PROJECT 5046-1910: REUSE OF SPENT COFFEE GROUNDS TO

PRODUCE BIODIESEL AND GLYCERIN DESIGN REPORT

Russell McClure, Dat Nguyen, Christine Santabarbara, Noah Skinner, Christopher Stone

Chemical Engineering Program

University of Cincinnati

15 March 2019
 1

Contents
Abstract............................................................................................................................................ 3
1. Scope Definition....................................................................................................................... 3
2. Design Basis ......................................................................................................................... 4
2.1 Plant Capacity ................................................................................................................... 4
2.2 Feed Specifications ........................................................................................................... 5
2.3 Product Specifications ...................................................................................................... 5
2.4 Process Specifications....................................................................................................... 6
3. Process Description .............................................................................................................. 8
3.1 Process Synthesis .............................................................................................................. 8
3.1.1 Full Scale Process ........................................................................................................ 8
3.1.2 Pilot Plant .................................................................................................................... 8
3.2 Recommended Process ................................................................................................... 10
3.3 Process Control ............................................................................................................... 12
3.4 Technology Risk ............................................................................................................. 13
3.5 Environmental Performance ........................................................................................... 13
3.6 Process Safety ................................................................................................................. 13
3.7. Regulations and Standards .............................................................................................. 14
3.8 Preliminary Equipment Specifications ........................................................................... 15
4. Process Economics ................................................................................................................ 17
4.1 Estimated Capital and Operating Costs .......................................................................... 17
4.2 Economic Analysis ......................................................................................................... 19
5. Recommendations and Future Work ..................................................................................... 19
5.1 Recommendation ................................................................................................................. 19
5.2 Future Work......................................................................................................................... 20
References ..................................................................................................................................... 21
Appendices .................................................................................................................................... 24
A. Hyperlinks to Safety Data Sheets ................................................................................... 25
B. Summary of Physical Properties ..................................................................................... 26
C. Material and Energy Balance for Process and Utility Streams ....................................... 27
D. Example Process Calculations ........................................................................................ 28
E. Emission Calculations..................................................................................................... 29
F. Example Economic Calculations .................................................................................... 30
G. Specification Sheets ........................................................................................................ 31
 2

H. Product Properties................................................................................................................. 32

Abstract
The main goals of this project are to produce useful products, such as biodiesel and
glycerin, using the direct transesterification of spent coffee grounds (SCGs) process developed by
Mingming Lu, Yang Liu, Qingshi Tu, and Gerhard Knothe. This project includes designing a full-
scale process for turning SCGs into FAME biodiesel and glycerin and performing economic
evaluation of the process assuming the plant is built as an attachment to a pre-packaged coffee
processing plant. The plant as currently designed has a net present value of negative $40 million.
Further optimizations to the plant need to be made in order for it to become profitable.

1. Scope Definition
The purpose of the project is to reduce food waste and generate value for local communities
by designing a pilot scale and full-scale process that produces fatty alcohol methyl ester (FAME)
biodiesel and glycerol by direct transesterification of SCGs [1].
The pilot scale process is envisioned to live on the back of a truck. The pilot scale will
match the local process design but will be scaled down to fit appropriately. The full-scale process
will be developed as an expansion of the Starbuck’s Augusta Soluble Coffee plant which produces
all Starbucks ready-to-drink (RTD) beverages and instant coffee for distribution across the US [2].
By doing that, the volume of SCGs collected will be high enough while the transportation cost for
this process can be minimized.
To determine the amount of SCGs produced at this site each year, a comparison was
completed between the size of the RTD and instant coffee market and Starbuck’s share of sales in
this space. To begin, RTD and instant coffee accounts for 13% of coffee preparation among US
consumers [3]. This subset of coffee preparation accounts for 28.6% of coffee sales in the US [4].
Based on data from Starbuck’s financial statements, the portion of their sales in this category give
Starbuck’s a 51.7% share of the RTD and instant coffee market [5]. After completing this analysis,
it was determined that 100,000 metric tons could be collected and processed at our facility. This
accounts for 6.7% of the SGCs produced in the US annually.
The feed and product rates of the full-scale and pilot scale process can be seen in the tables
below.

Table 1. Feed rates of raw materials

Feed Materials Hourly Feed Rate, kg/h Annual Feed Rate, MT/year
H2SO4 1,000 8,000
MeOH 350 2,800
CaO 540 4,300
Wet SCG (60% water) 12,500 100,000
 4

Table 2. Production rates

Products Hourly Production Rate, kg/h Annual Production Rate, MT/year
FAME biodiesel 860 6,900
Glycerol 90 720
Gypsum 1,300 10,000

Table 3. Feed and production rates per batch for pilot scale process
Feed Materials Batch Feed Rate, kg/h
H2SO4 8
MeOH 160
CaO 6
Wet SCG (60% water) 100
Products
FAME biodiesel 13
Glycerol 2

2. Design Basis
2.1 Plant Capacity
The plant will be designed to handle 12,500kg/h of wet SCGs (60% water). These coffee
grounds will be combined with 1,000kg/h of sulfuric acid which is used as a catalyst. All added
sulfuric acid is neutralized with 535kg/h of calcium oxide. An additional 350kg/h of fresh
methanol is added to the process to complete the transesterification of the fats within the coffee
grounds. The process will produce a total of 860kg/h of FAME biodiesel, 90kg/h of glycerol, and
1,250kg/h of gypsum. The plant is designed to operate continuously for 8,000 working hours each
year.
 5

2.2 Feed Specifications

The spent coffee grounds are expected to contain on average 60% by weight of water.
Coffee grounds were assumed to have no cost since the current recommendation is to add this
process to an existing coffee production facility. The acid content of the spent coffee grounds is
expected to be above 2 mg KOH/g oil which will be qualified by titration. The methanol is 99.9%
pure and will be confirmed using gas chromatography to ensure that there is less than 0.1% water
in the feed. The presence of water during transesterification can significantly reduce the reaction
rate [6]. 98% pure sulfuric acid will be purchased and validated based on the material density. 98%
pure CaO will be purchased to neutralize the sulfuric acid; the purity will be confirmed by titration.
Costs of all materials can be found in Table 4 below.

Table 4. Raw Material Purchase Values

Raw Material Purchase Cost (/metric ton)
Spent Coffee Grounds $0
99.9% Pure Methanol $392.01 [7]
98% Pure Sulfuric Acid $107.26 [8]
98% Pure Calcium Oxide $118.40 [8]

2.3 Product Specifications

The FAME biodiesel product is required to meet ASTM D7467, for which detailed
specifications can be seen in Appendix H [9]. Processing considerations are included to ensure
that the FAME meets the specifications for acid value, glycerin content, water content, and fat
content. Process measures are included to ensure the FAME product meet all of these
specifications including neutralization of the product with calcium oxide, washing the product with
water to remove glycerin, a flash operation to remove water and multiple reactors to convert all
the fat to biodiesel. Gas chromatography will be used to verify the purity of the FAME.
The glycerin product must be 99.70% pure, and detailed specifications can be seen in
Appendix H [10]. It is important to remove all methanol and water from the product; this is done
by distillation. Product purity for the glycerin will be confirmed by high performance liquid
chromatography. The purity of gypsum will be determined by both measuring the moisture content
of the product and through inductively coupled plasma mass spectrometry to ensure the correct
calcium and sulfur content. Sale values for all products are listed in the Table 5 below.

Table 5. Product Sale Values

Product Sale Value (/metric ton)
FAME Biodiesel $875.00 [11]
Glycerin $248.23 [11]
Gypsum (dihydrate) $8.00 [12]

There are three main by-products that will be produced by this process. The first is a stream
of steam coming from the coffee ground dryer. This stream will be predominately water vapor
with about 0.40%wt H2SO4. The flow leaving this vessel will pass through a scrubber to reduce
the sulfur released into the atmosphere. The second by-product are defatted spent coffee grounds.
This solid waste stream is non-hazardous and can either be landfilled or sent through a pyrolysis
 6

unit to create a soil additive. Finally, a water by product containing minor levels of glycerin and
methanol will be sent to waste water treatment.
2.4 Process Specifications
The current plant is planned to be an addition to an existing ready-to-drink or instant coffee
production facility. An example of such a facility is the Starbuck’s Augusta Roasting Facility; this
facility makes ready-to-drink beverages for Starbuck’s in North America [2]. When designing the
add on to such a facility, it will be important to keep biodiesel production separate from the food
grade production. The only crossover between beverage production and biodiesel production
should be spent coffee grounds and utilities. Following GMP standards for the production of
biodiesel will unnecessarily increase the project costs. In addition to being separate from beverage
production, the process will have an artificial boundary separating SCG preparation, extraction,
and transesterification from the product separation and purification.
The current process will require the following utilities: electricity, process water, natural
gas, 90psig steam, and tower water. A summary of the usage of each of these utilities can be found
in Table 6 below. Electricity will be used in 18 pumps throughout the process to move fluid through
different unit operations. 90psig steam will be used to heat the two transesterification reactors and
in three heat exchangers within the process. Process water is used at various point to dilute sulfuric
acid, wash spent coffee grounds, and wash the biodiesel product. Natural gas is used to generate
heat to dry the water from the acidified spent coffee grounds before the extraction begins. Tower
water is used for cooling in 9 different heat exchangers with an assumed inlet temperature of 90°F
and an outlet temperature of 120°F.

Table 6. Total Utility Usage

Utility Usage Units
Electricity 4.10 kW
90 psig Steam 70.2 MMBTU/h
Process water 13.5 gpm
Natural gas 36300 SCFH
Tower Water 4880 gpm

There are three main waste streams from this process. The first stream is steam with minor
amounts of H2SO4. This stream will be passed through a scrubber before release to the atmosphere.
The second stream contains the solid, defatted spent coffee grounds. This solid waste will either
be sent to a landfill as non-hazardous or sold to a different process to create a biochar soil additive.
The final waste stream is aqueous waste water. This stream will be sent to waste water treatment
with a COD of 630 and a BOD of 380. Table 7 below lists all waste streams and their amounts for
this process.

Table 7. Summary of Waste Streams and their Flows

Waste Identity Flow Rate Destination
Water Vapor 20,000lb/h Scrubber then Atmosphere
Defatted SCG 11,500lb/h Landfill
Waste Water 29ft3/h Waste Water Treatment
 7

This process includes 4 process area tanks to hold fresh methanol, fresh sulfuric acid,
FAME biodiesel product, and glycerin product. Additionally, there will also be 3 holding area for
wet spent coffee grounds, fresh calcium oxide and defatted spent coffee grounds. All tanks and
holding areas are designed to store 12h of feed or product from the production. Table 8 below lists
the various tanks and holding areas and their sizes.

Table 8. Summary of Holding Vessel Sizes

Tank Description Size
T-100 Fresh Sulfuric Acid Tank 1500gal
T-105 Wet Spent Coffee Grounds Hopper 4400ft3
T-200 Fresh Methanol Tank 1200gal
T-230 Fresh Calcium Oxide Holding Area 75ft3
T-270 Glycerol Product Storage Tank 200gal
T-290 FAME Biodiesel Storage Tank 2600gal
T-398 Defatted Spent Coffee Grounds 4400ft3
 8

3. Process Description
3.1 Process Synthesis
3.1.1 Full Scale Process
In developing this process, a few alternatives were considered. The first alternative used a
batch-based process to produce the biodiesel process. A batch process was chosen based on the
lower flow rate of the product and the need to change coffee grounds every 12 hours. The process
was developed using batch distillation and reaction and a single batch reactor for both the
extraction and transesterification. This process was abandoned after reviewing the function of the
Soxhlet apparatus used to develop this process. The Soxhlet apparatus has a cross flow of methanol
that is refluxed from the bottom pot of the reaction. The bottom pot contains extracted fats, the
biodiesel product, and methanol. The Soxhlet apparatus is similar to three separate unit operations,
a solids extractor, a mixed flow reactor, and a flash operation to recycle fresh methanol.
A better understanding of the Soxhlet apparatus led to our second design alternative. This
design included three separate processes to extract, react, and separate methanol from the spent
coffee grounds. The second alternative also included a more refined separation process to create
pure glycerin and biodiesel products. The separation process included a full distillation column to
separate methanol from the acidic biodiesel product, a neutralization of the biodiesel product, and
a liquid/liquid extractor using water to separate aqueous components from the biodiesel. The
aqueous phase from the extractor was then sent to a vacuum distillation to purify glycerin and a
second atmospheric distillation to purify waste water with the remaining methanol being recycled.
The biodiesel phase from the extraction went through a flash operation to remove water from the
product. Finally, the biodiesel was further distilled to remove the remaining fat in the product. The
process described above had a few key issues. First the distillation to remove the remaining fat in
the biodiesel process had a very high bottoms temperature requiring a hot oil system for the
reboiler; this dramatically increased operating and capital investment. Additionally, the heating
requirement for two of the columns was roughly three time the amount of energy produced in the
biodiesel. This makes this process undesirable from an energy standpoint. In order to solve these
issues a third design was developed.
Key changes in the third design were the addition of a second MFR to the process to further
react the fat in the biodiesel. The additional reactor removed enough fat in the biodiesel to allow
the removal of the final distillation for the biodiesel and required hot oil system. A second change
was made replacing the first distillation column to purify methanol with a flash drum. This cut the
heat duty for the unit operation in half and was still able to recover the majority of the methanol.
Finally, in order to reduce the amount of methanol that was lost with the defatted coffee grounds,
a water wash of the defatted coffee grounds was added to recover the methanol.

3.1.2 Pilot Plant

The pilot plant was designed to process 0.1MT of SCGs per batch. Rather than be a
continuous process like the full-scale plant, the pilot plant was designed to be partially batch
operation to allow for a variety of studies to be performed without the rigorous start-up and shut-
down required for continuous processing. The initial processing steps up to and including the
reaction are all designed to be batch processing, while the separation and purification of the
products was designed to be continuous to match the full-scale plant.
 9

The process starts in the 50-gallon stainless steel sulfuric acid impregnation vessel V-400.
50% sulfuric acid, water, and the wet SCGs are loaded to the vessel and heated to 70˚C, then the
slurry is mixed for about 3 hours. The slurry is then sent to the acidified SCG Dryer V-405, a 50-
gallon stainless steel jacketed tank, and heated to 105˚C for around 24 hours to remove all water
from the slurry [1]. The sulfuric acid and SCG slurry is then sent to the SCG Lipid Extractor, V-
500, a 100-gallon stainless steel Rotocel extractor. Here fresh methanol is used to extract the lipids
from the SCGs. Following this step, the defatted SCG slurry is sent to the solids rotary drum
separator V-505, where the defatted SCGs are separated out from the liquids. The liquids,
containing the lipids, sulfuric acid, and methanol, are sent to the transesterification CSTR, a
jacketed 100-gallon stainless steel tank. Here the solution is reacted at 70˚C until 99.9% conversion
is achieved, which is expected to take around 12 hours [1].

Figure 1. Pilot-scale design: Separation and purification

After the reactor, the remaining part of the process is continuous to better match the full-
scale process. The first vessel after the reactor is the 100-gallon stainless steel methanol removal
strip tank V-600, where the solution will be heated to about 190˚F to allow the methanol to
vaporize. Next the sulfuric acid will be removed in V-605, a 10-gallon stainless steel tank. Calcium
oxide will be added to V-605 where it will react with the sulfuric acid and form a precipitate. Next
the solution is sent to CL-610, a liquid-liquid extractor where water is added to separate the
glycerol, and small amounts of methanol that remain from the biodiesel. From the top of the liquid-
liquid extractor, biodiesel and a small amount of water is sent to V-615, a small strip tank to remove
any remaining water to reach the required purity to meet biodiesel specifications (see Appendix
H). From the bottom of the liquid-liquid extractor, glycerol and water enter column CL-625 where
the water comes out the distillate and the purified glycerol the bottoms of the column.
 10

Figure 2. Pilot-scale design: Separation and purification

3.2 Recommended Process

A block flow diagram for the process is seen below in Figure 3. The process has 8 general
blocks which starts with preparing the spent coffee grounds (SCG), reacting and extracting the fat
from the SCG and finally, a variety of separation units to ensure that all products and waste streams
meet specifications.

Figure 3. Block Flow Diagram of the recommended biodiesel production process

An overall material and energy balance for this process can be found in Table 9 below. The
process main inputs are wet spent coffee grounds, methanol, and water. These inputs are reacted
 11

to form glycerol and FAME biodiesel. A small amount of triacylgycerol is also produced which
represents unreacted fat in the biodiesel. Additionally, sulfuric acid is added to the process as a
catalyst and then later neutralized with calcium oxide to make calcium sulfate. Solid waste also
leaves the process in the form of defatted SCG. Specifications for the waste coming from this
process and emissions to the environment can be found in Section 2.4.

Table 9. Overall process material balance

Overall Mass Balance (lb/hr)
Input Output
Glycerol 0 197
Methanol 768 583
Calcium Oxide 1131 0
Calcium Sulfate 0 2746
Triacylgycerol 0 1
FAME Biodiesel 0 1901
Sulfuric Acid 2205 226
Water 761931 762300
Wet Spent Coffee Grounds 11133 0
Defatted Spent Coffee Grounds 0 9241

Total 777169 777195

The overall energy balance is found in Table 9 below shows that the majority of the energy
transferred through this process is in the form of the feed streams and product streams. There is
also 75MMBtu/h of heating used by this process supplied through steam. The 69MMBtu/h of
cooling used in the process is completed with tower water. Finally, a small amount of power is
added to the process through the pumps. The mass and energy balance around each individual
stream can be found in appendix C.

Table 9. Overall process energy balance

Overall Energy Balance (MMBtu/h)
Input Output
Feed Streams -5166.55
Product Streams -5160.98
Total Heating 75.113
Total Cooling -69.4516
Power Added 0.0073719

Total -5160.88 -5160.98

A complete process flow diagram showing all unit operations and streams can be seen in
drawings DWG 5046-02775-B and DWG 5046-02776-B. Walking through the various unit
operations, the process starts by pumping fresh sulfuric acid and process water into V-115 with
the wet spent coffee grounds. This unit operation creates a slurry of SCG in acid which is then
pumped to V-120 for drying. The V-120 drying unit is used to remove water from the SCG and
 12

embed the sulfuric acid onto the dried SCG. The dried SCG are moved to V-206 and combined
with methanol to extract the fat from the SCG. The liquid extract from this process is sent to two
MFRs in series (R-210 and R-211) to complete the transesterification reaction. Defatted SCG from
V-206 are sent to U-400 to wash the methanol from the defatted SCG.
The liquid stream leaving R-211 is combined with streams being recycled from various
other unit operations before entering V-215. The V-215 unit is a flash drum operating at 190°F to
remove methanol from the biodiesel stream. The methanol removed from this unit is cooled and
combined with fresh methanol before returning to V-206. The liquid biodiesel product leaving V-
215 is cooled and combined with the water wash from U-400. This combined acidic stream enters
R-245 with solid calcium oxide to neutralize the acid in the biodiesel water stream. The acid is
neutralized to water and solid calcium sulfate precipitate is removed from the liquid stream in V-
250. The solid calcium sulfate will be sold as gypsum.
Neutral biodiesel is pumped to CL-255 after leaving V-250. CL-255 is a liquid/liquid
extractor which washes the biodiesel product with water. This separates the aqueous components
in the mixture including methanol and glycerin from the biodiesel. The wet biodiesel product
leaves the tops of the liquid /liquid extractor and is heated to remove excess water from the
biodiesel product. Water leaves as a vapor from V-260 and a finished liquid biodiesel product is
pumped from the bottom of V-260 to storage in T-290. The water vapor leaving V-260 is recycled
to the entry of V-215 to recover the large amount of biodiesel in this vapor stream.
The aqueous phase leaving CL-255 is pumped to CL-265, a vacuum distillation column to
separate the glycerin product from the methanol and water streams. Glycerin product leaves the
bottom of CL-265 and is pumped to T-270 for storage. The methanol and water vapor leaving the
top of the column are sent to CL-350 for further purification of the water before it is sent to waste.
The water leaving the bottom of CL-350 is split with the majority of the flow recycled to the
defatted SCG wash. The methanol leaving the top of CL-350 is not pure enough to be reused in
the reactor so it is recycled to the V-215 for further purification.
Details on the major control loops can be found in section 3.3. Details on all streams’
composition, flow, and properties can be found in appendix C.

3.3 Process Control

Process control schemes will be implemented to:

• Maintain the flow of fresh methanol into the Rotocel Extractor V-206
• Control the flow of the raw materials (Methanol, Water, SCGs, sulfuric acid) into the
process, and the products (FAME, glycerol, gypsum) out of the process
• Control the flow of cooling water to the condensers on columns CL-265, and CL-350
• Control the flow of cooling water to heat exchanger E-217, E-226, E-300, E-305 and E-
316
• Control the flow of steam to heat exchanger E-214
• Control the distillate composition for columns CL-265, and CL-350 with flow indicators
on the distillate and reflux streams and a ratio controller to control the reflux ratio
• Control the maximum allowable liquid level in the run tanks T-100, T-105, T-200, T-270
and T-290
 13

3.4 Technology Risk

Nearly all technology risk associated with this process is due to the upscaling of the process
from lab volumes. Most of this risk is inherited within the H2SO4 soak reactor, the
transesterification reactor, and the separations process. We do not believe the other components of
the process to pose notable technology risk, as they are relatively straight forward separations
within the wider industry. There are no unusual pieces of equipment or machinery being used for
this process.
There is a lack of detailed data with regards to the H2SO4 soak reactor and the
transesterification reactor. We do not have a full accounting of how the processes interact with the
SCGs and where and how the reaction is specifically occurring. Questions such as, “is the reaction
occurring in the coffee bean, or just outside of it” remain unanswered until more data is collected.
This can lead to unexpected outcomes when scaling to the pilot plant scale.
There were also concerns raised with the viscosity of the transesterification product. If
methanol levels are not appropriate, the viscosity of the product was too high in lab settings.
Currently the plant design assumes relatively clean product and low enough viscosity. This may
lead to having issues with moving the substance through the various separation unit ops and piping.
The viscosity and flow rates of our product should be carefully investigated and appropriately
controlled for during the pilot plant phase of the project.

3.5 Environmental Performance

The environmental impact for this proposed expansion is primarily driven by the use of
natural gas, steam and electricity. Waste water byproduct generated in the process is also
considered in the environmental performance assessment.
This process emits approximately 1.98*1011 MT CO2/yr (detailed calculation in Appendix
E) which will have a huge impact on the environment. To simplify the calculations, steam is
assumed to be generated by burning natural gas. The majority of CO2 released is accounted for a
large amount of steam and natural gas used. Additionally, annually, this process generates around
2320 CCF of waste water which is required to be sent for waste water treatment.
To minimize environmental impact, water and methanol are recycled when possible to
reduce the amount of materials consumed. Distillation columns and heat exchangers are also
optimized to achieve the least amount of utilities consumption. While the manufacture of FAME
biodiesel from SCGs helps reduce food waste, the large amount of utilities consumed seems to
have a more negative influence on the environment.
The emissions by individual are not considered in this case due to limited information.

3.6 Process Safety

In order to protect personnel from injury caused by contact with hot surfaces, any lines
containing streams at a temperature greater than 120°F will be insulated. Pressure relief devices
listed in the following table are shown in the process flow diagram for the process to ensure
pressures do not exceed the safe operating pressure of the equipment.

Table 10. Safety Relief Devices

 14

Pressure Relief Associated Description

Valve Tag Equipment
PSV-100 T-100 Fresh Sulfuric Acid Feed Tank
PSV-105 T-105 Wet SCG Feed Tank
PSV-115 T-115 Sulfuric Acid Impregnation Vessel
PSV-120 V-120 Acidified SCG Dryer
PSV-200 T-200 Fresh Methanol Feed Tank
PSV-206 V-206 SCG Lipid Extraction – Rotocel
PSV-207 V-207 Solids Rotary Drum Seperator
PSV-210 R-210 Transesterification MFR
PSV-211 R-211 2nd Transesterification MFR
PSV-214 E-214 Reacted Materials Cooler
PSV-215 V-215 Methanol Removal Flash Drum
PSV-217 E-217 Methanol Cooler
PSV-218 E-218 Methanol Condenser
PSV-226 E-226 Acidified Biodiesel Cooler
PSV-230 T-230 CaO Feed Tank
PSV-245 R-245 Catalyst Removal
PSV-250 V-250 Neutralized Catalyst Removal
PSV-255 CL-255 Biodiesel Water Wash Column
PSV-260 V-260 Biodiesel Water Removal
PSV-265 CL-265 Glycerol Purification Column
PSV-270 T-270 Glycerol Product Tank
PSV-290 T-290 FAME Product Tank
PSV-300 E-300 FAME Cooler
PSV-305 E-305 Water and FAME Recycle Cooler
PSV-310 E-310 Glycerol Purification Column Condenser
PSV-315 E-315 Glycerol Purification Column Reboiler
PSV-350 CL-350 Methanol Water Separation Column
PSV-355 E-355 Methanol Water Column Condenser
PSV-360 E-360 Methanol Water Column Reboiler

3.7. Regulations and Standards

The regulations and standards followed for the preliminary design are outlined below.

• OSHA PSM
o OSHA PSM is the industry standard when dealing with toxic and/or flammable
materials, which include Bio-Oil, and the Biodiesel product
• CFR 1910 – Occupational Safety and Health Standards
o Details required safety equipment and structures for correct process operations
• EPA RMP
o An RMP (Risk Management Plan) is required for all facilities which deal with
extremely hazardous substances, this plan will be re-submitted every five years
to the EPA
 15

o This plan requires a five-year history of accidental releases of regulated

substances within the process, a prevention program to manage risk, and
emergency response program, and an overall management system to supervise
its implementation
• NFPA/NEC Classifications Class 1, Division 2
o The presence of flammable vapors will require adherence to construction and
operation procedures as outline by this standard
o This process is a Class 1, Division 2 location due to the handling of volatile
flammable liquids or gasses, being Biodiesel, Bio-Oil, Glycerin, Sulfuric Acid
• EPA Title V for Air Emissions
o All manufacturing facilities must adhere to section 5 of the clean air act
o Due to emissions being near or exceeding 100 ton/year, a Title V Permit must
be obtained by the EPA, with fees attached
o Plant is subject to NESHAP Requirements as it is a Chemical Manufacturing
plant
• ASME Safety Code A13
o ASME A13 will be followed and utilized to ensure all P&IDs are correctly
labeled, updated and handled
• ASME PTC 12.5
o To ensure heat exchangers are properly inspected and maintained, ASME PTC
12.5 must be followed
• TEMA Heat Exchanger Standards Class B&C
o TEMA Heat Exchanger Standards Class B&C will assist in the design and
construction of the proposed economizers in this process, to ensure that all
vessels are built to proper specifications and standards.
• ASME Section VIII
o Due to the high pressure of the proposed design, the systems must adhere to
ASME section VIII to ensure proper design, inspection and operation

3.8 Preliminary Equipment Specifications

Table 11. Preliminary equipment specifications
Tag Description Parameter
T-100 Fresh Sulfuric Acid Feed Tank 1448.34 gal
P-101 Fresh Acid Pump 19.3 ft3/hr, 0.987 bar-G
T-105 Wet SCG Feed Tank 32658.54 gal
P-106 SCG Screw Pump 438.3 ft3/hr, 0.987 bar-G
V-115 Sulfuric Acid Impregnation Vessel 13688 lb, D=4.42ft, L=44.2ft
P-116 SCG Acid Slurry Pump 547.9 ft3/hr, 0.987 bar-G
V-120 Acidified SCG Dryer 24.526 MMBtu/h
T-200 Fresh Methanol Feed Tank 1143.54 gal
P-201 Fresh Methanol Pump 15.5 ft3/hr, 0.987 bar-G
V-206 SCG Lipid Extraction Rotocel 1107.8 ft3/hr
V-207 Solids Rotary Drum Separator 837.4 ft3/hr liquid
P-209 Lipid Extracting Pump 899.3 ft3/hr, 0.987 bar-G
 16

R-210 Transesterification MFR 838.6 ft3/hr

Tag Description Parameter
R-211 Transesterification MFR 838.6 ft3/hr
P-212 Transesterification Product Pump 900.96 ft3/hr, 0.9867 bar-G
P-213 Water Recycle Pump from Flash 1.3087 ft3/hr, 0.6895 bar-G
Drum
V-215 Methanol Removal Flash Drum W=1956 lb, D=5.50 ft, L=6.37 ft
P-216 Methanol Recycle Pump 857 ft3/hr, 0.986 bar-G
E-217 Methanol Recycle Cooler -0.58 MMBtu/hr
E-218 Methanol Recycle Cooler -21.2230 MMBtu/hr
E-226 Acidified Biodiesel Cooler -0.1895 MMBtu/hr
T-230 CaO Tank 566.28 gal
P-235 CaO Screw Pump 7.60 ft3/hr, 0.986 bar-G
R-245 Catalyst Removal -20.85 MMBtu/hr, W=9831 lb, D=3.76 ft, L=37.46 ft
V-250 Neutralized Catalyst Removal -0.566 MMBtu/hr, A=11.02 ft2
P-251 Neutral Biodiesel Pump 320.7 ft3/hr, 0.487 bar-G
CL-255 Liquid-Liquid Extractor 303 ft3/hr
P-256 Wet Biodiesel Pump 40.0 ft3/hr, 0.986 bar-G
V-260 Biodiesel Water Removal W=610 lb, D=2 ft, L=7.40 ft
CL-265 Glycerol Purification Column W=15774 lb, D=9 ft, L=20 ft
T-270 Glycerol Product Tank 186.66 gal
P-271 Methanol/Water Recovery Pump 281.5 ft3/hr, 0.987 bar-G
P-277 Glycerol Product Pump 2.53 ft3/hr, 0.986 bar-G
P-287 Liquid Recycle Pump 2.38 ft3/hr, 0.986 bar-G
P-288 FAME Product Pump 49.0 ft3/hr, 0.986 bar-G
T-290 FAME Product Tank 2592 gal
E-300 Methanol Removal Column -44.63 MMBtu/hr
Condenser
E-305 Methanol Removal Column Reboiler 45.28 MMBtu/hr
E-310 Glycerol Purification Column -44.95 MMBtu/hr
Condenser
E-315 Glycerol Purification Column Reboiler 44.40 MMBtu/hr
E-316 Glycerol Product Cooler 0.0133 MMBtu/hr
CL-350 Methanol Water Separation Column W=13735lb, D=3ft, L=68ft
E-355 Methanol Water Column Condenser -5.0697 MMBtu/hr
E-360 Methanol Water Column Reboiler 6.6307MMBtu/hr
P-365 Washing Water Recycle Pump 173.5 ft3/hr, 0.986 bar-G
P-370 Methanol Recovery Pump 90.7 ft3/hr, 0.986 bar-G
P-375 Acidic Methanol Recovery Pump 279.7 ft3/hr, 0.987 bar-G
 17

4. Process Economics
4.1 Estimated Capital and Operating Costs

The purchased equipment included 18 pumps (P-101, P-106, P-116, P-201, P-209, P-212,
P-213 P-216, P-235, P-251, P-256, P-271, P-277, P-287, P-288, P-365, P-370, P-375), 11 heat
exchangers (E-214, E-217, E-218, E-226, E-300, E-305, E-310, E-315, E-316, E-355, E-360), 1
rotary drum dryer (V-120), 2 flash vessels (V-215, V-260), 2 pressure vessels (V-115, V-206), 2
solid separators (F-207, V-250), 6 tanks (T-100, T-105, T-200, T-230, T-270, T-290), 2 distillation
columns (CL-265, CL-350), and 1 liquid-liquid extractor (CL-255). All the capital costs were
summarized in Table 12 below.
 18

Table 12. Summary of capital costs

Total purchase costs $2.03MM
Total bare module costs $6.94MM
Direct permanent investment $17.02MM
Total depreciable investment $20.09MM
Total permanent investment $22.90MM
Working capital $1.70MM
Total capital investment $24.60MM

Using the Individual Factors (IF) method outlined by Guthrie, 1969, 1974, the estimated
purchased costs were calculated based on the CE Index of 567 which was the Chemical
Engineering Index value for 2013. The facility was assumed to be at sea level so when converting
operating pressures from psia to psig, 14.7 was subtracted from the pressure in psia.
In the IF method, free-on-board purchase costs of all equipment was estimated, and
individual factors (Seider at al., 2017) were incorporated to each unit operation to estimate the
overall installation and capital costs. The sum of these values constituted the total bare module
costs (CTBM). Direct permanent investment (CDPI) and total depreciable investment (CTDC) were
then calculated. Land, royalties, and startup were added to CTDC to estimate the total permanent
investment (CTPI). The working capital (WC) was then determined before being added to CTPI to
produce total capital investment (CTCI). These calculations were based on the projected CE Index
of 590 which was associated with the year of 2019. A summary is shown below.

Total Bare Module Cost, CTBM

Direct Permanent Investment, CDPI = CTBM + Csite + Cservice + Callocated
Site Prep (Csite) = 5% of CTBM
Services (Cservice) = 5% of CTBM
Allocated Costs (Callocated) = The sum of following individual costs
High pressure/Low-pressure steam: 930*[Steam flow(lb/h)]0.81
Cooling water: 1100*[water flow(gpm)]0.68
Electricity: 2900000*[Power(W)]0.83
Total Depreciable Capital, CTDC = CDPI + Ccon
Contingency and Contractor Fees (Ccon)= 18% of CDPI
Total Permanent Investment, CTPI = CTDC + Cland + Croyalties + Cstartup
Land (Cland) = 2% of CTDC
Royalties (Croyalties) = 2% of CTDC
Startup (Cstartup) = 10% of CTDC
Total Capital Investment, CTCI = CTPI + WC

Direct plant depreciation was estimated over a 10-year period. The working capital (WC)
was calculated based on a 1-week inventory, a 1-month cash reserve, a 1-month account
receivable, and a 1-month accounts payable. The purchased costs of pilot-scale equipment were
also included in the capital investment calculations.
All the operating costs were summarized in Table 13 below. Since our process was
designed to be a part of Starbuck’s Augusta Soluble Coffee plant, the SCGs were assumed to be
free. Also, four operators would be required for each shift.
 19

Table 13. Operating Costs

Raw materials $1.95MM
Utilities $5.55MM
Operations $2.47MM
Maintenance $1.60MM
Operating overhead $0.62MM
Property taxes and insurance $0.40MM
Depreciation $1.98MM
General expenses $0.73MM
Total production cost $15.30MM

4.2 Economic Analysis

Given an income tax rate of 40% and an interest rate of 22%, the venture loss was
determined to be $10.82MM.
Using the same income tax and interest rates as venture profit analysis, the net present
value (NPV) was determined to be negative $40.62MM over a 10-year period as shown in Table
X below. This means this investment would lead to a substantial financial loss. It should also be
noted that the cumulative PV remained negative for all years.

Table 14. Cumulative present value (PV) over 10-year period

Year Cumulative PV
0 ($22.90)
1 ($27.46)
2 ($29.94)
3 ($32.23)
4 ($35.99)
5 ($35.73)
6 ($37.45)
7 ($38.67)
8 ($39.66)
9 ($40.48)
10 ($40.91)
11 ($40.89)

5. Recommendations and Future Work

5.1 Recommendation
Based on the current process analysis, the design is extremely unprofitable with a net
present value of about negative $40MM. Thus, moving forward into the pilot plant and even full-
scale construction phase is not recommended until significant cost saving measures are discovered,
or the price of the products increases dramatically. Operating costs is determined to be $15MM
and exceeds our sales of $6.31MM. Most of the operating costs come from utilities. Other
significant costs are related to the requirement of four operators for the rather complicated process.
 20

5.2 Future Work

In general, all future work should be put towards attempting to make the process profitable
through cost optimizations. The main potential for making this process more cost effective would
be investigating methods for reduction in utility expenses within the process. Currently, there is a
significant amount of steam costs associated with the methanol removal, purification of glycerol,
and purification of the FAME biodiesel. If optimizations are found here, the process will be
significantly closer to profitability.
Creating bio-char out of the post-reaction SCGs was originally determined to be very
unprofitable at current expected bio-char sale prices when compared to the energy costs required
to turn the SCGs into bio-char. Potential for reduction in processing and energy use in the bio-char
creation process likely still exists, and with significant optimizations may once again become
profitable.
The profitability of glycerol production and methanol recycling should also be
investigated, as these processes might be more expensive then compared to just treating the
materials for discharge to appropriate waste treatment facilities. Both distillation columns have
significant steam energy costs that can be potentially eliminated in favor of simply treating and
discharging the waste.
Non-cost optimization recommendations for future work include better data collection of
the specific transesterification process. This project assumes that the transesterification reaction
occurs within the coffee beans and then the product is extracted by the methanol. The process also
assumes that treating the SCGs beforehand with H2SO4 is a necessary step in the whole process.
There are potential significant optimizations to be made if these assumptions are not accurate. For
example, the H2SO4 can be added after extraction of the lipids to perform the transesterification
while avoiding the more complicated washing of the SCGs with the acid. Because of unknowns
like the previously mentioned, a full accounting of the reaction process in the lab and full
understanding of where all the reactants end up would be beneficial.

 21

References
1. Liu, Y., et al., “Direct transesterification of spent coffee grounds for biodiesel
production,” Fuel, 199, pp. 157-161 (2017).
2. Starbucks®, “Roasting plants and distribution centers – Augusta Roasting Plant –
Augusta, Georgia,” https://www.starbucks.com/careers/find-a-job/manufacturing-and-
distribution (Accessed Dec. 10, 2018).
3. Statista, “Method of preparation among past-day coffee drinkers in the United States in
2018” https://www.statista.com/statistics/320339/method-of-preparation-among-past-
day-drinkers/ (Accessed Dec. 10, 2018).
4. “US Coffeehouse sales expected to reach $28.7 billion by 20221: Despite increased
competition from ready-to-drink coffee, US coffeehouse sales are expected to reach USD
$28.7 billion by 2021,” Tea & Coffee Trade Journal, 13 (Feb. 2018).
5. Starbucks®, “Fiscal 2017 Annual Report,”
https://s22.q4cdn.com/869488222/files/doc_financials/annual/2017/01/FY17-Starbucks-
Form-10-K.pdf (accessed Dec. 10, 2018).
6. Vardon, D. R., et al., “Complete utilization of spent coffee grounds to produce biodiesel,
bio-oil, and biochar,” ACS Sustainable Chemistry and Engineering, 1, pp. 1286-1294
(2013).
7. Methanex Corporation, “Current posted prices,” https://www.methanex.com/our-
business/pricing (accessed Dec. 10, 2018).
8. Index mundi, “Lime prices in the United States, by type,”
https://www.indexmundi.com/en/commodities/minerals/lime/lime_t5.html (accessed Feb.
22, 2019).
9. American Society for Testing and Materials, “Standard Specification for Biodiesel
Fuel (B100) Blend Stock for Distillate Fuels,” ASTM D6751-02, West Conshohocken,
PA (2002).
10. SRS International Corporation, “Glycerin Specifications,”
http://www.srsbiodiesel.com/technologies/glycerin-purification/glycerin-specifications/
(accessed Dec. 10, 2018).
11. NESTE, “Biodiesel prices (SME & FAME),” https://www.neste.com/corporate-
info/investors/market-data/biodiesel-prices-sme-fame-0 (accessed Feb. 22, 2019).
12. Turton R., et al., “Analysis, synthesis, and design of chemical processes,” 4th ed.,
Pearson Education, Upper Saddle River, NJ (2012).
13. Seider, W. D., et al., “Product and Process Design Principles – Synthesis, Analysis, and
Evaluation,” 4th ed., Wiley, Hoboken, NJ (2017).
14. Akers, S. M., et al., “Determination of the heat of combustion of biodiesel using bomb
calorimetry,” Journal of Chemical Education, 83 (2) (Feb. 2, 2006).
15. Ballesteros, L. F., et al., “Chemical, Functional, and Structural Properties of Spent
Coffee Grounds and Coffee Silverskin,” Food Bioprocess Technology, 7, pp. 3493-3503
(2014).
16. Sherkhane, A. Y., et al., “Conversion of spent coffee grounds into renewable energy,”
Proceedings of the National Seminar on Recent Advance in Waste Water Treatment and
Disposal, India (2017).
17. Correa J. L. G., et al., “Drying of spent coffee grounds in a cyclonic dryer,” Coffee
Science, 9 (1), pp. 66-74 (2014).
18. Kusdiana, D., and S. Saka, “Effects of water on biodiesel fuel production by
 22

supercritical methanol treatment,” Bioresource Technology, 91, pp. 289-295 (2004).

19. Duran, M. A., et al., “Fractionation of green coffee oil by molecular distillation:
modeling and simulation,” Journal of Materials Science and Engineering A, 1, pp. 264-
271 (2011).
20. Al-Hamamre, Z., et al., “Oil extracted from spent coffee grounds as a renewable source
of fatty acid methyl ester manufacturing,” Fuel, 96, pp. 70-76 (2012).
21. Park, J., et al., “In-situ transesterification of wet spent coffee grounds for sustainable
biodiesel production,” Bioresource Technology, 221, pp. 55-60 (2016).
22. Li, X., et al., “Energy recovery potential analysis of spent coffee grounds pyrolysis
products,” Journal of Analytical and Applied Pyrolysis, 110, pp. 79-87 (2014).
23. Kelkar, S., et al., “Pyrolysis of spent coffee grounds using a screw-conveyor reactor,”
Fuel Processing Technology, 137, pp. 170-178 (2015).
24. Yaman, S., “Pyrolysis of biomass to produce fuels and chemical feedstocks,” Energy
Conversion and Management, 45, pp. 651-671 (2004).
25. Laird, D., et al., “Impact of biochar amendments on the quality of a typical Midwestern
agricultural soil,” Geoderma, 158, pp. 443-449 (2010).
26. International Biochar Initiative, “Standardized product definition and product testing
guidelines for biochar that is used in soil,” Product Definition and Specification
Standards (2015).
27. Rehnlund, B., “Outlook on standardization of alternative vehicle fuels,” Atrax Energi
and IEA Advanced Motor Fuels Implementing Agreement, Sweden (2008).
28. Henan Doing Mechanical Equipment Co., Ltd, “Rotocel extractor in cooking oil
solvent extraction plant,” http://www.doinggroup.com/index.php?u=show-1277.html
(accessed Feb. 01, 2019).
29. The Dow Chemical Company, “DOWTHERM A Heat Transfer Fluid,”
http://msdssearch.dow.com/PublishedLiteratureDOWCOM/dh_0030/0901b803800303cd
.pdf (accessed Feb. 28, 2019).
30. CarbonFund, “Emissions Calculator,” https://carbonfund.org/business-calculator/
(accessed Mar. 11, 2019)
31. Lyons, B., White III, C., “Process Equipment Cost Estimation Final Report,”
https://www.osti.gov/servlets/purl/797810/ (accessed Mar. 11, 2019)
32. Mixer Direct, “50 Gal, 316SS, Slope Bottom Tank, #4 Finish,”
https://www.mixerdirect.com/collections/stainless-process-tanks/products/50-gal-316ss-
slope-bottom-tank-4-finish (accessed Mar. 11, 2019)
33. Best Value Vacs, “Pre-Built 50L Stainless Steel Jacketed Reactor,”Best Value Vacs,
“Pre-Built 50L Stainless Steel Jacketed Reactor,” https://www.bestvaluevacs.com/50l-
stainless-steel-jacketed-
reactor.html?utm_source=google_shopping&gclid=Cj0KCQiAn4PkBRCDARIsAGHmH
3fBZjHYpgibl0iTe829A3lKxeADeG69dg3lLf2UbfUyK2xHNj05gOYaAmjeEALw_wc
B (accessed Mar. 11, 2019)
34. Process Engineering Equipment, “100 Gallon Stainless Steel Jacketed Fermentation
Processing Tank W Internal Pres,” https://www.ebay.com/i/312225979731?chn=ps (accessed
Mar. 11, 2019)
35. Heinzen, “Drying,” https://www.heinzen.com/processing-solutions/drying (accessed
Mar. 11, 2019)
36. Apeks, “Distillation & Extraction System Pricelist,”
 23

https://www.apekssupercritical.com/wp-content/uploads/2013/09/Distillation-Bi-Fold-
0822132.pdf (accessed Mar. 11, 2019)
37. Alibaba, “Solid-liquid separator,” https://www.alibaba.com/product-detail/solid-liquid-
separator-for-pig-
manure_60776442009.html?locphyscl=9015711&pla_localcode=&pla_country=US&pla
_prdid=60776442009&src=sem_ggl&src=sem_ggl&adgrp=63830955303&cmpgn=1675
096474&pla_group=293946777986&ntwrk=g&pla_lang=en&gclid=CjwKCAiA_P3jBR
AqEiwAZyWWaLwzKb36-IDpuypDV447Nk3o-xvfp6pLAYmTz-
8_PmOQAG1Ww73GrhoCy5QQAvD_BwE&dvcmdl=&pla_adtype=pla&pla_channel=o
nline&position=1o4&pla_mrctid=131281262&device=c&mark=google_shopping&mark
=shopping&locintrst=#shopping-ads (accessed Mar. 11, 2019)
38. Central, “Electric Fully-Jacketed Kettle, 100 Gallon,”
https://www.centralrestaurant.com/Electric-Fully-Jacketed-Kettle-100-Gallon-
c108p29219.html?st-t=google_shopping_515-
729&gclid=CjwKCAiA_P3jBRAqEiwAZyWWaDaUuEY9VV1_KUivqJDrnSvL4TfVY
4t-O_Ym3C_CYQmnseAQM4WSxhoC5JIQAvD_BwE (accessed Mar. 11, 2019)
 24

Appendices
A. Hyperlinks to Safety Data Sheets
B. Summary of Physical Properties
C. Material and Energy Balance for Process and Utility Streams
D. Example Process Calculations
E. Emission Calculations
F. Example Economic Calculations
G. Specification Sheets
H. Product Properties
 25

A. Hyperlinks to Safety Data Sheets

Methanol
Sulfuric Acid
Calcium Oxide
Gypsum
Dowtherm A
Glycerin
Biochar
Biodiesel
Coffee Ground
Water
B. Summary of Physical Properties
The following tables summarize the physical properties of materials used in this project. These values can be found in section
9 (physical and chemical properties) of each safety data sheet referenced in Appendix A.

Physical Methanol Sulfuric Calcium Gypsum Glycerin Biodiesel Coffee Grounds Water
Property Acid Oxide

physical state liquid liquid powder solid liquid liquid powder liquid
color colorless colorless to white white/gray clear colorless white, grey, colorless
brown brown, red
molecular 32.05 98.08 56.08 - 92.09 - - 18.02
weight (g/mol)

boiling point 148.5 554-640.4 5162 - 554 298.4 - 212

(°F)
melting point -144 50 4737 - 64.4 - >2192 32
(°F)
flash point 49.5 - - - 320 >125 - -
(closed cup, °F)

vapor pressure 16.9 <.001 - - 0.0003 0.0027 - 2.72

at ambient (kPa)
specific gravity 0.79 1.84 - 2.32 - 2.87 1.261 - - 0.998
solubility in 1000 - - 0.2 - - Not soluble in -
water (g/L) water

auto-ignition 851 - - - 752 500 - -

temperature (°F)
octanol/water 0.77 - - - - - - -
partition coeff.
(L/kg)

C. Material and Energy Balance for Process and Utility Streams
Please refer to the Excel workbook titled “Appendix C” for all material and energy balances.

 28

D. Example Process Calculations

Please refer to the Excel Workbook titled “CHE 5046-1910 Process Calculations” for more
information.

 29

E. Emission Calculations

CO2 Equivalent for Electricity: 7.44*10-4 metric tons CO2/kWh

CO2 Equivalent for Natural Gas: 117 lb CO2 / MMBtu of Natural Gas (NG)

Electricity used per year: 32.810 MWH

CO2 from Electricity = Electricity usage * CO2 Equivalent
CO2 from Electricity = 32,810.8 kWh/year * 7.44*10-4 MT CO2 / kWh
CO2 from Electricity = 24.411 MT CO2 / year

Assuming 90 psig steam was generated from burning NG,

CO2 for Natural Gas = Gas Usage * CO2 Equivalent
CO2 for Natural Gas = (25.8525 + 70.1895) MMBtu / hr * 8000 hr /year * 117 lb/MMBtu NG /
0.000453592 MT/lb
CO2 for Natural Gas = 1.98*1011 MT CO2 / year
Total Emissions = 24.411 MT CO2 / Year + 1.98*1011 MT CO2/year
Total Emissions = 1.98*1011 MT CO2/year

 30

F. Example Economic Calculations

Please refer to the Excel Workbook titled “CHE 5046-1910 Economics Analysis” for more
detail.
 31

G. Specification Sheets

See the attached spec-sheet excel file named “CHE 5046-1910 Appendix G” for full unit-op
specifications.
 32

H. Product Properties

Table 15. Biodiesel Specifications

 33

Table 16. Biochar Product Specifications

 34

Table 17. Glycerin Specifications

Table 18. FAME Specifications