Beruflich Dokumente
Kultur Dokumente
Russell McClure, Dat Nguyen, Christine Santabarbara, Noah Skinner, Christopher Stone
15 March 2019
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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
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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 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.
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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
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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.
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.
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.
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.
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.
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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].
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.
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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
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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.
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.
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
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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.
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.
• 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
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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.
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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.
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
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References
1. Liu, Y., et al., “Direct transesterification of spent coffee grounds for biodiesel
production,” Fuel, 199, pp. 157-161 (2017).
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Augusta, Georgia,” https://www.starbucks.com/careers/find-a-job/manufacturing-and-
distribution (Accessed Dec. 10, 2018).
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2018” https://www.statista.com/statistics/320339/method-of-preparation-among-past-
day-drinkers/ (Accessed Dec. 10, 2018).
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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).
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Fuel (B100) Blend Stock for Distillate Fuels,” ASTM D6751-02, West Conshohocken,
PA (2002).
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http://www.srsbiodiesel.com/technologies/glycerin-purification/glycerin-specifications/
(accessed Dec. 10, 2018).
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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
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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)
28
E. Emission Calculations
30
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