FINAL YEAR PROJECT I: EXTENDED PROPOSAL

TITLE:
HYDROTHERMAL CARBONIZATION OF MALAYSIANS BIOMASS FOR
PRODUCTION OF COAL
PREPARED BY:
NORHANISAH BT MOHD ZAMRI
(17668)
SUPERVISOR:
DR TAZLI AZIZAN
Preliminary report submitted in partial fulfillment of the requirements for the Bachelor of
Engineering (Hons)
(Chemical Engineering)
JANUARY 2014

Universiti Teknologi PETRONAS

Bandar Seri Iskandar
31750 Tronoh
Perak Darul Ridzuan

ABSTRACT
Hydrothermal carbonization (HTC), a thermochemical pretreatment process, is a method used to
treat biomass under hot compressed water to produce hydrochar. Oil palm residues, which are
palm trunks, palm fronds and palm shell will be used as feedstock for producing carbonaceous
hydrochar .The main purposes of this study are to investigate the effect of reaction temperature,
residence time and the type of catalyst used on HTC process. In this study, a carbon rich
products, or hydrochar is synthesized by HTC of oil palm residues, at different operating
temperatures of 180 to 340C and different residence time between 30 to 150 minutes with the
presence of citric acid or ascorbic acid as a catalyst. The conversion of raw biomass to its
hydrochar occurred via dehydration and decarboxylation. To gain a detail insight on the raw
biomass and hydrochar produced, the materials will be characterized by CHNS, FTIR and SEM
analysis. Thermal gravimetric analysis (TGA) also will be conducted to study the combustion
behavior of the raw biomass and hydrochar produced.

Table of Contents
CHAPTER 1 ................................................................................................................................................ 2
INTRODUCTION .................................................................................................................................... 2
1.1 Background of Study ...................................................................................................................... 2
1.2 Problem Statement .......................................................................................................................... 3
1.3 Objective ......................................................................................................................................... 3
1.4 Scope of Study ................................................................................................................................ 3
1.5 Relevancy of the Project ................................................................................................................. 4
1.6 Feasibility of project ....................................................................................................................... 4
CHAPTER 2 ................................................................................................................................................ 5
LITERATURE REVIEW ......................................................................................................................... 5
2.1 Biomass ........................................................................................................................................... 5
2.2 Biomass Conversion Technology ................................................................................................... 6
2.3 Hydrothermal Carbonization........................................................................................................... 7
2.4 HTC of Oil Palm Wastes .............................................................................................................. 11
CHAPTER 3 .............................................................................................................................................. 12
METHODOLOGY ................................................................................................................................. 12
3.1 Project Flowchart .......................................................................................................................... 12
3.2 Project Gantt Chart........................................................................................................................ 13
3.3 Materials ....................................................................................................................................... 13
3.4 Experimental Method.................................................................................................................... 14
3.5 Characterization of biomass and hydrochar .................................................................................. 15
CHAPTER 4 .............................................................................................................................................. 17
CONCLUSION ....................................................................................................................................... 17
REFERENCES .......................................................................................................................................... 18

CHAPTER 1
INTRODUCTION
1.1 Background of Study
Nowadays, energy demand is increasing constantly as a result of population growth and evolving
industries. According to Euan (2015), 86% of energy consumed in 2014 represented by fossil
fuels. Due to depletion of fossil fuels and its effect on environment, the search for alternative
energy sources has gained great importance. Biomass is considered as one of the renewable
energy sources with the highest potential and some of the countries in Asia have established
targets to use fuels produced from biomass to replace fossil fuels (Ong, Mahlia, & Masjuki,
2011). Substitution of fossil fuels for energy for energy production with biomass will result in a
net reduction in greenhouse gas emissions and the replacement of a non-renewable energy
source. The biomass which is consisting mainly of agricultural and forestry waste can be
regarded as a renewable energy source with potential to supply the global energy demands.
Moreover, the use of biomass contributes to reduce the greenhouse effect. There are several
methods to convert biomass into value added product and one of it is hydrothermal carbonization
(HTC). HTC process is achieved in water at low temperature basically from 150C to 350C and
the pressure is held as high as to maintain water in liquid phase for several hours(Lin et al.,
2015). According to Lin et al., during the HTC treatment of the biomass, there are series of
significant decomposition such as dehydration, decarboxylation, condensation, polymerization
and aromatization before the solid hydrochar are produced. The aim of HTC is to produce a coal
like hydrochar which are more energy dense, easily friable and more hydrophobic than starting
material(Smith, Singh, & Ross, 2016). There are a lot of benefits from HTC process such as
increased the carbon efficiency, reduced pollutant emissions and also increase the heating value
of biomass. The purposes of this project are to investigate the effects of hydrothermal
carbonization temperature, residence time and also the presence of catalyst on the hydrochar
produced from the oil palm residues.

1.2 Problem Statement

The old method for converting biomass into energy is via direct combustion which produces
some pollutants and not environmentally friendly process. This conventional method also
produces only about 10% of energy from the biomass. The biomass, consisting mainly of
agricultural and forestry waste can be regarded as a renewable energy source with potential to
supply the global energy demands. Moreover, the use of biomass contributes to reduce the
greenhouse effect. Due to environmental concerns because of abundant waste from day to day, it
is an attractive option to create new technologies to convert biomass waste into value added
product. Malaysian biomass tends to be damp, and need extra drying for the conversion to a
better heating value. The fact that hydrothermal carbonization takes place in an aqueous reaction
medium means that wet biomass can be used, thus eliminating any energy-consuming pre-drying
steps before the HTC process.

1.3 Objective
The objectives of this project are:
i.

To characterize the HTC solid products

ii.

To determine the effect of process variable such as operating temperature, residence time
and catalyst use on hydrochar products

1.4 Scope of Study

This project is about the production of coal from hydrothermal carbonization process by using
Malaysians biomass. In addition, analysis on the characterizations of the coal from the HTC
process using the biomass also will be carried out. The yield of the coal will be determined by
varying the operating parameters which are:
i.

Operating temperature

ii.

Reaction Time

iii.

Presence of Catalyst

1.5 Relevancy of the Project

This project is important as energy demand is growing rapidly and fossil fuels cannot sustain
more in the near future due to depletion of the reserves and environmental impacts. Biomass is
one of the largest energy resources in the world and abundant in this country. Hence, this project,
which is to convert biomass to value added product via HTC process is very important as
alternative energy to replace fossil fuels.

1.6 Feasibility of project

This project is feasible as it deals with narrowed scope of experiment whereby only three
parameters are tested. It is within capability to be executed with helps and guidance from the
supervisor and the coordinator. It is positive that this project can be completed within the time
allocated with the acquiring of equipment and materials needed.

CHAPTER 2
LITERATURE REVIEW
2.1 Biomass
Biomass, which is mainly composed of carbon, hydrogen and oxygen, have solar energy
composed on its molecular bonds which made the biomass has high potential among the
renewable energy sources (Tekin, Karagz, & Bekta, 2014). According to Sue (2013), biomass
has always been a major source of energy for mankind, which contributed 10-15% of worldwide
energy demand. However, by 2050, nearly half of the global energy will be supplanted by
biomass as it is predicted that the world wide supply for oil reserves would be exhausted (Tekin
et al., 2014).
Biomass is commonly used as electrical or thermal energy, as fuel for transportation and as raw
materials for the production of chemicals; the applications for biomass continue to grow and are
increasing rapidly. Interest in biomass continues to grow and variety of studies has been
conducted on the use of biomass as a source for renewable energy and an alternative to fossil
fuels. There are several factors that play important roles in the selection of biomass as energy
source such as the calorific value, volatile matter content, ash content and also moisture content
(Sexena, Adhikari & Goyal, 2009).
Malaysia has tremendous biomass and wood waste resources available for immediate
exploitation. Annually, a minimum of 168 million tonnes of biomass waste is generated in
Malaysia and palm oil waste accounts for 94% of biomass feedstock while the remaining
contributors are agricultural and forestry by-products, such as wood residues (4%), rice (1%),
and sugarcane industry wastes (1%).
In 2000, Malaysia becomes worlds largest producer of palm oil by producing half of the world
palm oil production (10.8 million tonnes). Palm oil has made impressive growth in past four
decade and will be continue projected in period 2016 to 2020. Today, 4.49 million hectares of
land in Malaysia is under oil palm plantation compared to 3.31 million hectares in 1999. Table 1
shows the breakdown shows the breakdown of wastes from palm oil production in
2007(Abdullah & Sulaiman, 2013).

Wastes

Quantity (ktonnes)

Fronds

46,837

Empty fruit bunches

18,022

Palm pressed fibres (PPF)

11,059

Oil palm trunks (OPT)

10,827

Shell

4,506
Table 1: Oil Palm Wastes

2.2 Biomass Conversion Technology

There are two technologies that have been used to convert biomass into either biofuels with high
energy content or to other valuable chemicals (Tekin et al., 2014). As shown in the figure, the
first group is biochemical conversion technologies which use microorganisms and enzymes to
degrade the biomass compared to the second group which is thermochemical conversion
technologies that use heat to degrade the biomass.

Figure 1: Biomass Conversion Technologies

Decisive parameter that differentiates the combustion, gasification and pyrolysis process to one
another is the air supply to biomass feedstock (Comparing gasification, 2012). Pyrolysis is
anaerobic process, where the biomass is decompose with absolute absence of oxygen, while the
combustion takes place if oxygen is in excess. Meanwhile, if the oxygen supply is less than
combustion stoichiometric demands, the gasification will occurs.
Table below shows comparison of reaction conditions and typical product yields for
thermochemical conversion processes with char as a product.

Reaction conditions
Process

Pyrolysis:
slow
Pyrolysis:
intermediate
Pyrolysis:
fast
Gasification
HTC

Product distribution (weight%)

Temp. (C)

Vapor
residence
time

Char

Liquid

Gas

400

hour-week

35

30

35

500

10s-20s

20

50

30

500

1s

12

75

13

800

10-20s

10

85

180-250

(1- 12 h
processing
time)

50-80

5-20
(dissolved in
process
water, TOC)

2-5

Reference

Libra et al.
(2011)

Table 2: Comparison between thermochemical conversion

2.3 Hydrothermal Carbonization
2.3.1 History of Hydrothermal Carbonization
According to Ramke et al (2009), hydrothermal carbonization process was first described as
conversion of cellulose into coal-like materials by Fridrich Bergius in 1913. During that time,
many researchers had already attempted to convert biomass, that is, wood, which contains, apart
from cellulose, lignin, into coal by heating. However, the cellulose was decomposed. Bergius
stated that to prevent super-heating and decomposition of cellulose, the biomass must be in
contact with liquid water, which at mild temperature in high pressure vessel.
The discovery by Bergius then later followed by other studies such as Berl and Schmidt which
varied the type of biomass sample at different operating temperature range between 150C to
300C (Titirici, Funke, & Kruse, 2015). In 1960, .Schuhmacher et al. then analyzed the influence
of pH on the outcome of the HTC reaction and found serious differences in the decomposition
schemes, as identified by the C/H/O composition.Nowadays, many research groups try to
discover HTC by using different type of biomass and operating variables to get the highest yield
of coal. Besides the academic interest, several private companies have started large-scale HTC
production because the resulting char has coal-like properties and is expected to exhibit
favorable behavior with respect to combustion, gasification, and other thermal conversion
processes for decentralized applications.
7

2.3.2 The HTC Process

Hydrothermal carbonization (HTC) process, which also known as hydrothermal pretreatment is a
thermo-chemical conversion technique to convert wet biomass and waste streams into a high fuel
value solid product(Reza et al., 2014) . According to Pari, Darmawan, and Prihandoko (2014),
HTC is usually performed at temperature ranging from 180C to 280C over a period ranging
from a few hours to a day, employing the pressure greater than one atmosphere. In addition,
HTC process is capable of taking the wet biomass which has more than 30% water and this
factor made HTC process is suitable option to convert waste and biomass into solid carbon
instead of carbon gases through an exothermic process, producing carbon-rich materials. By
using cellulose monomer as an example, the equation for the reaction is:

There are several reaction mechanisms that occur to biomass during the HTC process such as
hydrolysis, dehydration, decarboxylation, polymerization and aromatization. Figure below show
the reaction pathways for degradation of biomass.

Figure 2: Reaction Pathway of Biomass

In HTC process, biomass is converted into a solid product called bio-char, a liquid product called
bio-oil and a gas product(Tekin et al., 2014). Biomass can be converted into a the target products
by manipulating the process variable such as reaction time, reaction temperature and also the
catalyst used, Figure 3 shows the products from the hydrothermal conversion of biomass.

Figure 3 : Products from HTC process

2.3.3 Parameters Governing HTC
Jain, Balasubramanian, and Srinivasan (2016) discussed about four parameters affecting the
production of hydrochar in HTC process which are temperature, residence time, catalyst use and
also substrate concentration.
i.

Temperature
Temperature will determine the fate of degradation reactions in HTC process. High
temperature leads to extensive dehydration and an increase in the degree of condensation
of the hydrochar.

ii.

Residence time
Reaction time plays an important role in the extent of reaction and the distribution of
different types of products and their quality. Longer residence time will cause excessive
polymerization and leads to condensed products.

iii.

Use of Catalyst
Catalyst will enhance the reaction rate reduces the energy of activation for the hydrolysis
of biomass.

iv.

Substrate Concentration
Low concentration of reactants will minimize cross reaction of the involved species and a
higher reactant to water ratio will lead polymerization at shorter residence time.

Table 1 shows the example previous study of HTC on different types of biomass by
manipulating their operating parameters.
Biomass

Operating Parameters
Temperature Residence Time
Catalyst
(C)
(Min)

References
Guo, Dong, Wu,
Shi, and Zhu
(2015)
Erdogan et al.
(2015)

Corn stalk

180 - 290

480

N/A

Orange pomace

175-260

30-120

N/A

Brewers spent
grain

200-240

840

Citric acid

Poerschmann et al.
(2014)

Wheat straw,
poplar wood &
olive residues

180-230

480

Citric acid

Wiedner et al.
(2013)

Paper sludge

180-300

30

N/A

Lin et al. (2015)

Water hyacinth

240

30-1440

N/A

Y. Gao et al.
(2013)

Eucalyptus bark

220-300

120-600

N/A

P. Gao et al. (2016)

Rice husk

200-300

120-960

N/A

Kalderis et al.
(2001)

Bamboo

180-260

10

N/A

Yang et al. (2016)

Fresh forest
residue

175-225

10-60

N/A

Bach, Tran &

Skreiberg (2016)

Primary sewage
sludge

140-200

30-240

N/A

Rapeseed husk

150-200

5-30

N/A

Cassava and
tapioca
flour

250

480

N/A

Pari et al. (2014)

Seaweed

200&250

60

N/A

(Smith and Ross

(2016))

Danso-Boateng et
al. (2013)
Elaigwu &
Greenway(2016)

Table 3: Previous research paper on HTC of biomass

10

2.4 HTC of Oil Palm Wastes

An oil palm industry is the largest biomass resources potential in Malaysia. The biomass
produced from the industry include oil palm trunks (OPT), oil palm fronds (OPF), empty fruit
bunches (EFB) and palm pressed fibres (PPF), palm shells and palm oil mill effluent
palm(POME) (Abdullah & Sulaim, 2013). Numbers of research have been done to convert the
biomass product form the oil palm industry to hydrochar or coal-liked materials via HTC
process.

Biomass

Description

References

EFB

Studied and evaluated the chemical, structural and

combustion properties of the hydrochar from EFB for its
potential use for energy generation through cocombustion with coal. The study also is to investigate
the feasibility of converting EFB to value added solid
products which is the hydrochar.

Parshetti, Kent
Hoekman, and
Balasubramanian
(2013)

EFB

The study was to identify the effect of reaction

temperature and reaction time for hydrothermal
treatment of EFB.

Kongpanya (2014)

Palm Shell

Studied the influence of reaction time and reaction

temperature of the HTC process of palm shell

Nizamuddin et al.
(2015)

Palm Shell

Studied about chemical, dielectric and structural

characterization of hydrochar produced from HTC

Nizamuddin et al.
(2016)

Palm leaves

Studied the characterization of hydrochar from HTC

process of palm leaves.

Youssef et al.(2015)

Table 4: HTC from oil palm residues

However, to date, there are no research done on the topic about HTC of palm fronds and palm
trunks. Thus, the main goals of this research are to study the characterization of hydrochar
produced from palm fronds, palm trunks and palm shell and the yield percentage of the coal by
varying the reaction temperature, reaction time and catalysts during the HTC process.

11

CHAPTER 3
METHODOLOGY
3.1 Project Flowchart

Conclusion
-Conclude the experiment and
prepare report for the project.
Data Collection
-Conduct the experiment and collect the
data. Analyze the data and come out with
results and discussion.
Experiment
- Design an experiment to study the
relationship between parameters
-Prepare chemical and equipment needed for
experiment
Literature review
-Preliminary research on existing studies on the topic
from journals and books
-Understnding HTC concept

Key Milestones

Submission of extended proposal defence (Week 7)

Oral proposal defence presentation (Week 8)
Submission of interim draft report (Week 13)
Submission of final interim report (Week 14)

12

3.2 Project Gantt Chart

No

Detail Work

1 2 3 4

Selection of project topic

Preliminary research work. Finding

research paper and journal related to
HTC.

Selection of biomass suitable for HTC.

Selection of operating parameter to be

tested.

Design the experiment and identify

equipment involved.

Submission of extended proposal defence

Proposal defence

10 11 12 13 14

Project work continue

8

Characterization of biomass selected

Submission of Interim Draft Report

10

Submission of Draft Report

Process

Milestone

3.3 Materials
The oil palm residues which are the palm fronds, palm trunks and palm shells will be used as raw
materials in this research. The oil palm residues will be collected from local supplier. Then the
biomass will be grinded into small pieces ranging from 1 to 5 mm. The biomass then will be
stored in sealed container until use.

13

3.4 Experimental Method

The hydrothermal carbonization of all biomass will be conducted in high pressure batch
reactor. Prior to the test, pre-weigh approximately 10g of the biomass and dispersed in 100 ml of
deionized water. For the first run of each biomass, the HTC will be conducted 220C and 60
minutes without the presence of catalyst. At the end of each experiment, the hydrochar will be
filtered, dried and weight to estimate the yield.
The biomass that gives the highest yield then will be selected for further research. The
HTC then will be conducted at temperature range between 180C to 340C and residence time
between 30 minutes to 150 minutes with the presence of citric acid or ascorbic acid as catalyst.

Run

Biomass

Palm trunk

Palm frond

Palm shell

Catalyst

Operating
Time (min)

Operating
Temperature
(C)

N/A

220

60

220

60

Citric acid

Ascorbic acid

180

220

260

9
10
11

*Plam trunk/
palm frond/
palm shell

60

300
*Citric acid/
Ascorbic acid

340
30

12

60

13

220

14

90
120

15
*Decided based on highest yield of hydrochar from Run 1-5

150

Table 5: HTC Operating Parameters

14

3.5 Characterization of biomass and hydrochar

The yield of hydrochar of each biomass will be calculated with the following formula
(Lin et al., 2015).
Hydrochar yield = Mass of hydrochar / Mass of feedstock

(1)

The elemental contents of biomass and hydrochar were determined by vario Micro cube
elemental analyzer (Elementar, Germany). The samples will be weighed around 1.5mg to 2.0 mg
in aluminium container before entering the analyzer. The equipment will evaluate the
composition of carbon, hydrogen, nitrogen and sulfur in the samples. The composition of the
oxygen will be calculated by difference method. According to Friedl, Padouvas, Rotter, and
Varmuza (2005), the value of HHV can be predicted from the elemental analysis by using the
following equation:
HHV(kJ/kg) = 3.55C2 232C -2230H + 51.2CH + 131N + 20600

(2)

where C, H and N are carbon, hydrogen and nitrogen contents of the samples. The energy yield
will be calculated by equation 3 expressed as follows:
Energy yield = (HHVhydrochar / HHVbiomass) X hydrochar mass yield

(3)

Figure 4: Elemental Analyzer

The combustion behaviours will be evaluated by a STA 600 Simultaneous Thermal
Analyzer (Perkin Elmer, USA). The sample will be weighed approximately 5mg to 10mg and fi
into small pan in TGA. A set of methodology will be programmed and the methods are:
i)

Hold for 1 minute at 50C

ii)

Heat from 50C to 800C at 20.00C/min with nitrogen flow rate of 20ml/min

15

From TGA profile, the moisture content, volatile matter, fixed carbon and ash of the samples will
be determined.

Figure 5: Perkin Elmer TGA

The functional groups of biomass and hydrochar will be investigated by Frontier FTIR
Spectrometer (Perkin Elmer) with a resolution 4cm-1, using pure KBr as the background.

Figure 6: FTIR Spectrometer

Scanning electron microscopy (SEM) which used electrons for imaging will be used to
study the surface morphology of feedstock and hydrochar. The samples will be placed onto
adhesive carbon tape on an aluminium stub, loaded in vacuum chamber with accelerating voltage
15 kV.

16

CHAPTER 4
CONCLUSION
As conclusion, this project is important as it deals with biomass which is one of alternative
energy that could be used to reduce the dependence on fossil fuels. Hydrothermal carbonization
(HTC) is believed to be one of effective ways to convert biomass into value added product which
is coal. Compared to other technique, the fact that hydrothermal carbonization takes place in an
aqueous reaction medium means that wet biomass can be used, thus eliminating any energyconsuming pre-drying steps before the HTC process. HTC process is still developing nowadays,
hence, further study and understanding of the hydrochar produced by HTC process is very
necessary.

17

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