(PDF) Synthesis of Green Diesel From Waste Cooking Oil Through Hydrodeoxygenation Technology With NiMo - γ-Al 2 O 3 Catalysts

11/14/2018 (PDF) Synthesis of Green Diesel From Waste Cooking Oil Through Hydrodeoxygenation Technology With NiMo/γ-Al 2 O 3 Catalysts
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reen Diesel From Waste Cooking Oil Through Hydrodeoxygenation Technology With NiMo/γ-Al 2 O 3 Catalysts
Available) in MATEC Web of Conferences 156(6):03032 · January 2018 with 7 Reads

matecconf/201815603032
ublication
Heri Heriyanto Sri Djangkung Sumbogo Murti

UNTIRTA 14.74 · Badan Pengkajian dan Penerapan Teknologi
Septina Is Heriyanti +1
Inayatu Sholehah
Badan Pengkajian dan Penerapan Teknologi
Show more authors
xygenation (HDO) of waste cooking oil (WCO) and trapped grease over sulfide catalysts was examined to produce high quality
ation fuel from low-grade resources. The hydrodeoxygenation of waste cooking oils was carried out in a high pressure of 30 and 60 bar
temperature of 300 – 400 °C in a batch reactor autoclave. NiMo/γ-Al2O3 catalyst was prepared and for the first time tested in
cessing of waste cooking oil. The content of NiMo/γ-Al2O3 in each catalyst was about wCo 5 wt.%. A maximum of 77,97 % green diesel
achieved at nearly complete conversion of waste cooking oil using NiMo/γ-Al2O3 at temperature of 400°C, pressure 60 bar and 4 hours
n time. The oxygen content was decreased from 14,25 wt.% to 13,35 wt.%, at temperature of 400°C, pressure of 30 bar and 1 hour of
me. The Hydrodeoxygenation process was much influenced by temperature, pressure, and time.
https://www.researchgate.net/publication/323753979_Synthesis_of_Green_Diesel_From_Waste_Cooking_Oil_Through_Hydrodeoxygenation_Technology_With_NiMog-Al_2_O_3_Catalysts 1/20
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MATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/20181560303 Ad

RSCE 2017
Synthesis of Green Diesel From Waste Cooking Oil Through

Hydrodeoxygenation Technology With NiMo/ɣ-Al2O3 Catalysts
Heri Heriyanto 1*), Sumbogo Murti, SD2, Septina Is Heriyanti2, Inayatu Sholehah1, Ayi Rahmawati1
1
Chemical Engineering Departement, Sultan Ageng Tirtayasa University, Cilegon, Indonesia, Jl. Jendral Sudirman km. 03 Cilegon
42435
2
Center of Technology Energy Resources and Chemical Industri, Agency for the Assessment and Application of Technology (BPPT),
Gedung Energi 625 Klaster V, Kawasan PUSPIPTEK, Tangerang Selatan 15314
Abstract. Hydrodeoxygenation (HDO) of waste cooking oil (WCO) and trapped grease over
sulfide catalysts was examined to produce high quality transportation fuel from low-grade
resources. The hydrodeoxygenation of waste cooking oils was carried out in a high pressure of
0
30 and 60 bar and high temperature of 300 – 400 C in a batch reactor autoclave. NiMo/ɣ-Al2O3
catalyst was prepared and for the first time tested in hydroprocessing of waste cooking oil. The
content of NiMo/ɣ-Al2O3 in each catalyst was about WCO 5 wt.%. A maximum of 77,97 % green
diesel yield was achieved at nearly complete conversion of waste cooking oil using NiMo/ɣ-
0
Al2O3 at temperature of 400 C, pressure 60 bar and 4 hours of reaction time. The oxygen
0
content was decreased from 14,25 wt.% to 13,35 wt.%, at temperature of 400 C, pressure of
30 bar and 1 hour of reaction time. The Hydrodeoxygenation process was much influenced by
temperature, pressure, and time.
1 Introduction Waste cooking oil is waste oil that can be

made from various types of cooking oil such as corn
Today energy needs continue to rise but inversely oil, vegetable oil, samin oil and so on which when
proportional to energy substitutes such as petroleum, viewed from the chemical composition of the
natural gas that can not be optimized. The amount of compounds are carcinogenic. In addition to the
available energy sources currently is sourced from fossil environmentally destructive wastes the chemical
fuels accounted for 94% of the national energy mix mix, content formed can be harmful to human health. The
comprising 47% of petroleum, 26% coal and 21% first sign of cooking oil damage is the formation of
natural gas [1]. With an economic growth of 6.3 to 6.8 acrolein in cooking oil. This acrolein causes itching
per year, energy demand is projected to grow around 6% in the throat when eating fried foods using cooking
per year until 2014. Fuel oil will continue to be prefered oil repeatedly. Acreolyn is formed from the
in the final energy demand, because in addition to the hydration of glycerol that forms an unsaturated
fact that fuel-based technologies are more efficient, fuel aldehyde.
prices can still continue to compete if compared to other
fuels such as coal and natural gas. More over, fuel oil 2.2 Green Diesel
still dominates the use of final energy, especially in the
transportation sector, because the use of fuel more Green diesel is a straight-chain hydrocarbon
practical and efficient and can not be replaced by other fraction similar to that produced by the
fuels. hydrogenation of triglycerides from vegetable oils
Considering Indonesia is the largest palm oil [4]. The injection of hydrogen with the support of a
producer in the world with oil palm production in 2014 bimetallic catalyst for the hydrotreating reaction of
reaching 33 million tons so that the potential of cooking the triglyceride compound is capable of breaking
oil produced is quite large [2]. In 2007 used cooking oil the ester or carboxylic group bond of the glycerol
(MGB) from various sources as much as 3.9 tons has not group [5,6]. Then followed the breaking of
been fully utilized. This gives a huge opportunity to carboxylic groups from the existing fatty acid
make Indonesia as a country that has a strong energy bonds as well as the saturation reaction of the
it b i it i t di l ith d bl h i b b d i t t i ht h i
resistance by processing it into greendiesel with double chain carbon bonds into straight chain
hydrodeoxygenation method, in addition to producing hydrocarbon compounds [7, 8, 9].
high fuel quality compared to biodiesel and petrodiesel,
also environmentally friendly [3]. 2.3 Hydrogenation and Hydrodeoxygenation
2 Literature Review Hydrogenation technology or Hydotreatment is

a branch of hydroprocessing such as catalytic
2.1 Waste Cooking Oil reactions using hydrogen to eliminate the atoms
heterogeneous (heteroatoms) such as sulfur,
*
Corresponding author: herfais@yahoo.com
© The Authors, published by EDP Sciences. This is an open access article distributed under the terms of the Creative Commons Attributio
icense 4.0 (http://creativecommons.org/licenses/by/4.0/).
ATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/201815603032

CE 2017
nitrogen, and oxygen, each of which is contained in analyzed in accordance to ASTM Standard such as
the compound hydrogen sulfide (H2S), ammonia viscosity, flash point and elemental analysis.The
(NH3) and water (H2O) in a process feedstock [10, operating conditions of each experiment were followed
11]. Hydrogenation process usually followed by below:
hidrodeoxygenation reaction (HDO),
decarboxylation (DCO), and decarbonylation WCO 200 g Autoclave reactor 500 ml
(DCN) or combination of them [11]. Catalyst 10 g
Sulfur powder 3 g
Hydrodeoxygenation (HDO) is a process for
eliminating oxygen hydrogenolysis of a material by HDO process
cutting the carbon-oxygen bond using hydrogen gas
[12, 13]. The content of oxygen in organic
compounds has a very important role in estimating
Filtration
the characteristics of the fuel to be generated.
Oxygen levels in vegetable oils that can reach more
than 50% by weight, have an impact on the low
calorific value, low thermal stability, corrosive, can
not be mixed with fossil fuels and the increasing
tendency towards polymerization reaction [14]. Gas product Liquid product
GC-TCD GC-FID, GC-MS, CHNS(O)

l i it fl h i t
Yield
(a)
WCO 200 g Autoclave reactor 500 ml

Catalyst 10 g
Sulfur powder 3 g
HDO process
0
P= 30 bar; T= 300 C; t= 1 hour
Fig. 1. Reaction pathway of hydrotreatment
Gas product analyze (GC-TCD)
Removing residue H 2 and

3 Methodology injecting fresh H2
The procedure in this study was including 10 grams of

NiMo/ -Al2O3 catalyst passed 200 mesh, 3 grams of
HDO process
sulfur powder and 200 grams of waste cooking oil into
P=30 bar; T=(300;330;360;400) oC; t=1 hour
the autoclave reactor. Then HDO processes were varied
on time, temperature, pressure, and number of reaction
stage with rotation speed of 800 rpm. After the HDO
process was finished, the product was filtered off and Filtration
separated between liquid and gas for analysis step.
However, in the 2-stage, after the first stage was
finished, gas in the reactor was replace by fresh
hydrogen, then the reaction was continuoued in the
second stage with the same pressure and time variations Gas product Liquid product
but with different temperatures. After the reaction
process was completed, product gas was analyzed using
GC-TCD Shimadzu GC-2014. The liquid product was GC-FID, GC-MS, CHNS(O)
GC-TCD
separated from solid material by filtering. Liquid product analyzer, viscosity, flash point
was analized using GC-FID. More over the physical and
chemical properties of liquid product was also tobe
MATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/20181560303

RSCE 2017
Yield
(b)
Fig. 2. Green Diesel Synthesis Scheme (a) Single
reaction (b) Two steps reaction 4 Discussion
4.1 Pressure and Temperature Profile
1-steel bottle; 2-valve; 3-pressure gauge; 4-reaktor;5-electrical

machine; 6-jacket; 7-thermocouple; 8 -controller
Fig. 3. Schematic and Equipments of Experimental

Fig. 4. Pressure profile on the time
Table 1. Operating Conditions

Temperature
Operating Condition ( oC)
Run Temperature Initial Time
Stage o
( ) (h )
amont T1( C) T2 pressure

P1 P2 t1(hour)t2
1 1 300 - 30 - 1 -
2 1 330 - 30 - 1 -
3 1 360 - 30 - 1 -
4 1 400 - 30 - 1 -
5 1 300 - 60 - 1 -
6 1 330 - 60 - 1 -
7 1 360 - 60 - 1 -
8 1 400 - 60 - 1 -
9 2 300 300 30 30 1 1
10 2 300 330 30 30 1 1
11 2 300 360 30 30 1 1
12 2 300 400 30 30 1 1 Fig. 5 Temperature Profile on The Time
13 1 300 - 60 - 4 -
14 1 400 - 60 - 4 -
The pressure and temperature profile of the above
reaction was observed at 4 hours reaction time. By
15 1 300 - 30 - 4 -
controlling the temperature of the coil heater in the
16 1 400 - 30 - 4 -
reactor it was desirabled that the reaction temperature
was immediately achieved and kept constant during the
reaction. The observation of the condition of the process
pressure was seen fluctuating even pressure drop on the
graph above. This pressure drop phenomenon follows
the Joule Thompson Effect theory. The hydrogen gas
stored in a guarded tube at a pressure of about 200-250
bar to remain in the gas phase was then injected into the
reactor at a pressure of 30 or 60 bar. As a result of this
pressure drop, the gas became inflate and the rapid

CE 2017
pressure drop was practically not allowing the

occurrence of external heat propagation into the system Fig. 7. Effect of Initial Pressure Reaction to Green
and vice versa (Q = 0). As a result of this adiabatic Diesel Yield

development the gas underwent temperature changed 4.4 Effect of Reaction Time to Green Diesel
both up and down (fluctuations). Yield
4.2 Effect of Temperature on Green Diesel

Yield Yield
(%w/w)
Yield
(%w/w)
Fig. 8. Effect of Reaction Time on Green Diesel Yield
Results at 4 hours of operating time are higher than

the operating time of 1 hour only. The longer the
Fig. 6. Effect of Temperature on Green Diesel Yield
reaction time, the cracking process also occurs more
optimally because the contact between reactants and
At the initial pressure condition of 30 bar and 1 hour
catalysts longer to produce more products that also cause
reaction time, the highest result is obtained at 400 oC
the green diesel increased.
operating temperature of 98.72% considering green
diesel C13-C22. This is because when the temperature is
4.5 Effect of Number of Stages of Reaction to
increased then the cracking process will occur more
easily and optimally. It is also caused by the addition of Green Diesel Yield
greater heat energy.
Yield
(%w/w)
4.3 Effect of Initial Pressure Reaction to Green
Diesel Yield
At 400 ° C and a reaction time of 1 hour, the green

diesel produced at a pressure of 60 bar is lower than the
pressure of 30 bar. It is predicted that at higher pressures
the incorporation of alkyl in short carbon chains results
in long-chain hydrocarbons C23 + which are not green
diesel but it was a small part of the wax [15].
Yield
(%w/w)
Fig. 9. Effect of Number of Stages of Reaction to Green

Diesel Yield
Results at 2 stages are higher than the reaction result

of only 1 stage. This is due to the cracking process at 2
stages occurs longer where every 1 stage is given 1 hour
so that if 2 stage then happened 2 hour reaction of
cracking. In addition, replacement with fresh hydrogen
makes the cracking process more optimal.
MATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/20181560303

RSCE 2017
2. Should be further studied related to raw

material pretreatment method, product
separation, catalyst used and product treatment
4.6 Effect of Reaction Temperature on before analyzed in order to obtain more optimal
Decreasing Oxygen Content result.
3. Need further study related to isomerization
reaction to get more comprehensive green
O Content diesel result.
(%wt)
4. Required product quality analysis such as
GCMS, calorific value and FTIR, cetane
number measure the success of research that has
been done.
A k l d t
Acknowledgments
Financial support from Center of Technology Energy
Resources and Chemical Industry - Agency for The
Assessment and Applycation of Technology for this
research are gratefully acknowledged.
Fig. 10. Effect of Reaction Temperature on Decreasing Reference

Oxygen Content [1] BPPT, Outlook Energi Indonesia 2015,
Jakarta, 2015
In a reaction that lasted 1 hour, waste cooking oil
which originally contained 14.25% oxygen can be [2] Dewajani H., Prosiding Seminar Nasional
reduced to 13.5 and 13.35% oxygen at reaction Energi Alternatif, Politeknik Negeri Malang,
temperature of 300 and 400oC respectively. Although (2008)
only less than 1% but with increasing reaction
[3] Dewajani H. dan Budiman A., Prosiding
temperature, it is possible to remove oxygen contained in
the fatty acid chain in waste cooking oil. Seminar Nasional Technoin UII, Yogyakarta,
(2012)
[4] He Z. Wang X., Catal Sustain Energy (1) 28-
5 Conclusion and Suggestion 52 (2012)
[5] Chew T.L., Bathia S. Bioresour, Technol (03)
5.1 Conclusion
009 (2008)
Based on the research that has been done, obtained some [6] Hilten R., Speir R., Kastner J,. and Das K.C.,
conclusions include: Bioresour Technol (102) 8288 – 8294 (1992)
1. The highest yield was obtained under operating
[7] Idem R.O., Katikaneni S.P.R., and Bakhshi
conditions with 2 stage reaction, where T1 =
300 oC, T2 = 400 oC, P1 = P2 = 30 bar, t1 = t2 = 1 N.N. ,Energy & Fuels, 10 (6) 1150 – 1162
hour that was equal to 98,93% (1996)
2. Factors affecting green diesel yields were [8] Ketaren S.D.G., Soares V.C.D., Ribeiro E.B.,
pressure, temperature, number of stages and
time. Carvalho D.A., Cardoso E.C.V., Rassi F.C.,
3. Oxygen levels decreased from 14.25% to Mundim K., Rubim J.C., and Suarez P.A.Z.,
13.35% at T = 400oC, P1 = 30 bar, t = 1 hour. Jounal Anal. Appl.Pyrolysis (71) 987 – 996
(2004)
5.2 Suggestions
[9] Maher K.D., and Bressler D.C., Bioresour
Suggestions that can be submitted for further Technol (98) 2351-2368 (2007)
research include: [10] Ma F., and Hanna M.A., Bioresour Technol
1. In order to improve the quality of green diesel (70) 1-15 (1999)
product produced, it is necessary to learn more
b h h d d i i i [11] Naveenji Arun Rajesh V Sharma Ajay K
about the hydrodeoxigenation operation [11] Naveenji Arun, Rajesh V. Sharma Ajay K.
condition made from used cooking oil, Dalai, Renewable and sustainable energy (48)
especially operating pressure and operating 240-255 (2015)
temperature need to be increased.
[12] Bendenzu S. Cid. R., Fierro J.L.G., and
Agudo L., Appl.Catal. A: General (197) 47-

CE 2017
60 (2000)
[13] Mohammad M., Kandaramath T., Yaakob Z.,
Chandra Y., Energy Rev (22) 121-132 (2013)
[14] Perego Carlo, Biomass to Advanced Biofuel,
(2015)
[15] Barton D.G., Soled S.L., and Iglesia E.,
Topics in Catalysis (6) 87 – 99 (1998)
(0) References (10)
king of Canola Oil: Reaction Products in the Presence and Absence of Steam
ERG FUEL
N. Bakhshi · S. Katikaneni · Raphael Idem
abstract
minar Nasional Energi Alternatif
Prosiding Seminar Nasional Energi Alternatif, Politeknik Negeri Malang, (2008)
A Dan Budiman
an Budiman A., Prosiding Seminar Nasional Technoin UII, Yogyakarta, (2012)
52
, Catal Sustain Energy (1) 2852 (2012)
Bathia
hia S. Bioresour, Technol (03) 009 (2008)
88-8294
peir · J Kastner · K C Das
r R., Kastner J,. and Das K.C., Bioresour Technol (102) 8288-8294 (1992)
7-996
· V C D Soares · E B Ribeiro · D A Carvalho · E C V Cardoso · F C Rassi · K Mundim · J C Rubim · P A Z Suarez
., Soares V.C.D., Ribeiro E.B., Carvalho D.A., Cardoso E.C.V., Rassi F.C., Mundim K., Rubim J.C., and Suarez P.A.Z., Jounal Anal.
(71) 987-996 (2004)
51-2368
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nd Bressler D.C., Bioresour Technol (98) 2351-2368 (2007)
nna M.A., Bioresour Technol (70) 1-15 (1999)
P CATAL · 87-99
L Soled
oled S.L., and Iglesia E., Topics in Catalysis (6) 87-99 (1998)
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11/14/2018 (PDF) Synthesis of Green Diesel From Waste Cooking Oil Through Hydrodeoxygenation Technology With NiMo/γ-Al 2 O 3 Catalysts

See all › See all › Join for free Login

Available) in MATEC Web of Conferences 156(6):03032 · January 2018 with 7 Reads

Heri Heriyanto Sri Djangkung Sumbogo Murti

Show more authors

the world's research

able via license: CC BY 4.0

a license: CC BY 4.0 Download full-text PDF

MATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/20181560303 Ad

Synthesis of Green Diesel From Waste Cooking Oil Through

1 Introduction Waste cooking oil is waste oil that can be

2 Literature Review Hydrogenation technology or Hydotreatment is

ATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/201815603032

GC-TCD GC-FID, GC-MS, CHNS(O)

WCO 200 g Autoclave reactor 500 ml

Fig. 1. Reaction pathway of hydrotreatment

Gas product analyze (GC-TCD)

Removing residue H 2 and

The procedure in this study was including 10 grams of

MATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/20181560303

4.1 Pressure and Temperature Profile

1-steel bottle; 2-valve; 3-pressure gauge; 4-reaktor;5-electrical

Fig. 3. Schematic and Equipments of Experimental

Table 1. Operating Conditions

amont T1( C) T2 pressure

ATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/201815603032

pressure drop was practically not allowing the

and vice versa (Q = 0). As a result of this adiabatic Diesel Yield

4.2 Effect of Temperature on Green Diesel

Fig. 8. Effect of Reaction Time on Green Diesel Yield

Results at 4 hours of operating time are higher than

At 400 ° C and a reaction time of 1 hour, the green

diesel but it was a small part of the wax [15].

Fig. 9. Effect of Number of Stages of Reaction to Green

Results at 2 stages are higher than the reaction result

MATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/20181560303

2. Should be further studied related to raw

Fig. 10. Effect of Reaction Temperature on Decreasing Reference

ATEC Web of Conferences 156, 03032 (2018) https://doi.org/10.1051/matecconf/201815603032

(0) References (10)

minar Nasional Energi Alternatif

Prosiding Seminar Nasional Energi Alternatif, Politeknik Negeri Malang, (2008)

, Catal Sustain Energy (1) 2852 (2012)

nna M.A., Bioresour Technol (70) 1-15 (1999)

Higher concentration yield of biohydrogen from optimal operation condition

CFD MODELING OF BROWN COAL LIQUEFACTION REACTOR

Article Full-text available

Heri Heriyanto · Denni Kartika Sari · Indar Kustiningsih

Sri Djangkung Sumbogo Murti · Muhammad Faizal · Lia Cundari · Novia

Performance of spent sulfide catalysts in hydrodesulfurization of straight run and nitrogen-removed...

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