School of Chemical Engineering

Faculty of Engineering
The University of New South Wales

CEIC3004

Process Equipment Design

Term 1 – 2022

Biodiesel Production from Algae Cultivated in Coal Seam Gas Wastewater

Design Report Draft

Date of Submission: 16/03/2022

Group 8

Name Student ID Email

Nathaniel Breen z5255133 z5255133@ad.unsw.edu.au
Zhan Huang z5255133 z5255133@ad.unsw.edu.au
Anthony Lam z5113512 z5113512@ad.unsw.edu.au
Christina Lim z5255133 Z5237238@ad.unsw.edu.au
Ruichen Ma Z5237238 Z5237238@ad.unsw.edu.au
Kristina Murphy z5207247 kristina.murphy@student.unsw.edu.au

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Document Control
REV DATE DESCRIPTION EDITOR REVIEWED
1 1/03/22 Document creation, initial formatting CL, KM NB, AL, RM
2 4/03/22 Copied in PFD NB All
3 5/03/22 Draft Extended Process Narrative finished NB, RM CL, AL, ZH, KM
4 8/03/22 Equipment selection finalised and justifications commenced All All
5 8/03/22 Draft executive summary added Anthony All
6 16/03/22 Draft finalised for submission All All

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Executive Summary
Current coal seal gas mining methodologies are prone to environment and health implications, namely the
contamination of adjacent freshwater aquifer purposed as a fresh water drinking supply. Thus, the venture
of coal seam gas mining has led to growing tensions between communities, involving companies,
farmers, and landowners. In response, the method of producing bio-oi from algae cultivated in CSG water
has been investigated.

The design proposed conforms to the provide criteria of 550 hectares of land and considerations have
been made to facilitate an annual algal biodiesel productivity of 1,500,000 litres. A brief outline of the
plant operation addresses the processes involved to be water treatment, algal cultivation, bio-oil
extraction, bio-oil stream treatment, transesterification, by-product purification, and product recovery
along with the corresponding equipment chosen for the implementation of these processes.

This report details an investigation into the equipment selection of the bio-oil production plant and
utilises selection techniques of MCDA and SWOT analysis, a complementary summary of justification
for each component to explain the selection process has also been provided. The components selected for
the project are “insert list of equipment” and an PFD, FST has been provided containing all the above
components. In addition to the equipment summary tables, calculations based on designs and the material
and energy balances are also demonstrated within the report.

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Contents
1 Introduction.........................................................................................................................................1

2 Process Overview................................................................................................................................1

2.1 Process Narrative.........................................................................................................................1

2.2 Process Flow Diagram.................................................................................................................2

3 Process Equipment..............................................................................................................................2

3.1 CSG Water Treatment.................................................................................................................2

3.2 Flotation Column.........................................................................................................................3

3.3 Hydrothermal Liquefaction..........................................................................................................4

3.4 Methanol & Sodium Hydroxide Mixer........................................................................................4

3.5 Heat Exchanger............................................................................................................................4

3.6 Transesterification Reactor..........................................................................................................5

3.7 Centrifuge....................................................................................................................................6

3.8 Methanol & Biodiesel Separator..................................................................................................7

3.9 Crude Biodiesel Purification........................................................................................................7

3.10 Crude Glycerol Purification.........................................................................................................8

4 References...........................................................................................................................................9

5 Appendices........................................................................................................................................11

Appendix A...........................................................................................................................................11

Appendix B............................................................................................................................................11

Appendix C............................................................................................................................................12

Appendix D...........................................................................................................................................12

Appendix E............................................................................................................................................13

Appendix F............................................................................................................................................13

Appendix G...........................................................................................................................................14

Appendix H...........................................................................................................................................15

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 Appendix I.............................................................................................................................................15

Appendix J.............................................................................................................................................16

Appendix K...........................................................................................................................................17

Sample calculations of reactor volume..............................................................................................17

Tables and Figures

Figure 1: Preliminary Process Flow Diagram for Biodiesel Production from CSG Wastewater................2

Table 1: MCDA for Raw CSG Water Treatment Method...........................................................................11

Table 2: SWOT Analysis for Algae Harvesting Technologies....................................................................11

Table 3: SWOT Analysis for Bio-oil Production Method...........................................................................12

Table 4: SWOT Analysis for MeOH & NaOH Mixer.................................................................................12

Table 5: SWOT Analysis for MeOH & NaOH Heater...............................................................................13

Table 6: SWOT Analysis for Transesterification Unit...............................................................................13

Table 7: SWOT Analysis for Biodiesel & Glycerol Separation..................................................................14

Table 8: SWOT Analysis for MeOH & Biodiesel Separation.....................................................................15

Table 9: SWOT Analysis for Biodiesel Washing Unit................................................................................15

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1 Introduction

2 Process Overview
2.1 Process Narrative
Water injected to the rock is used to break the coal seam during the coal seam gas mining. However, this
step brings the saline water to the ground which case the water pollution issue. This project is aiming to
build a demonstration plant within 55 hectares and use CSG water grows the algal to produce biodiesel
1,500,000 litres/year. The plant mainly includes three parts: CSG water cultivate the algal, bio-oil
extraction and transesterification, biodiesel and by-products refine.

Initially, raw CSG water from mining lease is collecting in a holding tank and pumped to the microfiltration
unit where remove the suspended solids and some dissolved salt. After purified, CSG water enters a
raceway pound with the nutrient doing system, the total footprint of raceway pound is 1000 x 450 m. 1v/v%
carbon dioxide continues aerate to the raceway pound to cultivate the algal by diffusers.

As the concentration of biomass reaching a suitable level, it goes to the second part of the process.
Harvesting the algal have been done by a flotation column. Chitosan is a potential additive in this stage to
increasing the flotation efficiency and low toxicity. Both the effluent from flotation column and
hydrothermal liquefaction unit were recycle though ceramic microfiltration for further use. Then the wet
algal stream enters a hydrothermal liquefaction unit to extract the bio-oil at 300°C and the dry biomass
leave the process. The hot bio-oil is cooling down to 40°C that suitable for transesterification reaction
happens by a shell and tube heat exchanger. At the same time, 8 times bio-oil methanol (in mole base) and
1.4wt% of bio-oil sodium hydroxide as catalyst were mixing by the injection inline mixing at room
temperature, then heated up to 40°C though another shell and tube heat exchanger. The bio-oil and mixture
of methanol/sodium hydroxide take a transesterification reaction in a Continuous Ultrasonic Reactor at
1atm to produce crude biodiesel.

The crude biodiesel comes out include excess methanol, biodiesel, and glycerol. The crude biodiesel and
crude glycerol are separated by centrifugation because of the density different. Then crude glycerol goes to
a neutralisation tank where the addition of acid promotes precipitation of salts. These salts are removed by
filtration, and a vacuum distillation column is used separate glycerol from methanol and water. The
glycerol is then absorbed onto activated carbon to remove any remaining impurities and achieve a purity of
98%. The crude biodiesel is separated though a distillation column due to the volatilities different, it
achieves around 98% recovery of methanol. The top product of distillation column is nearly the pure
methanol which recycle back to the inline mixer; bottom product is the impure biodiesel transfer into the
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final separation unit. The final separation unit include two parts: the washing column and drying column.
The washing column is spray washing, the water and crude biodiesel ratio is 3:1 where the water is the
recycle effluent after the wastewater treatment unit. The vacuum drier is the final step which evaporate the
water from biodiesel at room temperature.

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 2.2 Process Flow Diagram

Figure 1: Preliminary Process Flow Diagram for Biodiesel Production from CSG Wastewater
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3 Process Equipment
Footprint table- copy and modify for your equipment 😊

name
Design Temperature (°C)
Design Pressure (bar)
Shape & orientation
Height (m)
Diameter (m)
Footprint (m2)

3.1 CSG Water Treatment

Raw CSG water is not ideal for cultivating algae as the high turbidity can inhibit light penetration, thus
limiting photosynthesis. Elevated salinity has also been speculated to prohibit algae growth and processes
such as reverse osmosis (RO) filtration are suggested to decrease saline levels prior to inoculating with
algae cultures (Hamawand et al., 2014). Buchanan et al. (2013), disproved the negative effects of salinity
in their experiment comparing algae growth in CSG water with salinities of 1.7g and 11.6g TDS/L. While
algal growth was delayed in the higher salinity solution, after 20 days there was negligible difference of
algae concentrations in both solutions. A higher salinity has also been shown to improve algae growth for
certain species such as D. tertiolecta which has an optimal salinity of 10g NaCl/L (Aravinthan &
Harrington, 2014).

Accordingly, the unit need not remove dissolved salts but must be effective in removing suspended solids.
While RO filtration was considered as it has been commonly used in treating CSG water and experiences
significantly less fouling than other membranes, ultimately the excessive cost and low flux rate prevented it
from being the best option. Microfiltration (MF) was chosen as it is effective in capturing suspended solids,
is cheaper and has a significantly higher flux rate. A MCDA analysis for this unit can be found in Appendix
A.

3.2 Flotation Column

This unit aims to harvest algae after algae cultivation in the raceway ponds. Harvesting the algae is
estimated to account for up to 30% of the total cost of production, and as such, this unit must be a cost-
effective method of algae retrieval (Alkawari et al., 2018). Yield of algae should also be highly considered
alongside any potential damages to the algae cells that may occur, limiting bio-oil extraction in subsequent

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units. While the current cheapest method of harvesting is gravity sedimentation, the process is slow and
requires a large footprint. Given the constraint of land usage, flotation is a highly viable method as it has a
small footprint while maintaining a moderate cost and high recovery rate (Liu et al., 1999). This method
also has an advantage as microalgae tends to move upward, optimising high overflow rates (Laamanen et
al., 2016). Although centrifugation has a higher yield than flotation, this method is expensive and can cause
damage to algae cells prohibiting it from being a viable method of bulk harvesting. A SWOT table
comparing different separation methods for this unit can be found in Appendix B.

Flocculation is often used in combination with flotation as it can increase the efficiency of the process. The
impact on downstream processes, as well as environmental impacts of effluent water must be carefully
considered in respect to any coagulant added to flocculate the algae. Common additives include metallic
salts, polymers, or bio-flocculants. A large concern for most flocculants is toxicity and possible
contamination of the biomass. Chitosan is an organic compound that has been found to have low toxicity
and negligible effect on any downstream processes (Laamanen et al., 2016). Additionally, it has been found
to coagulate more effectively than common flocculants such as aluminium sulphate. The main drawback of
this flocculant is the expense as it has proven to be cost prohibitive, however the choice of flotation column
for the harvesting method as opposed to centrifugation accommodates for the usage of chitosan.

3.3 Hydrothermal Liquefaction

The purpose of this unit is to serve as a reactor for the thermochemical conversion of algae into bio-oil,
along with gaseous, aqueous, and solid by productions. The implementation of HTL is advantageous due to
the potential of being able to eliminate and reduce the requirement of a drying process for the feedstock.
Conversely alternate technologies of pyrolysis and gasification are economically unappealing due to the
requirement of a drying process (S. Amin,2009). The reactor will operate at the optimal temperature of
300C for the highest yield as reported in literature producing 29.37% wt. of bio-oil, (J. Arun, et al ,2018) .

The selection of HTL was performed based not only on the qualities of the produced crude bio-oil but the
various exits streams have also been considered. Algal biochar is a carbon rich charcoal that is produced as
residue during HTL, this biochar can be utilised as in the agriculture industry as a soil ameliorant to
enhance the nutrient and water retention capacity of soil (Cayuela et al., 2013) Additionally bio char is a
suitable adsorbent for the removal of metal dyes and other pollutants from wastewater. (Asha.S, et al,2021).
In line with the design objectives of economic viability and efficiency HTL is further justified by the
analysis of post HTL wastewater containing 80% of feedstock nutrients and low amount or organic
compounds which can be recycled to the algae cultivation process and allows for the optimisation towards a
higher bio-energy production from per unit biomass (P. Biller, et all 2012). A SWOT Analysis for this unit
can be found in Appendix C.

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3.4 Methanol & Sodium Hydroxide Mixer
The mixer is aiming to provide a well-mixed mixture though the heat exchanger to participate the
transesterification reaction with a low cost. Inline mixing is an economical way of continues mixing the
feed that viscosity below 50 mNs/m2 (Sinnott, 2005), both of methanol and sodium hydroxide solution are
in this range. Although stirred tank mixer also used in liquid-liquid mixing, inline mixing produces a
turbulent fluid which increasing the efficiency of heat exchanger in downstream (Couper & Fair, 2009) The
sodium hydroxide is a catalyst of transesterification reaction, it has less flow rate than methanol. (J.K.
Efavi, 2018) Major criteria of this design is the desired degree of the mixing, the energy consumption and
the cost. Therefore, injection model of inline mixer would be a preferred option for mixing the methanol
and sodium hydroxide based on it economically provides high quality feed to downstream. Appendix D
show a SWOT table of inline mixing.

3.5 Heat Exchanger

The purpose of this unit is to bring the process fluids, Sodium Hydroxide and Methanol, up to the
temperature required within the Continuous Ultrasonic Reactor (CUR). The reaction will occur at 40°C as
this provides the highest bio-diesel yield at the chosen reaction parameters. Thus, the heat exchanger unit
will need to increase the temperature of the process fluids from ambient temperature, assumed to be room
temperature or about 25°C, to the final reaction temperature 40°C. For this application a Shell and Tube
Heat Exchanger (STHX) has been chosen as it combines efficient heat exchange with ease of
construction/maintenance and a relatively small footprint (Walas, 1988). Plate and Frame Heat Exchangers
(PFHX) are accepted to be more thermally efficient than STHX (Sinnott, 2005), especially at very high
temperatures, however, due to the low heat duty required a heat exchanger with maximal thermal efficiency
is not necessary and thus a STHX will suffice. Further, STHX are capable of handling higher flowrates than
other heat exchanger options (INSERT CITATION) which is important for this application given the
required yearly production rate of 1,500,000 litres of biodiesel. Additionally, corrosion and the resultant
need for maintenance is an important factor to consider. Pure methanol which is to be used as the reactant
m2 K
in the CUR is not a particularly fouling substance having a fouling factor equal to water of 1.5 ×10−4
W
(Costa & Queiroz, 2008) and sodium hydroxide is an anti-fouling agent, often used in the cleaning of heat
exchangers to remove organic matter. Further, sodium hydroxide does not react readily with carbon steel
with corrosion rates of < 0.1mm/year and thus the heat exchanger tubes will not require replacing regularly
due to corrosion, greatly reducing maintenance costs across the life of the plant. Contrast this with a PFHX
which require speciality rubber gaskets made of compounds resistant to basic fluids which are expensive to
source and would need replacing more frequently than the tubes in a STHX, increasing maintenance costs.
Finally, in comparison to the notably space efficient PFHX, STHX are not incredibly economical on space
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but due to the low heat duty required, the length and number of tubes required will be small and thus the
volume of the heat exchanger will also be small, thus mitigating the issue of increased footprint of a STHX
when compared to a PFHX. For these reasons a STHX has been chosen over a PFHX for the heating of the
process fluids for use in the CUR. A SWOT Analysis of this unit can be found in Appendix E.

3.6 Transesterification Reactor

The objective of the transesterification reactor is to convert the triglyceride in bio-oil and methanol to
methyl esters (biodiesel) and glycerol. The reaction equation is written as below (Meher et al., 2006):

The bio-oil, mainly composed of

triglyceride, is reacted with methanol under the catalysis of homogeneous catalyst NaOH. The reaction is
reversible; thus, excess methanol is used to force the reaction to the right. The main issue of this reaction is
the immiscibility of methanol and triglyceride, the solubility of methanol in triglyceride is only 6~8% under
60℃ (Boffito et al., 2014). Batch reactor is widely used in biodiesel industry, but it has disadvantages like
labour-intensive, high operational cost, low productivity, and variabilities from batch to batch (Veljković et
al., 2012). CSTRs are more suitable for large scale plant and has much lower operational cost than batch
reactors (Sinnott & Towler, 2019), but their mechanical agitation cannot form fine MeOH-oil emulsions,
limiting the mass transfer and reducing the reaction rate (Boffito et al., 2014). The low reaction rate and
high flowrate require the volume of a single CSTR to be very large or many CSTRs in parallel which
increases footprint.

Continuous ultrasonic reactors are believed to be able to overcome the drawbacks of both batch reactors
and CSTRs (Boffito et al., 2014). The ultrasound can facilitate the reaction by inducing local cavitations
which increase the local temperature, provide both mechanical energy for mixing and activation energy for
initiating the transesterification reaction. As a result, the continuous ultrasonic reactor requires less energy
for agitation, lower reaction temperature and less catalyst than the conventional mechanical agitated reactor
(CSTR) (Jelena et al., 2010). The optimal reaction conditions were suggested by Zou & Chai (2017), which
requires the methanol to bio-oil molar ratio to be 8:1, the mass ratio of alkali catalyst to be 1.4wt% of bio-
oil, the reaction temperature to be 40 ℃ and the residence time to be 55 minutes. A 97% yield of biodiesel
can be attained under suggested conditions. Appendix F shows the SWOT table of transesterification
reactor.

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3.7 Centrifuge
This equipment aims to separate crude biodiesel from crude glycerol before both substances are processed
further. Since both chemicals will be subject to further refining in downstream processes, perfect separation
is not necessary at this stage. Good separation is however desirable as it will increase yield and reduce
wastage. This will allow the plant to achieve its production target more easily and make it more
economical. In industry, the most common methods of removing glycerol from algal biodiesel are gravity
separation and centrifugation (Raman et al, 2019), (Saleh et al., 2010). These processes are most suitable
for the separation because glycerol and biodiesel are immiscible and there is a large difference in density
between the two substances. Distillation columns are not often used in this separation process due their
higher complexity and extremely high operating costs (Demirel, 2006). Appendix G shows SWOT tables
for the gravity settling tank and centrifuge. The main criteria considered in this design decision were the
effectiveness, time taken for separation, footprint, costs and reliability. Centrifugation was chosen for this
process due to its effectiveness and shorter time for separation. While grav ity settling tanks have lower
capital costs and operating costs, the main considerations in line with the project brief are the effectiveness
of the process, footprint and environmental concerns. Centrifuges provide better separation of glycerol and
biodiesel, reducing wastage and increasing final product yields. Better separation also reduces downstream
processing requirements, reducing downstream costs. Centrifuges can achieve separation more quickly and
continuously. If gravity settling tanks were used, multiple tanks may need to be installed, and buffer storage
tanks would need to be used since gravity settling is a batch process. This would increase the footprint
requirements of this separation. This is not desirable considering the footprint constraints defined in the
brief.

3.8 Methanol & Biodiesel Separator

This unit aiming to recycle the high purity of excess methanol to reduce the OPEX and produce biodiesel
for posttreatment. In the transesterification reaction, excess methanol always been added in to keep
completely reaction (Paladino & Neviani, 2022). Even if the crude biodiesel purified though a washing
unit, the large amount methanol is potential for recycle to reduce the OPEX. Due to the large gap of boiling
point and volatilities of methanol and biodiesel, most of industry has choose distillation column as
separation unit in this step, normally it can achieve above 90% methanol recovery. In addition, biodiesel
thermally decompose when the temperature above 250 ℃ , the vacuum vessel usually been selected to
prevent influence the quality of biodiesel (Krunal Suthar, 2019) Flash evaporator is another option in this
process, it can be concerned as a distillation column with single stage which has short process duration and
low equipment cost. However, as increasing the desired recovery of methanol over 90%, the large heat duty
flash off the other chemical component in the bottom product to the top, this decreased the purity of
recycled methanol (Firuz Alam Philip, 2014). The criteria for this design are the purity of recycled

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methanol, recovery, and the cost. The vacuum distillation column was choosing because even the recovery
of methanol reaching 98%, it keeps the mole fraction of methanol in top product around 1(Firuz Alam
Philip, 2014). Appendix H shows a SWOT table between distillation column and flash evaporator.

3.9 Crude Biodiesel Purification

The crude biodiesel contains impurities such as excess caustic catalyst, methanol, soaps, and glycerol (Bart
et al., 2010). Impurities can largely reduce the engine life; therefore, the crude alkyl esters must satisfy
EN14214 standard to be classified as biodiesel (Berrios & Skelton, 2008). The objective of final separation
unit is to remove the impurities of biodiesel to a level that satisfies the relevant standards. There are
generally two methods to purify the crude biodiesel, wet washing, and dry washing. Since water is used in
our product recovery process, the option of dry washing can be ruled out. In addition, dry wash technique is
expensive, and the resultant biodiesel usually needs further separation process such as distillation to meet
the standards (Bart et al., 2010) (Suthar et al., 2019).

There are several recognized wet washing techniques which are spray washing, bubble washing and wash
by stirring (Limmun & Sansiribhan, 2020). However, bubble washing method requires 10% phosphoric
acid for at least 24 hours and the process needs to be repeated 2 to 3 times to get pure biodiesel, thus very
inefficient for large scale plants (Limmun & Sansiribhan, 2020) (Srivastava et al., 2008). The washing by
stirring method requires large amount of water consumption. The water to crude biodiesel ratio must be 3:1
and multistage washing is needed to meet the EN14214 standard (Rahayu& Mindaryani, 2007). Therefore,
spray washing is thought to be the most suitable technique at this stage as it requires less water
consumption and relatively simple equipment. Appendix I shows the SWOT table of biodiesel washing
equipment.

After the wet washing process, the trace water in biodiesel is removed by a vacuum drier which allows
water to evaporate at room temperature (Bart et al., 2010) (Yuan & Yang, 2017).

3.10 Crude Glycerol Purification

This equipment aims to purify the crude glycerol obtained from the centrifuge to achieve a glycerol purity
of at least 98%. While the brief specifies a required concentration of at least 95%, glycerol of higher purity
can be sold more easily and at higher prices. Technical grade glycerine which is suitable for industrial
applications requires a purity of 98% (Quispe et al., 2013). Hence 98% purity was chosen as the design
objective for this process. The main impurities in crude glycerol are salts, water, methanol, and organic
material (Contreras-Andrade et al., 2015), (Pitt et al., 2019). The most common method used in glycerol
purification from bio-diesel production is neutralisation by the addition of an acid followed by filtration for
salt removal, then vacuum distillation, and absorption onto activated carbon (Pitt et al., 2019), (Quispe et
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al., 2013). This can achieve high purity (>99%), however the distillation process is energy intensive, and
hence expensive to run (Contreras-Andrade et al., 2015). An emerging alternative to this process is
membrane filtration. It involves neutralisation by the addition of an acid followed by separation of salts by
gravity settling. The glycerol mixture is then run through an ultra-filtration membrane before being
absorbed onto activated carbon. While this alternative process is simple to operate and has a lower energy
requirement it can only achieve a purity of 93-94% (Chol et al., 2018). This does not satisfy the brief or the
chosen design objective for this equipment. The vacuum distillation process was chosen for the crude
glycerol purification because it can achieve the requirements set out in the brief, and the design objective
chosen. While it is more energy intensive and costly, there are no budget requirements specified for this
project. An MCDA analysis for the crude glycerol purification process can be found in Appendix J. Foot
printing calculations are included in Appendix …

Neutralisation CSTR
Design Temperature (°C) 25
Design Pressure (bar) 1.013
Shape & orientation Vertical Cylinder
Height (m) 0.16
Diameter (m) 0.14
Footprint (m )
2
0.0143

Carbon Absorption Tank

Design Temperature (°C) 25
Design Pressure (bar) 1.013
Shape & orientation Horizontal Cylinder
Length (m) 0.18
Diameter (m) 0.06
Footprint (m )
2
0.034

Centrifuge
Design Temperature (°C) 25
Design Pressure (bar) 1.013
Shape & orientation Vertical Cylinder

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Height (m) 0.20
Diameter (m) 0.20
Footprint (m2) 0.031

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4 References
Abdul Raman, A. A., Tan, H. W., & Buthiyappan, A. (2019). Two-Step Purification of Glycerol as a Value Added by Product
From the Biodiesel Production Process. Frontiers in Chemistry, 7. https://doi.org/10.3389/fchem.2019.00774

Alkarawi, M. A., Caldwell, G. S., & Lee, J. G. (2018). Continuous harvesting of microalgae biomass using foam flotation.  Algal
Research, 36, 125-138.

Aravinthan, V., & Harrington, D. (2014). Coal seam gas water as a medium to grow Dunalliella tertiolecta microalgae for lipid
extraction. Desalination and Water Treatment, 52(4-6), 947-958.

Bart, Jan C. J., Palmeri, Natale Cavallaro, Stefano. (2010). 11.2 Biodiesel Plant Design and Engineering. In Biodiesel Science and
Technology - From Soil to Oil (pp. 467-487). Woodhead Publishing.
https://app.knovel.com/hotlink/pdf/id:kt009L2395/biodiesel-science-technology/biodiesel-plant-design

Bay, K., Wanko, H., Ulrich, J. (2006). Absorption of Volatile Organic Compounds in Biodiesel: Determination of Infinite Dilution
Activity Coefficients by Headspace Gas Chromatography. Chemical Engineering Research and Design, 84(1), 22-28.
https://doi.org/10.1205/cherd.05050

Berrios, M., Skelton, R.L. (2008). Comparison of purification methods for biodiesel. Chemical Engineering Journal, 144(3), 459-
465. https://doi.org/10.1016/j.cej.2008.07.019

Boffito, D.C., Leveque, J.M., Pirola, C., Bianchi, C. L., Vibert, R., Perrier, A., Patience, G. S. (2014). Batch and Continuous
Ultrasonic Reactors for the Production of Methyl Esters from Vegetable Oils. In Production of Biofuels and Chemicals
with Ultrasound (pp.87-114). Springer, Dordrecht. https://doi.org/10.1007/978-94-017-9624-8_3

Buchanan, J. J., Slater, F. R., Bai, X., & Pratt, S. (2013). Algal growth and community structure in a mixed-culture system using
coal seam gas water as the water source. Environmental technology, 34(6), 695-701.

Chol, C. G., Dhabhai, R., Dalai, A. K., & Reaney, M. (2018). Purification of crude glycerol derived from biodiesel production
process: Experimental studies and techno-economic analyses. Fuel Processing Technology, 178, 78–87.
https://doi.org/10.1016/j.fuproc.2018.05.023

Contreras-Andrade, I., Avella-Moreno, E., Sierra-Cantor, J. F., Guerrero-Fajardo, C. A., & Sodré, J. R. (2015). Purification of
glycerol from biodiesel production by sequential extraction monitored by 1H NMR. Fuel Processing Technology, 132,
99–104. https://doi.org/10.1016/j.fuproc.2014.12.016

Firuz Alam Philip, A. V., Adisorn Aroonwilas. (2014). Simulation Analysis of Energy Performance of
Distillation-, Stripping-, and Flash-Based Methanol Recovery Units for Biodiesel Production. Ind.
Eng. Chem. Res., 53, 12770-12782. https://doi.org/doi.org/10.1021/ie5003476
Hamawand, I., Yusaf, T., & Hamawand, S. (2014). Growing algae using water from coal seam gas industry and harvesting using an
innovative technique: A review and a potential. Fuel, 117, 422-430.

Ihsanullah, Shah, Ayaz, Ahmed, & Ali. (2015). Production of Biodiesel from Algae. Journal of Pure and Applied
Microbiology, 9(1), 79–85.

J.K. Efavi, D. K., V. Apalangya,E. Nyankson, E.K. Tiburu, D. Dodoo-Arhin, B. Onwona-Agyeman, A. Yaya,.
(2018). The effect of NaOH catalyst concentration and extraction time on the yield and properties
of Citrullus vulgaris seed oil as a potential biodiesel feed stock. South African Journal of Chemical
Engineering, 25, 98-102. https://doi.org/10.1016/j.sajce.2018.03.002
Jelena M. Avramović, Olivera S. Stamenković, Zoran B. Todorović, Miodrag L. Lazić, Vlada B. Veljković (2010). The
optimization of the ultrasound-assisted base-catalyzed sunflower oil methanolysis by a full factorial design. Fuel
Processing Technology, 91(11), 1151-1157. https://doi.org/10.1016/j.fuproc.2010.06.001

Krunal Suthar, A. D., Milind

Joshipura. (2019). A review on separation and purification techniques for biodiesel
production with special emphasis on Jatropha oil as a feedstock. Asia-Pacific Journal of Chemical
Engineering 14(5). https://doi.org/doi.org/10.1002/apj.2361

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Krunal Suthar, Ankur Dwivedi, Milind Joshipura (2019). A review on separation and purification techniques for biodiesel
production with special emphasis on Jatropha oil as a feedstock. Asia-Pacific Journal of Chemical Engineering, 14(5).
https://onlinelibrary.wiley.com/doi/full/10.1002/apj.2361

Laamanen, C. A., Ross, G. M., & Scott, J. A. (2016). Flotation harvesting of microalgae.  Renewable and Sustainable Energy
Reviews, 58, 75-86.

Limmun, W., Sansiribhan, S. (2020). Water-spray washing technique as a purification process in the production of biodiesel. E3S
Web of Conferences, 187. 03006. https://www.webofscience.com/wos/woscc/full-record/WOS:000624452800011

Liu, J. C., Chen, Y. M., & Ju, Y. H. (1999). Separation of algal cells from water by column flotation. Separation Science and
Technology, 34(11), 2259-2272.

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Renewable and Sustainable Energy Reviews, 10(3), 248-268. https://doi.org/10.1016/j.rser.2004.09.002

Paladino, O., Neviani, M. Sustainable Biodiesel Production by Transesterification of Waste Cooking Oil and
Recycling of Wastewater Rich in Glycerol as a Feed to Microalgae. Sustainability2022,14,273.
https:// doi.org/10.3390/su14010273
Pitt, D., Domingos, A., & Barros, A. (2019). Purification of residual glycerol recovered from biodiesel production. South African
Journal of Chemical Engineering, 29, 42–51. https://doi.org/10.1016/j.sajce.2019.06.001

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new trends in combustion. Renewable and Sustainable Energy Reviews, 27, 475–493.
https://doi.org/10.1016/j.rser.2013.06.017

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world congress on engineering and computer science (pp. 24-26). WCECS San Francisco, USA.
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1673-1677. https://doi.org/10.1016/j.fuel.2007.08.018

Viktor Polishсhuk, Svetlana Tarasenko, Ievgen Antypov, Nataliya Kozak, Andrii Zhyltsov, Andrii Bereziuk (2020). Investigation
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13
5 Appendices
Appendix A
Table 5.1: MCDA for Raw CSG Water Treatment Method
Rating (1-5) Score
Criteria Rank Weight
RO MF RO MF
Footprint 6 8 3 3 24 24
Capital cost 4 12 1 4 12 48
Ease of Use 9 2 4 4 8 8
Fouling 8 3 4 2 12 6
Operating costs 7 5 2 4 10 20
Environmental impact 3 16 2 4 32 64
Safety 2 20 3 3 60 60
Effectiveness 1 22 5 4 110 88
Flux 4 12 2 4 24 48
Total 100 292 366

Appendix B
Table 5.2: SWOT Analysis for Algae Harvesting Technologies
Unit Strengths Weaknesses Opportunities Threats
Cross flow  Low capital cost  High  Can alter pore  Process must be
 High harvesting maintenance cost size to suit stopped regularly
filtration biomass size for maintenance
efficiency  High operating
 Highly energy cost  Can combine  Algae cells may
efficient  Frequent change multiple units to be damaged
 Does not require of membrane remove different through abrasion
chemical addition filter sizes of biomass of membrane
Flotation  Highly energy  High operating  Can be used for  Added coagulant
efficient cost various could
 Highly scalable  High capital cost microalgae contaminate the
 Rapid operation  Microalgae must species biomass
 Small footprint be destabilised  Works effectively  Toxicity of the
at high overflow coagulant can
rates impact end
 Increased product and
efficiency when environment
coagulant is
added
Centrifugation  High harvesting  Time consuming  Used in  Algae cells may
efficiency process laboratory for be damaged by
 Does not require  Energy intensive testing high gravitational
chemical addition  High operating force
 High harvesting cost
efficiency  High capital cost

14
Appendix C
Table 5.3: SWOT Analysis for Bio-oil Production Method
Unit Strengths Weaknesses Opportunities Threats
Hydrothermal  High energy  Require high  biochar to act as  Energy balance
efficiency operating pressures pollutant adsorber unfavourable if
Liquefaction  High energy and  Less knowledge  aqueous stream to water content of
carbon products and experience on server as nutrient biomass >90%
 Suitable for wet efficient process stream for algae  Variation of
biomass water treatment cultivation  Feedstock
 Higher bio-oil composition
yield  and quality

Pyrolysis  High energy  Required energy  Produces more  Must overcome

efficiency intense drying solid biochar technical and
 High energy and process  Low cost and economic barriers
carbon content  High operating neutral CO2 to compete with
product cost balance  traditional fossil
 Low operating  Long residence fuel-based
pressure times techniques
requirement

Appendix D
Table 5.4: SWOT Analysis for MeOH & NaOH Mixer
Unit Strengths Weaknesses Opportunities Threats
Inline Mixing  Low cost  Do not work well  Economical in low  Some mixers are
 Small footprint for high viscosity viscosity fluid difficult to
 Easy in operating or laminar flow mixing, where manufacture in
and setup (Sinnott, 2005) methanol and laboratory sizes
 Additional Sodium hydroxide down to 1/8
centrifugal pump are low viscosity viscosity (Couper
is required & Fair, 2009)
 The flow rate ratio
and viscosity ratio
should be fixed
before setup, it
determined the
length of the
mixer viscosity
(Couper & Fair,
2009)

15
Appendix E
Table 5.5: SWOT Analysis for MeOH & NaOH Heater
Unit Strengths Weaknesses Opportunities Threats
Shell and Tube  Large surface area  Not particularly  Can be oriented  Needs to be
contained in a small space efficient if vertically to save cleaned regularly
Heat volume allows for large volumes are space and tubes perhaps
Exchanger fast, efficient heat required   Made with replaced due to
transfer  Plate HX's are floating corrosion
 Well established slightly more head floating head  Inefficient heat
technology, abundant efficient with heat to ease cleaning transfer
rules of thumb and transfer  Service fluid  Need to be
engineers with  Cannot be allocated to remade if total
working knowledge expanded to suit tube side for capacity of the
of these HX changing needs corrosion and plant is increased
 Easily constructed, like a plate HX fouling reasons
suitable for pressure can  Can use Coal
if required,   Seam
 Cleaning is easy  Gas, Biodiesel, or
potentially dried
biomass to create
energy to heat
process fluid

Appendix F
Table 5.6: SWOT Analysis for Transesterification Unit
Unit Strengths Weaknesses Opportunities Threats
Batch  Low capital cost  Labor-intensive leads to  Well suited for  Can not be applied
 Easy to understand high operational cost small scale plant to large scale
Reactor and design  Long empty-clean-reset  Widely used in plants
 More flexible than time between batches industry  Difficult to
CSTR in some  The outlet composition (Veljković, 2012) increase the scale
respects: it can can vary from batch to (production) of the
accommodate batch, causing issues to plant without
variations in downstream separation adding more batch
feedstock type, units. reactors
composition &
quantity (Sinnott &
Towler, 2009)
CSTR  High productivity  MeOH is poorly soluble  Suitable for large  Low conversion
 Easy to operate and in bio-oil, only 6~8% at scale plant and slow reaction
control 60 ℃ (Boffito et al.,  More adaptable to rate could require
 Lower operational 2014) design many CSTRs in
costs than batch  Mechanical stirring improvements series
reactor (Sinnott & cannot form fine MeOH- compared to batch
Towler, 2009) oil emulsion, limiting the reactor
mass transfer rate, thus,
reducing the reaction rate
(Boffito et al., 2014)
 High energy consumption
for intense stirring (2 kW/
3
m ¿(Sinnott & Towler,
2009)
Continuous  High productivity  Design could be more  Suitable for large  Continuous
 Induce cavitation complex than CSTR, scale plant Ultrasonic Reactor
Ultrasonic which increases especially for large scale  Amount of catalyst is a relatively new

16
 Reactor local temperature process where many required is less method 
(Jelena et al., ultrasound probes would than CSTR (Jelena  Not yet widely
2010).  be needed. et al., 2010). used in industry
 Increase mass  Only require 1/3 to
transfer by 1/2 energy that is
emulsifying consumed by
immiscible liquid mechanical
(MeOH & agitation (Jelena et
triglycerides) al., 2010).
(Boffito et al.,  The temperature of
2014).  feed streams can
 Can achieve high be lower than
yield in much CSTR which saves
shorter reaction energy (Zou&
time (Boffito et al., Chai, 2017)
2014).

Appendix G
Table 5.7: SWOT Analysis for Biodiesel & Glycerol Separation
Unit Strengths Weaknesses Opportunities Threats
Gravity Settling  Simple to use  Separation is not  Use of multiple  Must be run
 No moving parts- perfect- batchwise- will
tanks would make
Tank reduced subsequent need intermediate
maintenance, refining of both maintenance easier storage tank so
improved products is downstream
reliability required processes can be
 No energy costs  Separation is very run continuously,
slow may need multiple
 Multiple gravity gravity tanks
 Not effective if
settling tanks and
bio-diesel droplets
storage tanks will
are very small
lead to a larger
(Saleh et al., 2010)
footprint.
Centrifuge  Faster separation  High initial capital  Can be run  If centrifuge
 Better separation costs (Saleh et al.,
continuously breaks/requires
2010)
(Towler & Sinnot,
 High maintenance maintenance, there
2013)- higher requirements is no back-up.
(Saleh et al., 2010)
recovery of bio-
 Separation is not Installing a backup
diesel perfect- would increase
subsequent
refining of both capital costs
products is
required
 Higher energy
costs

17
Appendix H
Table 5.8: SWOT Analysis for MeOH & Biodiesel Separation
Unit Strengths Weaknesses Opportunities Threats
Distillation  High recovery  High energy  Efficiency for  If the feed includes
with a high purity consumption large capacity the water, distillation
Column  Reboiler sensitive with plant efficiency will
the methanol oil ratio, decrease, because
low ration reduce the water has similar
heat duty dramatically. volatilities with
(Firuz Alam Philip, methanol (Sinnott,
2014) 2005)
Flash  Relative low  Decrease the purity of  Fast process  Sometimes single
energy recycled methanol at speed stage flash cannot
Evaporator consumption high recovery (Firuz achieve the required
 Easy in operation Alam Philip, 2014) recovery, a double
 Low equipment flash unit is
cost (Firuz Alam necessary. (Firuz
Philip, 2014) Alam Philip, 2014)

Appendix I
Table 5.9: SWOT Analysis for Biodiesel Washing Unit
Unit Strengths Weaknesses Opportunities Threats
Spray Washing  Requires the least  More complex  Less likely to  Can mask
water consumption, equipment form undesirable problems with
the water to bio-oil (Polishсhuk et al., emulsion of soap product quality
ratio is 0.8:1 2020). (Polishсhuk et (Polishсhuk et
(Limmun&  Large wash tanks are al., 2020). al., 2020).
Sansiribhan, 2020). required (Limmun&  Since less water
 Slightly more Sansiribhan, 2020). is used, less
efficient than other wastewater
wet washing would be
techniques. generated.
Bubble Washing  Uses less water  Very inefficient,  The cheap  The bubble can
than wash by especially for large equipment can mix the water
stirring (Srivastava scale plant save some capital with biodiesel
et al., 2008).  Requires processing cost vigorously,
 The equipment is time up to 24 hours leading to
relatively cheap and multistage undesirable
 The process does washing (Srivastava et emulsion
not require constant al., 2008). (Polishсhuk et
observation, which al., 2020).
saves operational
cost (Polishсhuk et
al., 2020).
Wash by Stirring  Like other wet  Time-consuming.  Less likely to  Generates most
washing method, it  Uses most water form undesirable wastewater,
can efficiently among the three wet emulsion of soap increasing the
remove alkali washing methods than bubble difficulty for
catalyst. (Rahayu& washing. wastewater
Mindaryani, 2007). treatment.
 The process cannot be  Risk of causing
automated environmental
 The process needs to issues.
be repeated many
times (Polishсhuk et
al., 2020).

18
Appendix J
Table 5.10- Glycerol Purification MCDA Pairwise Comparison and Criterial Ranks
Enviro
Maint Opera nment Time
Footpr Capita Ease enance ting al Effecti efficie
- int l cost of Use costs costs impact Safety veness ncy Score Rank Comments/Justification
Footprint is a criteria that should be carefully
Footprint - 0.5 0.5 0.5 0.5 1 0 0 0.5 3.5 6 considered as the design brief specifies the
constraint of 55 hectares.
Capital cost is an important criteria as the plant
must be economically viable enough to receive
Capital funding. Construction of the plant cannot go
0.5 - 1 1 0.5 0 0.5 0 0.5 4 4
cost forward without sufficient initial capital to
cover purchase of equipment. There is however
no budget constraint in the brief.
Ease of use should be considered as equipment
requiring heavy monitoring can significantly
Ease of
0.5 0 - 1 0.5 - 0 0 0 2 8 increase labour costs however it is not as
Use
important as other criteria because revenue
from the plant can be used to help cover costs
Maintenance cost should be considered as a
Maintena criteria however with little impact as revenue
0.5 0 0 - 0.5 0 0 0 0 1 9
nce costs from the sale of bio-diesel can be used to cover
the cost.
Operating cost should be considered as a
Operatin criteria however with little impact as revenue
0.5 0.5 0.5 0.5 - 0 0 0 0.5 2.5 7
g costs from the sale of bio-diesel can be used to cover
the cost.
Environm 0 1 1 1 1 - 0 0 0.5 4.5 3 Environmental impact is an important critera.
ental The brief states that there is already tension
impact between resource companies and other
landowners due to the environmental impact of
CSG mining. The addition of an
environmentally damaging process would
greatly increase this tension. The NSW
government has also placed a ban on CSG
leases until suitable regulations can be put in
place. These regulations will likely target the
environmental impact of the process. If the bio-

19
 diesel production process developed is not
environmentally- friendly, there will be
increased government scrutiny, and the pilot
plant may be made redundant by the new
regulations.
Safety is one of the most important
Safety 1 0.5 1 1 1 1 - 0 1 6.5 2 considerations. Engineers have a moral
responsibility to design safe processes.
Effectiveness is a very important criteria. The
Effectiven project brief stipulates bio-diesel production of
1 1 1 1 1 1 1 - 1 8 1
ess 1 500 000 litres/year. If the equipment is not
effective this will not be achieved.
Time efficiency is an important criteria due to
the large volume of material to be processed. If
Time processes take too long, larger pieces of
0.5 0.5 1 1 0.5 0.5 0 0 - 4 4
efficiency equipment and a larger footprint will be
required. This will also lead to higher capital
cost and maintenance costs.

Table 5.11- Glycerol Purification MCDA

Rating (1-5) (5 is best) Score
Criteria Criteria Rank Weight
Vacuum Vacuum
Membrane Process Membrane Process
Distillation Process Distillation Process
Footprint 6 10 3 1 30 3
Capital cost 4 10 2 3 20 6
Ease of Use 8 7 3 3 21 9
Maintenance costs 9 7 3 3 21 9
Operating costs 7 7 2 4 14 8
Environmental
impact 3 12 3 4 36 12
Safety 2 17 3 5 51 15
Effectiveness 1 20 5 1 100 5
Time efficiency 4 10 4 2 40 8
Total Score 333 75

20
Table 5.12- Distillation Process MCDA Justification
Criteria Rating Justification
While there are large footprint requirements for this process, it will be run continuously so will not require any
Footprint 3 buffer storage tanks. There is also no need to store process fluid for a long period of time which would greatly
increase the footprint.
Vacuum distillation columns have high capital costs (Sinnott & Towler, 2019). The other equipment required are
Capital cost 2
simple vessels, and filters
The distillation column must be monitored, however all processes in this option are widely used in industry, and
Ease of Use 3
operators are likely to have experience with them
Maintenance costs 3 Maintenance of the distillation column and filter will be the main contributors to maintenance costs
Operating costs 2 This process has high energy costs due to distillation column(Contreras-Andrade et al., 2015)
Environmental This process does not involve the release of any harmful material to the environment however high energy usage
3
impact will increase carbon emissions (Contreras-Andrade et al., 2015)
Main safety concerns are the use of acid in the pre-treatment stage and operation of the vacuum distillation column.
Safety 3
These are not particularly hazardous.
Effectiveness 5 The process can achieve >99% glycerol purity (Contreras-Andrade et al., 2015)
This process can be run continuously and does not require a gravity settling stage unlike the membrane process
Time efficiency 4
(Chol et al., 2018)

Table 5.13- Membrane Process MCDA Justification

Criteria Rating Justification
This process requires multiple gravity settling tanks and storage tanks due to the batch nature of gravity settling.
Footprint 1
This increases the footprint required
Ultrafiltration membranes have high capital costs (Sinnott & Towler, 2019). However these are not as high as a
Capital cost 3
distillation column.
Each stage in this process is easy to run, however the use of membranes in this particular separation is not
Ease of Use 3
common. There may be unexpected challenges (Chol et al., 2018).
Maintenance costs 3 Relatively high maintenace costs due to fouling of the membrane, and membrane replacement costs
Very low operating costs. The main operating costs are associated with pumping the process fluid between
Operating costs 4
vessels and pressurising the fluid in the membrane.
Environmental This process does not involve the release of any harmful marterial to the environment. Low energy useage also
4
impact reduces carbon emissions.
The main safety concerns are the use of acid in the pretreatment stage and the pressure required to operate the
Safety 5
membrane. This pressure is not very high, hence the safety concerns for this process are minimal
This process can achieve 93-94% glycerol purity (Chol et al., 2018). This does not meet the project brief or the
Effectiveness 1
chosen objective

21
Time efficiency 2 The gravity settling stage reduces time efficiency for this process

22
Appendix K
Sample calculations of reactor volume
The volumetric flowrate of biodiesel in Litre/hour can be calculated, assuming the plant works nonstop
24/7 all year round:

1,500,000 L/ yr
v(biodiesel)= =171.2 L/hr
365 × 24

According to biodiesel standards EN14214, the density of biodiesel should be from 860-900 kg/m^3. For
the simplicity of calculation, the average value was taken. According to Bay et al. (2006), the average
molecular weight of biodiesel is 294.86 g/mol. Therefore, the molar flowrate of biodiesel can be calculated:

171.2 L/hr ×0.880 kg / L

F ( Biodiesel )= =511mol /hr
0.29486 kg /mol

Therefore, the molar flowrate of glycerol would be 170 mol/hr from stoichiometry. It was assumed that the
volume of the materials does not change during the reaction and the bio-oil to methanol molar ratio is 1:6.
The biodiesel yield is determined to be no less than 97% which is approximated as 100% in the calculation.
Therefore, the molar ratio of outlet stream of the reactor should be:

Methanol :Glycerol : Biodiesel=3 :1 : 3

Therefore, the volumetric flowrate of glycerol and methanol in the outlet stream can be calculated, all the
density and molar mass value of methanol and glycerol should come from Perry’s Chemical Engineering
Handbook:

511mol / hr × 0.032 kg/mol

v ( Methanol )= =20.6 L/hr
0.792 kg /L

170 mol/hr ×0.0921 kg /mol

v ( Glycerol )= =12.4 L/hr
1.260 kg / L

Since the residence time of reactants in the continuous reactor is determined as 55min (Zou & Chai, 2017),
the volume of the reactor can be calculated as the product of residence time and total volumetric flowrate:

55
Volume of reactor = hr × ( 171.2+20.6+12.4 ) L/hr =187.2 L
60

Appendix … Crude Glycerol Purification Calculations

Neutralisation CSTR

23
 Residence timeis the main sizing parameter for vessels .

volume
Residence time= (Towler∧Sinnot , 2013)
volumetric flow

For neutralisation tank , desired mean residencetime is30 minutes ( Pitt et al , 2019 )

3
Assuming the vessel mainly contains 70 % glycerol 15 % water∧15 % methanol , density is calculated at 1125 kg /m

V
0.5 h=
kg kg
75.3 ÷1125 3
h m
3
V =0.143 m

'
For CST R s ,optimum proportions are liquid level equal ¿ the tank diameter (Walas ,1990) .

Assuming tank is 85 % full during operation ,

Diameter=0.14 m

Height=0.16 m

Footprint =0.0224 m 3

Activated Carbon Absorption Vessel

Residence timeis the main sizing parameter for vessels .

volume
Residence time= (Towler∧Sinnot , 2013)
volumetric flow

for activated carbon tank , desired meanresidence time is 3 hours ( ( Manosak et al . ,2011 ) )

3
Assuming the vessel contains mainly glycerol , density is assumed ¿ be 1261 kg /m

V
3 h=
kg kg
55.72 ÷ 1261 3
h m
3
V =0.133 m

For vessel , optimum length/diameter=3(Walas ,1990)

24
 Assuming length/diameter=3 ,

Diameter=0.06 m

Length=0.18 m

Vessel is horizontal , so footprint=L × π × d

3
Footprint =0.034 m

Centrifuge

Residence time for a liquid−liquid centrifuge is generally10−30 seconds(Towler∧Sinnot , 2013) .

volume
Residence time= (Towler∧Sinnot , 2013)
volumetric flow
Assuming t h e vessel contains 33 %  glycerol∧67 %  biodiesel , density =996.93
Assuming t h e centrifugeis cylindrical , meanresidence timeis 15 seconds ,
15 volume
=
60× 60 230.7 ÷ 996.93
3
V =0.01m
Assuming a centrifuge h as similar dimensions ¿ a reaction vessel , h eig ht=diameter(Walas , 1990)
Heig h t=0.20 m
Diameter=0.20 m

25