Renewable Fuel Production by in Situ Hydrotreatment of Spent

9th Int'l Conference on Advances in Science, Engineering, Technology & Waste Management (ASETWM-17) Nov. 27-28, 2017 Parys, South Africa
Renewable Fuel Production by in Situ
Hydrotreatment of Spent Coffee Grounds
C. Truter, R. Venter, and S. Marx

Abstract— Renewable diesel production from bio-oils is more
expensive in comparison to petroleum diesel, with the production of
bio-oils from pyrolysis and liquefaction being significant
contributors. The aim of this project is to assess the liquid yield
obtainable by the in-situ hydrotreatment of spent coffee grounds
through hydrotreatment. The spent coffee grounds are covered with
a solvent and hydrotreated in a low or zero oxygen environment
within a batch reactor loaded with catalyst. At certain conditions a
significant increase in liquid product yield is observed, indicating
that not only does hydrotreatment take place, but liquefaction
forming bio-oils. These bio-oils are also then hydrotreated
increasing the liquid yield obtained from the reactor.
Keywords— in situ hydrotreatment, liquefaction, renewable
fuel, spent coffee grounds.
I. INTRODUCTION
Due to the large volumes of fossil fuels required to supply
the global demand for fuel, the confirmed reserves of fossil
resources are being exhausted [1]. Additionally, the
consumption of fossil fuels is leading to an increase in carbon
dioxide emitted into the atmosphere, with the global
transportation industry playing a substantial part [2].
Alternative energy sources for fossil fuels, such as biodiesel,
renewable diesel and bio-ethanol may be the key to the
reduction of the global dependence on fossil resources. Most
commonly these alternative fuels are produced from edible
feedstock for instance rapeseed oil, sunflower oil, palm oil or
soybean oil [3]. The use of edible feedstock is leading to an
imbalance of the global food supply in a world that is already
facing food insecurity [3]. Therefore, a waste to energy
concept is more widely acceptable in which waste and nonedible feedstock are used for the production of alternative
fuels.
Spent coffee grounds (SCG) are the fine residue obtained
when coffee grounds have been milled and infused with hot
water to produce various beverages. On a dry weight basis,
SCG contain between 11 wt.% - 20 wt.% of fatty acids that
Manuscript received November 6, 2017. This work was supported by the
North-West University (NWU) Potchefstroom Campus, Faculty of Engineering.
C Truter is a final year chemical engineering student at NWU (e-mail:
chantel.truter0@gmail.com).
R. Venter is a Post-Doctoral Researcher at the Chemical Engineering
Department, North West University, Potchefstroom campus. e-mail:
10303685@nwu.ac.za
S. Marx is NRF Research Chair in Biofuels, School of Chemical and
Minerals
Engineering
North
West
University
(e-mail:
Sanette.Marx@nwu.ac.za).
https://doi.org/10.17758/EARES.EAP1117083
209
can be converted into bio-oil [3].
Renewable diesel is preferred to bio-diesel due to the
difference in fuel properties, specifically considering the cold
flow properties and oxygen content [4]. The composition of
renewable diesel is very similar to the composition of
petroleum diesel, resulting in an alternative fuel that can be
used as a 100% blend [4]. Three main methods are used for
the upgrading of bio-oil subsequently used in the production
of renewable diesel; hydrodeoxygenation/hydrotreating,
zeolite upgrading or emulsion formation [5]. The
hydrotreatment process has also been used for the production
of C12-C18 n-alkanes from triglyceride based oils [5]. The
major advantage hydrotreatment has over trans-esterification
is the zero-oxygen content within the liquid fuel product,
resulting in an increased storage life and higher energy
density [6]. During hydrotreatment, hydrogen reacts with
both the oxygen atoms and unsaturated carbon bonds to
produce saturated C-C bonds and water.
Renewable diesel produced by means of the hydrotreatment
of biomass is a costly procedure due to the fact that multiple
stages are essential for suitable oil extraction to be used as
feedstock. In order to reduce the cost of production, in situ
hydrotreatment is considered for the production of renewable
diesel as alternative to more traditional approaches such as
liquefaction and pyrolysis for oil production to be used as
feedstock for hydrotreatment. In this study, spent coffee
grounds were directly hydrotreated using typical
hydrotreating conditions to assess the feasibility of in situ
renewable fuel production.
II. EXPERIMENTAL METHODS
A. Materials
Spent coffee grounds were used as feedstock in this study,
procured from a local coffee brewery, Toro®. Additionally,
isooctane (99 %), 1-methylnapthalene (95 %) and ethylene
glycol (99 %) were used as solvents. The isooctane and 1methylnapthalene were procured from Sigma – Aldrich. The
ethylene glycol was procured from ACE and the ethanol from
Rochelle Chemicals. Nitrogen (99.999 %), Hydrogen (99.999
%) and H2S in Argon (14.9 %) was purchased from Afrox
Potchefstroom. NiMo/y-Al2O3 commercial catalyst was
obtained from a commercial catalyst supplier.
The feedstock, spent coffee grounds, were analyzed by Irene
Analytical Services based in Pretoria. The analysis results are
shown in Table I.
9th Int'l Conference on Advances in Science, Engineering, Technology & Waste Management (ASETWM-17) Nov. 27-28, 2017 Parys, South Africa
TABLE I - SPENT COFFEE GROUND COMPOSITION OBTAINED FROM EXTERNAL
ANALYSIS AT ARC - IRENE ANALYTICAL SERVICES
Content
Value
Dry Matter (%)
94.5
Ash (%)
1.34
Protein (Nx6.25) (%)
12.71
Fat (Ether extraction) (%)
12.86
Carbohydrates (calculated) (%)
67.62
Neutral detergent fibre (%)
66.11
Acid detergent fibre (%)
31.14
Acid detergent lignin (%)
11.88
Hemicellulose (%)
34.97
Cellulose (%)
19.26
Lignin (%)
10.54
accumulated within the Buchner funnel is then analyzed
using a gas chromatograph mass spectrometer (GC-MS).
In order to ensure that all the liquid is recovered from the
aluminum cup and the reactor, it was rinsed using
dichloromethane and filtered through the filter paper in the
Buchner funnel. The dichloromethane was then evaporated
leaving the liquid product behind. The solids (catalyst and
char mixture) which remain on the filter paper is dried and
weighed.
The total liquid yield of the run is calculated as the
percentage of the feed that has been converted into liquids
using equation 1.
(1)
represents the mass of the liquid product and
the
mass of the feedstock. The diesel yield is then calculated
using equation 2 as the fraction of the total liquid product
with a boiling point within the 240°C to 370°C diesel fraction
range.
B. Methods
1)Apparatus
All the experiments were done in a batch autoclave reactor.
The vessel of the reactor has a volume of 350 cm3, a
maximum operating temperature of 420°C and a maximum
pressure of 200 bar, however the release valve of the vessel is
set at a pressure of 150 bar. A heating jacket was used to heat
the reactor and a magnetic coupled stirrer is fitted at the top
of the reactor. Compressed air and cooling water was used to
protect the magnetic coupled stirrer from overheating during
the reaction.
2)Catalyst Preparation and Activation
A catalyst to reagent weight ratio of 1:10 was used in this
study. The catalyst is dried over an hour at 100°C and placed
inside an aluminum cup fitted in the reactor. The reactor is
closed off and purged with nitrogen for 30 min, removing any
unwanted air inside the reactor. The reactor is pressurized
with H2S and heated to 400°C. The reactor is held at these
operating conditions for 1 hr. after being cooled with
compressed air and a fan to 35°C.
(2)
epresents the fraction of the liquid product falling in the
diesel boiling range. The diesel selectivity is further
calculated using equation 3:
(3)
Finally, the yield for the diesel, kerosene and naphtha from
the SCG is calculated as illustrated in equation 4.
(4)
Represents the different factions within the liquid
product.
The sample for the GC-MS (Agilent 7890A, 5975C inert
MSD, with triple axis detector) is diluted in a vial and
consists of 0.02 g sample and 1.3 g DCM. The DCM is added
as diluent into the vial. The calibration standard for the GCMS pertaining to the simulated distillation was obtained from
Supelco, Pennsylvania, USA and contains normal alkanes
from C8 to C40 (Bachler , et al., 2010). The data obtained
from the analysis completed using the GC-MS is further
processed and simulated distillation curves are drawn up
using a modified method in order to determine the boiling
ranges for the liquid product obtained.
After separation of the contents of both the reactor and the
aluminum cup the higher heating value of the liquid product
was tested using a bomb calorific meter (IKA® C500). The
sample is prepared according to the calibration of the meter
used. The sample is weighed and the weight transferred to the
calorific meter. The sample is loaded into the bomb together
with a cotton thread that is ignited in the presence of pure
oxygen. The increase in temperature of the water in the
calorific meter is noted and used to determine the higher
heating value of the sample in the bomb.
3)Reaction
After the reactor system is depressurized into the chemical
hood, the reactor is purged with hydrogen for 5 min.
displacing all the remaining H2S in the reactor. The solvent is
introduced into the reactor by injection through a rubber
septum. The biomass is added into the reactor by re-opening
the reactor while purging with nitrogen, introducing the
biomass and closing the reactor off again. The reactor is
purged with hydrogen for 3 min displacing the nitrogen and
then pressurized with hydrogen to 8 MPa (initial operating
pressure). The magnetic stirrer is switched on together with
the heating oven. The reactor is heated to the operating
temperature of 390°C and kept there for 1 hr. The reacting
system is allowed to cool to 35°C before the content of the
reactor is removed and analyzed.
C. Liquid Product Analysis
The liquid and solid product is removed from the reactor
after the cooling process has been completed. The content of
both the aluminum cup and the reactor is separated from the
solid product by using a Buchner funnel. The liquid product
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9th Int'l Conference on Advances in Science, Engineering, Technology & Waste Management (ASETWM-17) Nov. 27-28, 2017 Parys, South Africa
III.
depolymerization of the lignocellulose may occur leading to
the formation of kerosene and naphtha fractions in the liquid
product.
In consideration of the boiling range distribution and the
liquid product composition comparisons of each solvent
loading the low solvent to biomass ratio is more favorable for
the production of renewable fuel that may be comparable to
petroleum diesel in further studies. Additionally, not only is
diesel formed during hydrotreatment but also kerosene as part
of the liquid product. Thus, more valuable fuel compounds
are extracted from the feedstock although separation is
required after the hydrotreatment process.
RESULTS AND DISCUSSION
A. Hydro-Processing of SCG in the Presence of isooctane
1)The Effect of Solvent Loading on the Boiling Point
Distribution Range of the Liquid Product
The hydrotreatment of different solvent loadings with a
constant feedstock mass of 5 g was studied and compared.
Error! Reference source not found. represents the simulated
distillation curves for the 55 g and 6 g solvent loadings. The
conditions at which the comparison was done, were 8 MPa,
390°C and one-hour of residence time at constant reaction
temperature.
Fig. 2 - The effect of solvent loading on the liquid product
composition for the hydrotreatment of SCG in the presence of
isooctane. ( n-Alkanes i-Alkanes Aromatics. Cyclic
alkanes Olefins
Oxygenates)
Fig. 1 - The effect of solvent loading on the boiling range
distribution for 55 g and 6 g solvent loadings during the
hydrotreatment of SCG in the presence of isooctane. ( 55 g solvent
6 g solvent)
The composition of the liquid product formed for both the
high (55:5) and low (6:5) solvent loadings are illustrated in
Error! Reference source not found.. The high solvent
loading hydrotreatment run resulted in mostly n-alkane
compounds as part of the liquid product formed during the
hydrotreatment of the SCG. Contrary to the high solvent
loading run, a lower solvent loading run resulted in more
isomers, aromatics and cyclic compounds forming.
The solvent loadings were varied at 55 g and 6 g to 5 g of
biomass respectively. The 55 g loading resulted in a diesel
fraction of 99 wt.%. A significant increase in kerosene
fraction is noted at a fraction of 16.42 wt.% for the 6 g
solvent loading as illustrated in Error! Reference source not
found.. The 55 g solvent loadings resulted in no noteworthy
quantities of kerosene formation. A higher solvent to biomass
ratio resulted in the formation of kerosene as well as diesel
fractions in the liquid product. Moreover, the production of
kerosene indicates that not only has the fatty acids in the
spent coffee grounds been converted to renewable diesel but
additionally the lignocellulose containing cellulose,
hemicellulose and lignin and other ingredients such as
proteins have undergone liquefaction and hydrotreatment,
resulting in the lighter kerosene fraction. The formation of
the lighter fractions such as kerosene and naphtha may be
attributed to depolymerization of the materials other than
fatty acids such as lignocellulose during the hydrotreatment
process. Various articles such as reviewed in [7] indicate that
a high selectivity and conversion of lignin is obtained through
polymerization using super critical fluids. Isooctane has a
critical pressure of 25.7 ± 0.2 bar and a critical temperature of
270.75 ± 0.4°C [8]. Therefore, isooctane is at super critical
conditions during the hydrotreatment process and
https://doi.org/10.17758/EARES.EAP1117083
2)The effect of biomass loading on the liquid product yield
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9th Int'l Conference on Advances in Science, Engineering, Technology & Waste Management (ASETWM-17) Nov. 27-28, 2017 Parys, South Africa
Fig. 3 - The effect of biomass loading on the liquid product yield
during hydrotreatment of SCG in the presence of isooctane (
Diesel yield
Kerosene yield
Naphtha yield)
through liquefaction are thereafter hydrotreated, resulting in a
hydrotreated liquid product.
3)The Effect of Biomass Loading on The Liquid Product
Composition
The hydrotreatment of different biomass loadings with a
constant isooctane loading of 6 g was studied and compared.
The conditions at which the comparison was done, were 8
MPa, 390°C and one-hour of residence time at constant
reaction temperature. After each run the reactor content was
filtered using a Buchner funnel and the remaining catalyst on
the filter paper was washed with dichloromethane (DCM)
extracting all the liquid product from the solids. Fig. 3 shows
the diesel, kerosene and naphtha yield obtained for each of
the biomass loadings in grams per kilogram SCG.
The diesel yield for the 5 g biomass loading was 309 g/kg
SCG. The diesel yield for the 4 g biomass loading was 430
g/kg SCG and 264 g/kg SCG for the 3 g biomass loading.
From figure 4-1 it is clear that the highest diesel yield was
obtained from the 4 g biomass loading as well as the highest
kerosene and naphtha yield is also observed with the 4 g
biomass loading. This indicates that for the experimental
setup in this study the 4 g biomass loading proves to be the
most favorable choice from a biofuel production point of
view. Experimental error for this project was determine by
repeating the 4 g biomass, 6 g solvent loading experiments
and an experimental error of 6.22% was calculated.
The liquid product of the 5 g biomass feed loading
comprised of 31 wt.% of diesel and 5 wt.% of kerosene with a
total liquid product yield of 36.98 %. The 4 g biomass feed
delivered a 43 wt.% of diesel, 10 wt.% of kerosene and 1
wt.% of naphtha with a total liquid yield of 62.60 % and the 3
g loading of biomass contained 26 wt.% diesel and 9 wt.%
kerosene with a total liquid yield of 35.01 %. The highest
yield was obtained at the biomass loading of 4 g, assuming
that a harmonious ratio of biomass to solvent has been
reached, resulting in a significantly higher liquid yield
attained in comparison to the three and five gram spent coffee
ground loadings.
This resulted in a diesel selectivity for the 5 g biomass
loading at 5.76, the 4 g loading with 3.77 and the 3 g biomass
loading with 3.08. A preference towards the production of
diesel is shown for all three cases although a decrease in
diesel selectivity is noted with a decrease in the biomass
loading.
For the 4 g biomass loading case, the liquid product had an
average gross calorific value (CV) of 44.334 MJ/kg. This
value is comparable to literature which is 45 MJ/kg for
renewable diesel (Anon., 2016). The higher heating value for
spent coffee grounds was measured to be 22.14 MJ/kg which
was increased with 22.194 MJ/kg to 44.334 MJ/kg by means
of in-situ hydrotreatment of the SCG.
Moreover, on a dry weight basis, SCG contains between 11
wt.% – 20 wt.% fatty acid oil (Phimsen, et al., 2016). For all
three the biomass loadings in this study a liquid product yield
greater than 20 wt.% was obtained, indicating the likelihood
of liquefaction and hydrotreatment of the SCG simultaneously
taking place during hydrotreatment. The bio-oils produced
https://doi.org/10.17758/EARES.EAP1117083
The hydrotreatment of different biomass loadings with a
constant isooctane mass of 6 g was studied and compared.
The conditions at which the comparison was done, were 8
MPa, 390°C and one-hour of residence time at constant
reaction temperature. All the runs were washed with
dichloromethane (DCM) extracting all the liquid product
formed. Fig. 4 illustrates the liquid product composition for
each biomass loading obtained.
Fig. 4. - The effect of biomass loading on the liquid product
composition during hydrotreatment of SCG in the presence of
isooctane. ( n-Alkanes i-Alkanes Aromatics
Cyclic
alkanes
Olefins
Oxygenates)
The largest fraction of all three biomass loadings were nalkanes. The 4 g biomass loading resulted in the largest
fraction of isomers in the liquid product, leading to a decrease
in the peak area of the straight alkane chains formed. This
may be due to an optimal biomass to solvent ratio for the
favoritism of isomers. A higher content of isomers within the
liquid product may lead to favorable cold flow properties of
the liquid product.
Similar peak areas are seen for the 4 g and 5 g biomass
loading in consideration of cyclic component formation, with
a small increase in aromatic compounds for the 3 g biomass
loading in comparison to the 4 g and 5 g biomass loadings.
Insignificant amounts of alkenes and oxygenates were found
in all three the compared cases
B. Hydro Processing of SCG In the Presence of Different
Solvents
For the optimal biomass and solvent loading ratio
determined, the hydrotreatment of varying solvents with a
constant feedstock mass of 4 g and constant solvent mass of 6
g was studied and compared. The conditions at which the
comparison was done, were 8 MPa, 390°C and one-hour of
residence time at constant reaction temperature.
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9th Int'l Conference on Advances in Science, Engineering, Technology & Waste Management (ASETWM-17) Nov. 27-28, 2017 Parys, South Africa
Isooctane as solvent resulted in a diesel fraction of 69 wt.%
with a kerosene fraction in the liquid product of 16 wt.%. A
diesel fraction of 85 wt.% with a kerosene fraction of 15 wt.%
was obtained using the ethylene glycol as solvent. For the
methylnaphthalene a much smaller diesel fraction of 38 wt.%
is noted, resulting in a kerosene fraction of 62 wt.%. For both
these solvents no naphtha or heavy fractions were observed
At the same operating conditions, biomass and solvent
loadings, ethylene glycol as solvent resulted in the highest
diesel fraction. The largest kerosene fraction was obtained
using
methylnaphthalene as solvent
during the
hydrotreatment of SCG.
2-methyl-cis-cyclohexane, decahydro-2-methyl-naphthalene,
(2-methy-1-butenyl)-benzene
and
1,2,3,4-tetrahydro-5methyl-naphthalene. For the hydrotreatment of the SCG
experimental case in the presence of 1-methyl-naphthalene
the components that did not match with a component in the
case without the SCG are assumed to be formed from either
the lignocellulose that has undergone liquefaction and
hydrotreatment or from cracking of the C15-C18 n-alkanes.
After the hydrotreatment of the SCG in the presence of all
three solvents investigated during the experimental period, no
significant amounts of oxygenates are present in the liquid
product of each case. The absence of oxygenates is a clear
indication of successful deoxygenation in each case.
IV.
The effects of varying solvent loadings, varying biomass
loadings and different solvents during the hydrotreatment of
SCG was examined in a batch reactor system. The solvent to
biomass ratio was varied at a high of (55:5) and low of (6:5)
individually. The biomass loading was varied at 5 g, 4 g and
3 g respectively. Lastly, three different solvents, namely;
isooctane, ethylene glycol and 1-methylnaphthalene were
tested.
The low solvent to biomass ratio of (6:5) resulted in the
formation of a higher ratio in the kerosene fraction, whilst
maintaining a high diesel ratio of 83.58 wt.% in the presence
of isooctane. The low solvent to biomass ratio was thus found
not only feasible for the production of renewable diesel from
SCG through hydrotreatment but additionally formed
kerosene which indicates the possibility of liquefaction of the
lignocellulose within the SCG. These two fractions will
however have to be separated in an additional step.
The 4 g biomass loading in the presence of isooctane
resulted in the highest diesel yield of 430 g/kg SCG and
additionally resulted in the formation of higher kerosene and
naphtha fractions in the liquid product. As seen for the low
solvent to biomass ratio (6:5), the increase in kerosene and
naphtha factions formed may be attributed to the liquefaction
of lignocellulose that has simultaneously undergone
hydrotreatment.
The different solvents used during the hydrotreatment of
SCG, resulted in significant differences in the diesel to
kerosene ratio of the liquid product as well as the liquid
product composition. Similarities between the liquid product
composition for the different solvents may be attributed to the
compounds other than fatty acids in the SCG.
For all the experiments conducted complete oxygen
removal and saturation of olefins have been observed. The insitu hydrotreatment of SCG is feasible for the production of
renewable diesel and a decrease in cost for the production of
renewable fuel is achievable by the implementation of in-situ
hydrotreatment of SCG
Fig 5. -The effect of solvent on the liquid product composition for
the hydrotreatment of SCG. ( n-Alkanes i-Alkanes
Aromatics
Cyclic alkanes
Olefins
Oxygenates)
The liquid product composition for each solvent is
illustrated in Fig 5. It can be seen that for the
methylnaphthalene solvent the largest contributor to the
composition of the liquid product are aromatic compounds,
followed by n-alkanes and cyclic components. For both the
ethylene glycol and the isooctane, n-alkanes are the largest
contributors of the liquid product composition in each case.
Hydrotreatment in the presence of isooctane resulted in the
highest isomer content. The NiMo hydrotreating catalyst is
known for the isomerization of n-alkanes. Renewable diesel
distilled from the liquid product will exhibit improved cold
flow properties as a result of its higher isomer content.
The C15-C18 n-alkanes observed in the liquid product are
assumed to be formed due to the hydrotreatment of the fatty
acids within the SCG. All the components found in the liquid
product of an experimental run can either be attributed to the
hydrotreatment of fatty acids in the SCG, hydrotreatment of
the solvent or hydrotreatment of the other compounds such as
the lignocellulose in the SCG as well as cracking of the
longer n-alkane chains. The latter two attributions form
components which fall in the kerosene boiling range.
A comparison between the liquid product composition of
the hydrotreatment of SCG in the presence of 1-methylnaphtalene with a solvent to biomass ratio of (6:5) and the
hydrotreatment of 1-methyl-naphthalene only (6 g) was done.
The following components were found in both cases; 1-ethylhttps://doi.org/10.17758/EARES.EAP1117083
CONCLUSION
APPENDIX
Appendixes, if needed, appear before the acknowledgment.
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9th Int'l Conference on Advances in Science, Engineering, Technology & Waste Management (ASETWM-17) Nov. 27-28, 2017 Parys, South Africa
ACKNOWLEDGMENT
The financial assistance of the National Research
Foundation (NRF) towards this research is hereby
acknowledged. Opinions expressed and conclusions arrived at
are those of the author and are not necessarily to be attributed
to the NRF.
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C Truter Was born on 1 November 1995 in Klerksdorp
and matriculated in 2013 at Hoërskool Secunda. Started a
B.Eng chemical engineering at the NWU, Potchefstroom
campus in 2014. Set to graduate in 2017.
She obtained a bursary from Sasol in 2014 to complete a
B.Eng chemical engineering and is set to work for Sasol in
January 2018 after graduation.
She has been a member of the engineering student
association for four years. Contributing to the
development of the Engenius kids program (program
Author’s formal
aimed photo
at the development of mathematics and science in local schools).,
engineering schools and engineering community service project.
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