and weeping, particularly in the context of scaling up production capacity. The
outcomes of this study will not only enhance the efficiency of biofuel production but also
contribute valuable insights to the broader field of chemical engineering.

Scope
1.5.1 Geographical Scope

The case study for the research project was SCOUL.

1.5.2 Technical Scope

The project adopted use of ASPEN Plus to design, simulate and optimise the design and hydraulic
parameters of the distillation column.

1.5.3 Time Scope

The research covered a period of five months that is from November 2023 to March 2024.
CHAPTER THREE: METHODS AND MATERIALS

Overview

Distillation is one of the most important separation techniques used in various industries, such as
petrochemical, chemical, and pharmaceutical industries, to separate and purify liquid mixtures into
their individual components. The success of the distillation process depends on the design and
operation of the distillation column, which comprises a series of trays or packing material that
allows for the separation of the components based on their boiling points. The process involves
heating the mixture, allowing it to vaporize, and then condensing the vapors back into a liquid.
The efficiency of the distillation process is influenced by several factors, such as column diameter,
number of trays, packing type, reflux ratio, and operating pressure, among others.

Research Instruments

Aspen Plus was used to design and simulate the pyrolysis process. Aspen Plus is a powerful
process simulation software tool widely used in the chemical engineering industry for designing
and optimizing processes. It provides a user-friendly graphical interface for constructing process
flowsheets and running simulations to analyze process behavior under various operating
conditions. Aspen Plus uses various thermodynamic models to accurately predict the behavior of
different process components and can simulate various unit operations such as distillation,
reaction, and separation processes. It also allows for the simulation of heat and mass transfer
processes and can predict the properties of various process streams. The software has an extensive
library of components and thermodynamic models, allowing for the modeling of complex
industrial processes. One of the most powerful features of Aspen Plus is its ability to optimize
process performance using a range of optimization tools. The software can perform sensitivity
analysis to identify critical variables affecting process performance and use them to optimize the
process design. It can also perform economic analysis to evaluate the profitability of the process
and identify areas for improvement. Aspen Plus is widely used in the chemical process industries
to design and optimize various processes such as distillation, reaction, and separation processes. It
is also used to model and simulate various energy systems such as gas turbines, power plants, and
refrigeration cycles. The software's versatility and user-friendly interface make it a valuable tool
for engineers, researchers, and students in the field of chemical engineering.

Column design

Specific objective 1 was achieved by successfully designing and running a distillation simulation
model. A RadFrac distillation column was modelled in the simulation environment. The first step
was component specification. The Case study of the research was SCOUL (Sugar Corporation of
Uganda Limited). As such, the components to the purifier distillation column were ethanol and
water.

Component Type Component name Alias

ID
ETHANOL Conventional ETHANOL C2H6O-2
WATER Conventional WATER H2O

Thermodynamic method

The selection of an appropriate thermodynamic package is a critical aspect of process simulation,

especially when dealing with complex separation processes such as distillation. In this research
project, the Soave-Redlich-Kwong (SRK) thermodynamic package was chosen.
The SRK equation of state was chosen because it was capable of accurately predicting phase
behavior and equilibrium properties of hydrocarbon and non-polar mixtures. The SRK equation
provides an accurate representation of the complex interactions between ethanol and water during
the separation. Furthermore, the STEAMNBS was chosen along the SRK thermodynamic method
in consideration of the presence of water vapor in equilibrium with the liquid water.

Feed specification

The initial composition of the feedstock was analysed from SCOUL (Sugar Corporation of Uganda
Limited). The feed specifications were the same for all the different simulation cases. The adopted
Feed specifications are shown in the table below:

State Variables
Temperature 30 C
Pressure 1 bar
Total flow basis Mass
Total flow rate 1000 Kg/hr
Composition Mass Fraction
Ethanol 0.1
Water 0.9

The RadFrac specifications are shown in the figure below.

Reflux and boil up ratio variation.

The reflux and boil up ratios were varied independently varied between 1 and 10. For each
variation, the other parameter was help constant at 1. The distillate mass flow, ethanol mass
fraction in the distillate were recorded. Also, the operating energy cost per hour was evaluated and
recorded for every simulation. This figure was evaluated with the cost estimation analysis was
automatically performed using ASPEN Process Economic Analyzer (APEA).

Hydraulic analysis and optimisation

This was performed with the column analysis tools in ASPEN Plus. The hydraulic analysis found
in the column internals section of the modelled column. The hydraulic data was then generated by
the simulation.
 This created an internal section for the column and the internals specified. The column was
specified to have 2 sections that is stage 2 (below the condenser stage) up to stage 21 just above
the feed stage and then from stage 22 to stage 35 above the reboiler stage. These sections were
modelled as shown below. sieves internals were selected.

Tray Tray Diameter

Details Spacing/Section
Packed Height
Name Start End Mode Internal Tray/Packing Number of Passes
Stage Stage Type Type
CS-1 2 21 Interactive Trayed BUBBLE-CAP 1 0.6096 m 0.4396 m
sizing
CS-2 22 35 Interactive Trayed BUBBLE-CAP 1 0.6096 m 0.46624 m
sizing

Column hydraulics optimization

This was conducted by adjusting tray spacing and column diameter to avoid entrainment and
flooding.

Data Analysis
The data was analyzed using statistical methods, descriptive and referential analysis for each phase
of assumptions, questions, objectives, or problems. Statistical package for excel for Microsoft
office was used to analyze the data collected and interpretation was presented using bar graphs and
tables.

CHAPTER FOUR: RESULTS AND DISCUSSIONS

Distillation column design

Ethanol/water separation was performed in a RadFrac distillation column as shown in figure

above. The column was modelled with 1 inlet (FEED) and 2 outlets (TOPPROD, BOTTOMS).
The FEED stream was specified as from the fermentation units of SCOUL. The TOPPROD was
the distillate stream after distillation and contained a higher concentration of ethanol as compared
to the BOTTOMS stream that contained higher fractions of water. The table below shows the
simulation results at reflux ratio of 1 and boil up ratio of 1.

Units FEED BOTTOMS TOPPROD

Mass Flows kg/hr 1000 662.62 337.38
ETHANOL kg/hr 100 0.00 100.00
WATER kg/hr 900 662.62 237.38
Mass Fractions
ETHANOL 0.1 0.00 0.30
WATER 0.9 1.00 0.70

The feed, consisting of 100 kg/hr of ethanol and 900 kg/hr of water, entered the distillation column
at a total flow rate of 1000 kg/hr. The bottoms product stream, with a mass flow of 662.62 kg/hr,
primarily contained water, indicating successful separation of ethanol. Meanwhile, the top product
stream had a mass flow of 337.38 kg/hr, predominantly comprising ethanol. This result signifies
the effective concentration of ethanol in the top product. The distillation column operates by
exploiting the different boiling points of ethanol and water. As the mixture is heated within the
column, ethanol, with its lower boiling point, vaporizes more readily. The ascending vapor cools
down in the column, and condenses to form the top product, effectively concentrating ethanol. The
remaining liquid in the column, with a lower ethanol concentration, is collected as the bottom
product.

However, the distillation process is not only sensitive to vapor-liquid equilibrium of the
components but also expensive and so the need for designers to optimise the design parameters.
In this section, results from the study and optimisation of reflux and boil up ratios in effect to
ethanol concentration and energy cost variations are shown.

Boil up ratio variation at reflux ratio specification of 1.

The table below gives the summary of results obtained at different values of boil up ratio simulated
at reflux ratio specification of 1.
 Boil up ratio Distillate mass Ethanol mass fraction in Operating energy cost
flow distillate (USD/hr)
1 339.604 0.294 14.76
2 499.646 0.200 22.48
3 597.007 0.168 27.2
4 662.632 0.151 30.4
5 709.879 0.141 32.69
6 745.521 0.134 34.42
7 773.366 0.129 35.77
8 795.720 0.126 36.85
9 814.061 0.123 37.74
10 829.381 0.121 38.48

Variation of distillate mass flow against molar boil up ratio at reflux ratio specification of 1.

As the boil-up ratio increased from 1 to 10, the distillate mass flow rates also increased. This trend
is consistent in distillation processes. A higher boil-up ratio means more heat is being supplied to
the column, leading to increased vaporization of the components.

Distillate mass flow variation

against molar boil up ratio
900.000
Distillate mass fraction

800.000
700.000
600.000
500.000
400.000
300.000
200.000
100.000
0.000
0 2 4 6 8 10 12
Boilup ratio
However, this increase in distillate didn’t significantly mean that more ethanol was separated. So,
a stream component evaluation was conducted to study the mass fraction evaluation of ethanol in
the stream.

Variation of ethanol mass fraction in distillate stream against molar boil up ratio at reflux
ratio specification of 1.

Ethanol mass fraction in

distillate variation against
molar boil up ratio
0.350
Ethanol mass fraction in

0.300
0.250
0.200
distillate

0.150
0.100
0.050
0.000
0 2 4 6 8 10 12
Boil up ratio

An observation was made that as the boil-up ratio increased from 1 to 10, the ethanol mass fraction
in the distillate decreased. Though higher boil-up ratios resulted in increased vaporization of the
more volatile component (ethanol), the distillate became more diluted with the less volatile
component (water). This also supports the earlier observed trend of increasing distillate mass flow.
Like the distillate mass flow trend, there is a diminishing rate of improvement in ethanol mass
fraction at higher boil-up ratios. This is because, as the system approaches its maximum separation
capacity, further increases in the boil-up ratio may not proportionally increase the ethanol mass
fraction. The data suggested that there may be an optimal point for achieving the desired ethanol
concentration in the distillate but there was need to study how the boil up ratio variation affected
energy consumption costs.

Variation of calculated operating energy cost against molar boil up ratio at reflux ratio
specification of 1.
 Operating energy cost (USD/hr)
against molar boil up ratio
45
Calculated cost per hr

40
35
30
25
20
15
10
5
0
0 2 4 6 8 10 12
Boil up ratio

It can be observed that as the boil up ratio increased, the energy requirement and calculated cost
per hour increased gradually. This trend was expected since higher boil-up ratios required more
energy input to provide the necessary heat for vaporization in the distillation column. The increase
in operating energy costs aligned with the trend of increasing distillate mass flow. Higher boil-up
ratios demand more energy to drive the distillation process and produce a higher distillate flow
rate but doesn’t necessarily produce more concentrated ethanol streams.

Reflux ratio variation at reflux ratio specification of 1.

The table below gives the summary of results obtained at different values of reflux ratio simulated
at boil up ratio specification of 1.

Reflux Distillate mass Ethanol mass fraction in Operating energy cost

ratio flow distillate (USD/hr)
1 339.604 0.294 14.76
2 271.890 0.368 16.28
3 231.790 0.431 17.19
4 204.752 0.488 17.8
5 185.346 0.540 18.23
6 170.615 0.586 18.57
7 159.046 0.629 18.84
8 149.699 0.668 19.05
9 141.959 0.704 19.23
10 135.464 0.738 19.37

Variation of distillate mass flow against molar reflux ratio at boil up ratio specification of 1.

Distillate mass flow variation

against molar reflux ratio
400.000
Distillate mass flow

350.000
300.000
250.000
200.000
150.000
100.000
50.000
0.000
0 2 4 6 8 10 12
Reflux ratio (molar)

As the reflux ratio increased from 1 to 10, there was a consistent decrease in the distillate mass
flow rates. This trend is anticipated in distillation processes and can be attributed to the
fundamental role of the reflux ratio in affecting the separation efficiency and product composition.
A higher reflux ratio signifies a greater fraction of the condensed vapor being returned to the
column as liquid reflux. This increased reflux has several impacts on the distillation process. A
higher reflux ratio improves the column's ability to separate components by providing more
opportunities for vapor-liquid equilibrium to occur. This results in a greater concentration of the
more volatile component (ethanol) in the vapor phase. The increased reflux reduces the amount of
vapor that rises through the column. Therefore, the overall distillate mass flow decreases because
less vapor is being condensed and collected as the top product. So, a mass fraction analysis was
performed.

Variation of ethanol mass fraction in distillate stream against molar reflux ratio at boil up
specification of 1.
 Ethanol mass fraction in
distillate variation against
molar reflux ratio
0.800
Ethanol mass fraction in

0.700
0.600
0.500
distillate

0.400
0.300
0.200
0.100
0.000
0 2 4 6 8 10 12
Mlar reflux ratio

As the reflux ratio increased from 1 to 10, there was a noticeable rise in the ethanol mass fraction
in the distillate. This trend aligned with the fundamental principles of distillation and reflects the
impact of the reflux ratio on separation efficiency and product composition. A higher reflux ratio
implied a greater proportion of the condensed vapor being returned as liquid reflux. As such,
increasing the reflux ratio improved the separation of ethanol from the mixture. The higher reflux
provided additional opportunities for vapor-liquid equilibrium, leading to a more concentrated
ethanol vapor rising through the column. The higher reflux ratios result in a reduction of less
volatile components (water) in the distillate. Therefore, the ethanol mass fraction in the distillate
increased because the distillate became more enriched with ethanol.

Variation of calculated operating energy cost against molar reflux ratio at boil up ratio
specification of 1.
 Operating energy cost
(USD/hr)
25
Operation energy cost per hour

20

15

10

0
0 2 4 6 8 10 12
Molar reflux ratio

As the reflux ratio was increased from 1 to 10, there was a slow upward trend in operating energy
costs. This trend was expected and attributed to the fundamental role of the reflux ratio in
influencing the energy requirements for the distillation column. However, the increment is lower
as compared to that of the increase in the boil up ratio. As such, an optimisation analysis was
performed between the two design ratios to obtain the required concentration.

Optimization of operating parameters for optimal ethanol concentration in the top product
stream with minimal operating energy costs.

The optimised figures were obtained by studying the two factors and running the simulation for
obtaining appropriate concentration.

After optimisation Before optimisation

Reflux ratio 3 1
Boil up ratio 1 1
Ethanol Mass fraction 0.434 0.296
Operation cost per hour (USD/hr) 17.13 14.74

Before optimization, the reflux ratio was 1, and the ethanol mass fraction in the distillate was
0.2964. After optimization, the reflux ratio increased to 3, leading to a significant improvement in
the ethanol mass fraction, which increased to 0.4340. This is consistent with earlier analyses,
where higher reflux ratios were associated with enhanced ethanol enrichment in the distillate. The
optimization process successfully exploited this relationship to achieve a higher ethanol
concentration in the final product. Before optimization, the operating cost per hour was 14.74
USD, and after optimization, it increased to 17.13 USD. The increase in operating cost is expected
when refining the separation process to achieve higher product purity and concentration. This is
consistent with the earlier analysis where higher reflux ratios, associated with the optimization
process, led to increased operating energy costs. The trade-off between product quality and
operational cost is evident in the optimized results.

Ethanol mass fraction in

distillate
0.5
0.45
0.4
0.35
0.3
0.25
0.2
0.15
0.1
0.05
0
Before optimisation With optimisation

Column hydraulic analysis

A column hydraulic analysis was performed on the optimized designed parameter results in
ASPEN plus to further observe, study and optimise the hydraulic performance of the column. The
figure below represented the initial state of the column.

Initial hydraulic analysis

From the produced column diagram above, despite the column design parameters being fully
converged and optimized to give the optimum separation, the fluid hydraulics in the column were
not properly configured. There are often 3 colours: blue, red, and yellow. The blue color of a
column indicates stable flow within the column, yellow indicates flow near stability limit while
red indicates out the limit. This is a major industrial constraint because the operating conditions
(mostly product requirements) vary time to time and the failure to configure the column hydraulics
implies plant inefficiencies. Column hydraulics simulation was conducted on the designed column
with the optimised reflux and boil up ratios. Hydraulic plots were generated for each stage.
Hydraulic plots for stage 5 and 32 are shown blow.
Stage 5 was chosen randomly in the specified upper section of the column that is (stage 2 to 21)
and incidentally it was operating outside the entrainment level. This implied that the whole of this
section suffered from weeping.

For section 2 below the feed, the operating conditions were very close to the operating conditions
and so the column hydraulics too, needed to be configured and optimized. These were adjusted to
cater to up to 40% increase in column capacity without the need for changing the column sizes in
such a way that weeping and flooding are avoided.

Results for optimised hydraulic parameters of the column.

Section1
Property Value Units
Section starting stage 2
Section ending stage 21
Calculation Mode Sizing
Tray type SIEVE
Number of passes 1
Tray spacing 0.9096 meter
Section diameter 0.435821 meter
Section height 18.192 meter
Section pressure drop 0.171254 bar
 Section head loss (Hot liquid 1943.719 mm
height)
Trays with weeping None
Section residence time 0.051845 hr
Section 2
Section starting stage 22
Section ending stage 35
Calculation Mode Sizing
Tray type SIEVE
Number of passes 1
Tray spacing 0.6096 meter
Section diameter 0.46624 meter
Section height 8.5344 meter
Section pressure drop 0.110306 bar
Section head loss (Hot liquid 1254.313 mm
height)
Trays with weeping None
Section residence time 0.014084 hr

The results in the table above show the different hydraulic design specifications and generated data
for the column to ensure no weeping and flooding is encountered up to 40% production increase.
In Section 1 of the analysis, the modifications are evident in the tray spacing, section diameter,
and section height. These adjustments were strategically made to facilitate a higher number of
trays within the given column dimensions. The increase in tray spacing to 0.9096 meters allowed
for better vapor-liquid contact, contributing to improved separation efficiency. Similarly, the
adjustments in section diameter (0.435821 meters) and section height (18.192 meters) indicate a
careful balancing act to maintain structural integrity while accommodating increased column
capacity.
An optimised hydraulic column

From the new hydraulic simulation, it was evident that the column now was operating within the
safe limits. Further plots were obtained for stages 5 and 32 to elaborate the difference.
The section pressure drop, and head loss are crucial parameters in assessing the hydraulic
performance of the column. The reported values (0.171254 bar and 1943.719 mm, respectively)
demonstrated the system's ability to handle increased liquid and vapor flow without compromising
operational stability. The absence of weeping on the trays is indicative of the success in preventing
undesired liquid bypassing.
CHAPTER FIVE: CONCLUSIONS AND RECOMMENDATIONS

Conclusions

The optimization of the distillation process, particularly adjusting reflux ratios, successfully
improved the ethanol mass fraction in the distillate.

The optimization, while improving product quality, comes at the cost of increased operating energy
expenses. Balancing the desired ethanol concentration with economic considerations is crucial for
practical and cost-effective process operations.

The hydraulic analysis, with adjusted parameters to accommodate a 40% increase in column
capacity, showcases a systematic approach to enhance the distillation column. The absence of
weeping and flooding, coupled with pressure drop and head loss considerations, indicates
successful hydraulic adaptation to higher throughput.

The combination of simulation, optimization, and hydraulic adjustments has resulted in an

improved ethanol purification process.

Recommendations

Investigate advanced control strategies to dynamically optimize reflux ratios and other key
parameters in response to changing feed compositions and operating conditions.

Develop dynamic simulation models to assess the real-time impact of varying conditions on
process performance, providing insights for more robust control and optimization strategies.

Conduct a life cycle assessment to evaluate the environmental impact of the ethanol purification
process, considering factors beyond operational energy costs.

Investigate the use of different tray designs and materials to further enhance vapor-liquid contact
efficiency and overall column performance.