Chapter 1 Introduction

______________________________________________________________________________

In a world being poisoned by its own near-sighted wisdom, God has provided man with a
microscopic black hole big enough to swallow much of what ails us and that microscopic material
is “activated charcoal”.

Since 3750 B.C., mankind is utilizing activated charcoal for the edification of its civilization. The
Egyptians and Sumerians produced charcoal for the reduction of copper, zinc and tin ores in the
manufacture of bronze. Without realizing it, the Egyptians began to capitalize on charcoal's anti-
bacterial, anti-fungal properties. Hippocrates (circa 400 B.C.), and then Pliny (50 A.D.), recorded
that people used to adsorb the unpleasant odors from putrefying wounds and from within the
intestinal tract. In 2nd century A.D. Claudius Galen was the most famous doctor of the Roman
Empire, produced hundreds medical treaties, many of them referring to the use of charcoals of
both vegetable and animal origin, for the treatment of a wide range of diseases.

In addition, even today, activated carbon is rated as ‘safe and effective’, by the American Food
and Drug Administration (FDA) for acute toxic poisoning and it, cuts down on the amount of gas
produced by gas-producing foods, and adsorbs the bacteria that form the gas. Crafted by the
Creator's hands, its history resurrected from the burial sands of ancient Egypt, charcoal is one of
the single greatest benefactors to the human race.

This carbonaceous highly porous, absorptive medium has a complex structure primarily of carbon
atoms. The networks of pores in activated carbons are channels created within a rigid skeleton of
disordered layers of carbon atoms, linked together by chemical bonds, stacked unevenly, creating
a highly porous structure of nooks, crannies, cracks and crevices between the carbon layers. The
intrinsic pore network in the lattice structure of activated carbons allows the removal of impurities
from gaseous and liquid media through a mechanism referred to as adsorption. This is the key to
the performance of activated carbon.

Charcoal, this savior material can be obtained easily from biodegradable waste (or bio-waste), this
has been prompted by attempts to move away from landfill as the automatic choice for dealing

1
with our rubbish, and to reduce emissions of greenhouse gases by avoiding burning fossil fuels.
For producing charcoal, activated charcoal, compost and fertilizers, bio-wastes can play an
important function. The Charcoal Powder itself has numerous of pores, the Charcoal Powder pores
can effectively to suck air and all kinds of floating material, to sulfide, hydride, methanol, benzene,
phenol and other harmful chemical substances to absorption, decomposition odor and
deodorization. The technology in making Jute Stick Charcoal Powder is available locally and
skilled manpower is also available in our country. In this experiment, dry leaves, rice-straw and
sugarcane bagasse have also been used to produce a high quality charcoal powder with a surface
area of around 200 m2 /g.

Therefore, we took this thesis work to study the processing of our bio waste. If we can develop
affordable activated carbon producing technology, we can earn a huge revenue by exporting.

2
Chapter 2 Literature Review
______________________________________________________________________________

Charcoal, a light, solid, non-agglomerating organic matter obtained from animal and plant origin,
is mainly composed of carbon and the remaining ashes. It results from decomposition by heat in
the absence of air at temperature above 600℃. The limited access of reliable and affordable energy
sources makes charcoal a standout material of the modern urbanization and civilization. 2.7 billion
people over the entire world are facing energy crisis today and almost 40% of them in the global
population and specifically 95% of population in the African and Asian sub-continent are highly
entrusted to biomass derived charcoal and activated carbon [1]. Biomass, agricultural byproducts
have proved to be promising raw materials for the production of charcoal carbon because of low-
prices, renewability, cost- effectiveness, eco-friendliness.

2.1 Waste Scenario of Bangladesh

Bio-waste is a form of bio mass, this waste material is capable of decomposing under aerobic and

anaerobic conditions. The environment is imperative to reduce the amount of resources we have
consumed and the management of bio-wastes touches a number of policy fields, climate change,
energy, bio-diversity, habitat protection, agricultural and soil protection are related with bio-waste
management. Lignocellulosic biomass is considered the feedstock of carbon related material.
Sugarcane bagasse, the fibrous matter that is remained after sugarcane stalks are crushed to extract
juice; the rice straw has high hemicellulose and cellulose content that is suitable for conversion
into ash content, on the other hand, dry leaves and jute sticks are part of trees.

Charcoal and Activated Caron from these materials are of higher value and Bangladesh is now
producing Jute Stick Charcoal industrially. We have two factories in Pabna, Jamalpur, Rajshahi,
Narayanganj, Faridpur and total 25 mills [39] among different parts of our country, which are set
up to produce different dust powder. And producers are eyeing to fetch an estimated taka 2.5
thousand crore by jute stick ash each year. They are not able to produce activated carbon because

3
of not having enough knowledge and technical support. They have to export the charcoal dust to
abroad for further processing. Some industry also try to produce activated carbon from coconut
shell. There are many opportunities for activated carbon in our country. We have huge demand for
activated carbon in effluent treatment plant, which has to be imported from abroad in high price.

2.2 Form of Activated Carbon

Activated carbon is basically amorphous [3-5], tasteless [6], non-graphite [7], microcrystalline [8,
9], form of carbon and a black solid substance which resembles powder or granular charcoal [10,
11]. A non-graphite activated carbon means it cannot be converted into crystalline graphite even
at a temperature of above 3000℃ [12]. According to Cuhadaroglu and Uygun [2], activated carbon
cannot be characterized by any distinctive chemical formula. Activated carbon has been noticed
to be associated with oxygen, sulfur, hydrogen, nitrogen, halogen and other heteroatoms [13-15].
Oxygen is found to be predominant in the form of functional groups such as carbonyl, carboxyl,
phenols, lactone and others [16,17].

Figure 2.1: Activated Carbon

4
2.3 Bio waste to Activated Carbon
Bio-wastes are commonly known as biomass briquettes, green wastes are compressed compound
s various organic materials. Generally the materials are ground nut- shell, municipal solid wastes,
agricultural wastes. This study on activated carbon has been done with rice straw, sugarcane
bagasse, jute stick and dry leaves. Compared to fossil fuels and other type of energy sources, they
produce low net total greenhouse gas emissions because the materials used are already a part of
carbon cycle. [18]

2.4 Utilization of Activated Carbon

Activated charcoal has the amazing ability for trapping toxins and chemicals in its millions of tiny
pores. However, it is not used when petroleum, alcohol, lye, acids and other corrosive poisons are
invested. It does not absorb toxins while it works through the chemical process of adsorption. In
the body, adsorption is the reaction of elements, including nutrients, chemicals, toxins, soaked up
and assimilated into blood stream. The porous surface of activated charcoal has a negative electric
charge that causes positive charged toxins and gas to bond with it [19]. The main uses for activated
carbon are-

2.4.1 Whitens Teeth

Activated charcoal helps whiten teeth while promoting good oral health by changing the pH
balance in the mouth, helping prevent cavities, bad breath and gum disease. It absorb plaque and
microscopic tidbits that stains teeth.

2.4.2 Alleviates Gas and Bloating

Activated charcoal is a good option to prevent uncomfortable gas and bloating, by binding the gas
causing byproducts in the foods that causes discomfort. A study in the American Gastroenterology

5
found that activated charcoal also prevents intestinal gas following a typical gas producing meal.
500 milligrams of dose before one hour of gas producing meal will be an effective way to solve
bloating.

2.4.3 Alcohol Poisoning and Hangover Prevention

Alcohol is rarely consumed in its pure form; mixers that include artificial sweeteners and
chemicals are common. Activated charcoal removes these toxins. When activated charcoal is taken
for the same time as alcohol, studies showed that it can reduce alcohol in blood concentration.

2.4.4 Mold Cleansing

Toxic mold causes depression, kidney and liver failure, decreased brain function, heart diseases,
eye irritation, headaches, vomiting, impaired immune system function, and severe respiratory
distress. Activated carbon is a good option for mold cleansing.

2.4.5 Water Filtration

Activated charcoal traps water, including solvents, pesticides, industrial wastes and other
chemicals and that is why it is used largely in the world.

2.4.6 Digestive Cleanse

It promotes a healthy digestive tract by removing toxins that cause allergic reactions, oxidative
damage and poor immune system function. By removing the toxins from body system, it reduce
joint pain, increase energy and increase mental function.

6
2.5 Activated Carbon Preparation
There are two different processes for activated carbon; chemical and physical treatment [20, 21].
Both treatments are responsible in varying the shape and size. For the experiment, physical
preparation has been done which is described below-

2.5.1 Physical Treatment

Thermal or physical treatment is a two-step process, carbonization and activation [22, 23,24]. It is
mainly dry oxidation which involves the reaction between samples and gaseous stream of CO2 and
air. It is done at temperature reaching above 700℃.Carbonization is referred to the process in
which high carbon content solid residues are formed from organic material usually by pyrolysis in
an inert atmosphere [25]. Moisture and volatiles are driven off leaving this solid residue (char),
liquids (condensable vapor), and permanent gases during this thermal decomposition process. This
experiment is done by slow pyrolysis as a part of carbonization process which maximizes the char
yield and is characterized by slow heating rate, long solid and gas residence time and relatively
low temperature in the absence of oxygen [26]. Conversion characteristics are grouped into
thermochemical (ash and volatile contents, reactivity of volatile products); intra-particle rate
(particle thermal properties, moisture content) – these experiments are done for bio-wastes sample
and charcoal product. Particle size, shape and physical properties (ash content, density, moisture
content) – these are done in the analytical laboratory.

2.5.2 Chemical and Physio-chemical Tests

2.5.2.1 Moisture Content

Water content or moisture content is the quantity of water contained in a material. Generally water
content is difficult to measure because of the complex intermolecular bonding properties within
substance matrix. For measurable water content to be justifiably determined, and proper levels

7
sustainable in a processing environment in the testing and evaluation process of moisture analysis.
Understanding and maintaining the correct moisture content of a material is essential for
manufacturing processors and testing laboratories [27]. The moisture content in Mc percentage is
B−F
given by- Mc= 100
B−G
Where,
B= mass in the gram with lid plus original sample
F= mass in the gram with lid plus original sample
G= mass of container with lid in gram

2.5.2.2 Volatile Organic Content

It is an important test of determining volatile organic matter in activated carbon and coal type of
material. A furnace heated by electricity, where the sample is heated at 900℃ for 7 minutes. The
percentage of volatile matter is calculated from the loss of mass from the sample. [27]
The volatile matter from the material on dry basis,
100(B−F)−Mc(B−G)
Vd = 100
(B−G)(100−Mc)

Where,
B= mass in the gram of crucible, lid and sample before heating
F = mass in the gram of crucible, lid and contents after heating
G = mass in the gram of the empty crucible and lid
Mc= moisture as a percentage by mass.

2.5.2.3 Ash Content

This was done at 700℃ for 20 minutes in a muffle furnace which has air circulation and has
temperature regulation. After one hour of ignition in the muffle furnace the crucible is placed in

8
the desiccator. Depending on the type of activated carbon, ashing will take 3 hours to 16 hours.
Ashing is considered achieved when the weight has been constant. [27]
F−G
Mc= 100
B−G
Where,
G= mass of empty crucible in gram
B= mass of crucible plus dried sample in gram
F= mass of crucible plus ashed sample in gram

2.5.2.4 Fixed Carbon Analysis

Fixed carbon is the solid residue combustible residue that remains after a coal particle is heated
and the volatile matter is expelled. The fixed-carbon content of a coal can be determined by
subtracting the percentage of moisture, volatile matter and ash from a sample. Since gas-solid
combustion reaction is slower than gas-gas combustion reaction, a higher fixed carbon percentage
indicates that the coal will require a longer combustion time.

2.5.3 Effect of Temperature

Heating rate, carbonization rate and nitrogen flow time- largely depends on the temperature of the
carbonization process. The increase in temperature would increase fixed carbon and ash content
percentage and decrease the volatile organic matter percentage. Asadullah et al. [28] studied the
effect of temperature on the yield and the properties of activated carbon prepared from jute stick
char from the physical activation. They found the temperature of 750℃ gave the highest Bet
surface area. Tsai et al. [29] they found also that higher temperature was favorable for activated
carbon in terms of surface area, total pore volume, true density and porosity, but with lower yield.

9
2.5.4 BET Surface Area and Pore Sizes of Activated Carbon

The pore size of the activated carbon has been categorized into three types; micropore (poresizeo2
nm), mesopore (2nmoporesizeo50 nm),and macropore (poresize450 nm) [30,31]. By BET
(Brunauer, Emmett and Teller) the specific surface area of a sample is measured – including the
pore size distribution. This information is used to predict the dissolution rate, as this rate is
proportional to the specific surface area. Thus, the surface area can be used to predict
bioavailability. Further it is useful in evaluation of product performance and manufacturing
consistency. The specific surface determined by BET relates to the total surface area (reactive
surface) as all porous structures adsorb the small gas molecules. The surface area determined by
BET is thus normally larger than the surface area determined by air permeability. In this
experiment, BET surface area has been determined for the carbon obtained from jute stick, rice
straw, sugarcane bagasse and dry leaves. Li et al.[32] stated that activated carbon with different
pore characteristics can also be produced even from the same starting material. This can be
achieved by varying the operating variables and activation agents. It shows that, starting material
and the condition of carbonization and activation are the most important factors the affect the types
of porosity of the resulting activated carbon[33,34].

10
Chapter 3 Experimental Methods
______________________________________________________________________________

Description of the experimental work of this thesis work is discussed here. This thesis work was
totally dependent on laboratory work. All the laboratory works which were done to complete the
thesis work are explained in this section. The apparatus which were used during thesis session are
also enlisted here. The data recording process and procedure to determine the proximate analysis
of the sample and activated carbon are also included in this section. Moisture content, Ash content
and Volatile matter content of the sample and product were determined through experimental work
and Fixed carbon was calculated. Again, activation procedure is also discussed here.

3.1 Sample Collection

Bio-waste Jute stick has been collected from Madaripur district of Basngladesh while the dry
leaves were collected from the lawn of Department of Chemical Engineering, BUET. On the other
hand, Sugarcane Bagasse was bought from Joypurhut district of Bangladesh and Rice straw were
collected from rural area of Chandpur.

3.2 Sample Preparation

The bio wastage sample needed to be prepared for proximate analysis and activation. Also all the
sample needed to be in same size. From the collected amount of sample, each type of sample in a
small amount is taken and had been cut down to approximately 2 inch by using kitchen scissors.
The four types of processed samples were then kept in Aluminium foil and dried in the oven for
clear the moisture.

11
 Rice Straw Bagasse

Jute Stick Dry Leaves

Figure 3.1 Bio Waste Sample after Cutting

Oven dried materials were then grinded in a coffee grinder to make the small powder like material.
After being grinded in a grinder, the powder-sample were undergone through sieving. ASTM 35
Sieve was used for sieving. So the powder size was approximately 0.5 mm. The powder like
samples had been stored in plastic sample container and the mouth of those container were tightly
closed so that they were not further attacked by moisture from surrounding environment.

12
 Rice Straw Bagasse

Jute Stick Dry Leaves

Figure 3.2 Bio Waste Sample after Grinding and Sieving

3.3 Proximate Analysis

Proximate analysis of all the raw materials was done. For our bio-waste sample ASTM D1762 was
followed for proximate analysis. Equipment used for this work included an electric muffle furnace,
analytical balance, drier and silica glass crucible.

13
3.3.1 Moisture Content Determination
Moisture content of Jute Stick, Rice Straw, Bagasse and Dry Leaves was measured by finding
the weight differences of the samples before and after keeping them in a dryer at 105°C for 30
minutes in Petri dishes in single layer.

3.3.2 Ash Content Determination

Each type of sample was taken in a porcelain crucible and heated in an electric muffle furnace.
Heating in a furnace was done for ~4 hours to get Ash form of substances. From the difference of
the weight of each bio-waste sample and bio-waste ash, the ash% of samples were measured.
The four types of bio-waste have different combustion temperature and for ensuring the full
conversion into ash of these materials. Rice straw ash, dry leaves ash and bagasse ash were
produced similarly by combustion at 600°C and came out along with some black unburnt particles,
whereas the jute stick has a bit higher combustion temperature. So, it was further heated at higher
temperature 750°C and kept it constant for 20 minutes to ensure the complete conversion of ash.
Ash% of bio-waste samples were calculated similarly.

3.3.3 Volatile Matter Content Determination

For measurement of %volatile matter (in wet basis), granular samples were taken in four
identical (but somewhat different in weight) fused silica glass crucibles and burnt at 900°C for
7 minutes and then the weight difference before and after burning was measured. Volatile %
in dry basis was calculated for each sample by subtracting the % moisture from volatile% in
dry basis.

3.3.4 Fixed Carbon Determination

Fixed carbon % was calculated by subtracting ash%, volatile% and moisture content % from
the total weight of the samples.

14
3.4 Experimental Procedures for Activation
Producing activated carbon was the most important part of this thesis work. Different temperature
and environment were used. Activation procedure was done in the Mass Laboratory and Fuel
Laboratory of Department of Chemical Engineering, BUET. Sample powder of four type of bio-
wastes were firstly dried to remove the moisture. Then empty volatile matter crucibles were
weighted with lead. Sample were taken fully loaded in the volatile matter crucible as oxygen free
environment was needed. Weight was taken and by subtracting from the previous weight, weight
of the sample used was determined. Then all the volatile matter crucibles with lead were placed in
the furnace. For first two batch N2 gas flow was used to create inert atmosphere but due to leak in
furnace complete inert condition could not be achieved.

Activated Carbon from Rice Straw Activated Carbon from Bagasse

Activated Carbon from Jute Stick Activated Carbon from Bagasse

Figure 3.3 Activated Carbon from Different Bio Waste Sample

15
Temperature for first two batch was 7000 C. For third, fourth and fifth batch, temperature was set
at 7000 C. For last batch temperature was 6000 C. Initial temperature for every batch was 300 C.
Temperature was increased at the rate of 100 C per minute. After reaching the set temperature,
volatile matter crucibles were kept there for different time. For first four batch set time was 15
minutes and for last two batch set time was 10 minutes. After cooling, ash particle was removed
carefully. Then the weight of the activated carbon was taken and yield percentages was calculated.
The product was kept in the aluminum foil for further analysis.

3.5 Experimental Procedures for BET Surface Analysis

This characterization method explicates the determination of the overall specific external and
internal surface area of disperse or porous solids by measuring the amount of physically
adsorbed gas according to the BET (Brunauer-Emmett-Teller) method.

The analysis was done by following ASTM S3663-03. At first, Liquid Nitrogen was taken and
was filled in cold trap dewar, then the cold trap dewar was mounted. Gas cylinder valves were
open to pass the gas mixer and sample was taken in the sample holder and weight was recorded.
After that the sample is absorbed and later desorbed by nitrogen of different concentration by using
an adsorption instrument “Micromeritics Flowsorb-II”. This was done at liquid nitrogen
temperature (77k). An adsorption isotherm was developed as the result of this process. The total
surface area by the BET theory and the pore volume for each sample were analyzed and reported.

16
Chapter 4 Result and Discussions
______________________________________________________________________________

Our thesis work had mostly laboratory work. It has mainly three parts. Analysis of the bio waste,
Activation of the bio waste and analysis of the product. All the readings from those parts are
presented separately. Those are shown in tabular form along with graphical representation.

4.1 Proximate Analysis

Proximate analysis was done for both the bio waste and the product. Moisture content, volatile
matter content and ash content were determined in the laboratory and fixed carbon was calculated.
Mainly fixed carbon is one of the most important parameter for the quality of the activated carbon.

4.1.1 Proximate Analysis of Bio waste

The proximate analyses of all the sample are shown in Table 4.1. As shown in the table moisture
content was low in all sample. Volatile matter content was the highest in every sample but dry
leaves have the least value (58.09 %) among them. Ash content was low in all sample except dry
leaves (28.71 %). Bagasse and Jute Stick have almost same value for fixed carbon (6.2549 % and
6.46 % respectively). Rice straw has higher value of fixed carbon (19.181 %) than others do.

Table 4.1 Proximate Analysis of Bio Waste

Name of the Moisture Volatile Matter Ash Content Fixed Carbon

Sample Content (%) Content (%) (%) (%)

Rice Straw 2.089 75.07 3.66 19.181

Bagasse 7.0151 84.28 2.45 6.2549

Jute Stick 5.13 79.12 9.29 6.46

Dry Leaves 5.01 58.09 28.71 8.19

17
4.1.2 Proximate Analysis of Activated Carbon

The proximate analyses of all the activated carbon are shown in Table 4.2. Activated
Carbon from Bagasse and Dry Leaves have almost same value of moisture content
(3.3 % and 3.42 % respectively). Moisture content of Activated Carbon from Rice
straw is higher than other sample even higher than all precursor. Activated Carbon
from Bagasse and Jute stick have almost similar volatile matter content (78.03 %
and 74.1 % respectively). In addition, Activated Carbon from Dry leaves has the
lowest value of volatile matter content (30.94 %). As for Ash Content, Activated
Carbon from Dry Leaves has the highest value (53.42 %). Fixed Carbon is very low
for Activated Carbon from Rice Straw (4.82 %) though its precursor has the highest
among other bio waste sample. Activated Carbon from Dry Lea has the highest value
of Fixed Carbon (12.22 %)

Table 4.2 Proximate Analysis of Activated Carbon

Name of the Moisture Volatile Matter Ash Content Fixed Carbon

Sample Content (%) Content (%) (%) (%)

Rice Straw 10.65 69.52 15.01 4.82

Bagasse 3.3 78.03 8.31 10.36

Jute Stick 8.28 74.1 8.77 8.85

Dry Leaves 3.42 30.94 53.42 12.22

18
4.2 Activation of the Bio Waste
Activation was done in several times. Total six batch was run for activation. For first two batch
Nitrogen flow was used to create inert condition. But as furnace and total system had some
problem, all the sample were turned into ash. Then VOC crucible was used. Then activation could
be achieved. Temperature and time at the peak temperature were varied. We had an intention to
check the relation between activation and temperature. But limited time and lab facility and also
lengthy sample preparation did not allow us to fulfill our intention. Data from last four batch are
tabulated here. And the activated carbon form the sixth batch were used for further analysis.

Table 4.3 Data from Activated Carbon from Bio Waste

3rd Batch, Dry Sample, Highest Temperature: 7000c &

time at highest temperature: 15 minutes

Sample Name Sample Used, gram Yield

Rice Straw 0.7636 12.06

Bagasse 0.5788 3.5

Jute Stick 0.5095 2.1

Dry Leaves 1.3154 39.19

4th Batch, Dry Sample, Highest Temperature: 7000c &

time at highest temperature: 15 minutes

Sample Name Sample Used, gram Yield

Rice Straw 1.0028 13.31

Bagasse 0.8987 10.01

Jute Stick 0.8675 6.29

Dry Leaves 1.33 37.74

19
 5th Batch, Dry Sample, Highest Temperature: 7000c &
time at highest temperature: 10 minutes

Sample Name Sample Used, gram Yield

Rice Straw 2.003 16.88

Bagasse 1.1329 9.35

Jute Stick 0.9454 2.81

Dry Leaves 4.3295 39.59

6th Batch, Dry Sample, Highest Temperature: 6000c &

time at highest temperature: 10 minutes

Sample Name Sample Used, gram Yield

Rice Straw 2.129 23.23

Bagasse 1.3302 16.66

Jute Stick 1.1559 11.47

Dry Leaves 5.0117 45.62

Last batch showed the best performance as highest amount of sample was used in that batch. We
found that complete inert condition was more suitable for activation. Here inert means absent of
oxygen. In first two batch nitrogen was used to make the furnace environment oxygen free, but
failed. Then VOC crucibles were used to make the oxygen free environment. Oxygen cannot enter
into the sealed VOC crucibles. In most case using more amount of sample resulted into better
yield. As more amount of sample took more of the volume of the crucible, oxygen had less space
to enter. And as result better yield could be achieved. Stream would be better for physical
activation but due to lack of facility stream flow could not be used.

20
 Rice Straw Activation
25

20
Yield in Percentage

15

10

0
0 0.5 1 1.5 2 2.5
Sample Used, g

Figure 4.1 Graph for Yield vs used Sample of Activated Carbon from Rice Straw of Different
Batch

Rice straw showed almost linear relation. We got better yield by increasing the amount of the
sample. It was not deviated in any batches.

Bagasse Activation
18
16
14
Yield in Percentage

12
10
8
6
4
2
0
0 0.2 0.4 0.6 0.8 1 1.2 1.4
Sample Used, g

Figure 4.2 Graph for Yield vs used Sample of Activated Carbon from Bagasse of Different
Batch

Bagasse also showed linear relation. Though in the 5th batch yield was found less than the previous
batch. But in other cases, better yield was found by using more sample.

21
 Jute Stick Activation
14

12
Yield in Percentage

10

0
0 0.2 0.4 0.6 0.8 1 1.2 1.4
Sample Used, g

Figure 4.3 Graph for Yield vs used Sample of Activated Carbon from Jute Stick of Different Batch

Without data from the 5th batch bagasse also showed linear relation. May be in the 5th batch some
error could not be avoided. Yield of jute stick increased greatly with the using amount.

Dry Leaves Activation

50
45
40
Yiled in Percetnage

35
30
25
20
15
10
5
0
0 1 2 3 4 5 6
Sample Used, g

Figure 4.4 Graph for Yield vs used sample of activated carbon from Dry Leaves of different
batch

Dry leaves showed almost same yield for different amount of sample. And yield of dry leaves is
far better than the other sample. Highest value of other yield even could not cross the half of the
value of the dry leaves.

22
 Comparison of All Bio Wastage
50

45

40
Yield in Percentage

35

30
Rice Straw
25
Bagasse
20
15
Jute Stick
10 Dry Leaves
5

0
0 1 2 3 4 5 6
Sample Used, g

Figure 4.5 Comparison Graph for Yield vs used sample of activated carbon from all Bio Waste
of Different Batch

By comparing all the data found, we came to a decision that jute stick and bagasse showed almost
same yield, yield of rice straw was better but yield of the dry leaves was best. Though we could
use higher amount of dry leaves. As crucible, fully loaded by dry leaves, will weigh higher than
other sample.

23
4.3 BET Surface Analysis and Pore Volume Determination

Both the analysis was done in the analytical laboratory of chemical engineering department,
BUET. Surface analysis was done to check the quality of the activated carbon. As we only used
physical activation process, so our surface area and pore volume were low. Here, data of the
surface area and pore volume are given below both in tabular and graphical form.

Table 4.4 Data of Pore Volume of Activated Carbon from Bio Waste

Pore Volume of Activated

Pore Volume of
Name of the Sample Activated Carbon, Carbon from other research, Reference
cm3/g cm3/g

Rice Straw 0.0731 0.65 38

Bagasse 0.1879 0.53 36

Jute Stick 0.2821 0.57 37

Dry Leaves 0.0917 0.35 22

Pore volume of Activated Carbon from Jute Stick has the highest (0.2821 cm3/g) among the
other Bio Waste Sample. Activated Carbon from Rice Straw and Dry leaves has very low pore
volume (0.0731 cm3/g and 0.0917 cm3/g respectively). Pore volume data of Activated carbon
from same Bio Sample from other research work is also shown in the Table 4.4. Our bio waste
sample has much lower value of pore volume than literature data. Jute Stick has almost half

24
value (49%). But Bagasse is second (achieving 35%) followed by Dry Leaves (26 %) and Rice
straw (11%).

Table 4.5 Data of BET Surface Area of Activated Carbon from Bio Waste

BET Surface Area

BET Surface Area Analysis from
Name of the Sample Analysis, m2/g other Research, Reference
m2/g

Rice Straw 72.64 ± 10.76 1250 38

Bagasse 147.45 ± 47.63 923 36

Jute Stick 202.05 ± 65.83 1266 37

Dry Leaves 56.06 ± 16.31 1070 22

BET surface area was much lower for Dry Leaves; And Jute Stick has the highest BET surface
area. All the BET Surface area of our activated carbon is lower than literature value. We could
not achieve higher surface area as we used only physical activation process. In the literature
value, all the sample was prepared by chemical activation process or used steam for activation in
all of them jute stick showed much close value with the literature data.

25
4.4 Possible Applications
Synthesized activated carbon can be used in waste water treatment, chemical and petroleum
industries, separation, purification, catalysis, energy storage, batteries, fuel cells, nuclear power
stations, electrodes for electric double layer capacitors, pharmaceutical, hydrometallurgy and
others.
Physical properties of activated carbon are crucial in determining its best application.
Commercially Synthesized activated carbon has a surface area ranging from 1500~500 m2/g [22]
and has a pore volume that fluctuates between 0.5~1.4 cm3/g [22]. We could not achieve desired
due to limitation. With further research, these Bio Waste sample can be used commercially for
producing Activated Carbon and can be used in many applications.
Bangladesh produce lot of Bio Waste annually which detrimental to environment. So, Activated
Carbon from Jute Stick and Bagasse can be used in food industries as well as for decolourization,
deodorization and taste removal purposes. In medicine field, for dealing with harmful chemical
and drug adsorption, resulting material can be a good option. In gas cleaning applications, it can
be used for air filters and air conditioning purpose. It can be used for color removal and
backwashing as well.

26
Chapter 5 Conclusion and Future Works
______________________________________________________________________________

5.1 Conclusion

Many researchers have proved bio Waste products previously as a suitable source for producing
activated carbon. Activated Carbon was produced from four types of bio-waste- rice straw,
bagasse, jute sick and dry leaves and among them only,. According to theory, the volatile matter
content and fixed carbon value will increase after the effect of temperature. Hence, the ash content
result and fixed carbon results are conjugated with the theory. But the fixed carbon result of rice-
straw has given slight deviation and the value for sample was 19.18 and that of the activated
product was 4.82. Due the moisture rate fluctuation and temperature maintenance problem, the
result was not accurate. Sample of rice straw was not enough for the experiment as well as the
inert condition provided in the laboratory had to be more accurate for getting the parallel
theoretical result. Jute stick has the highest BET surface area 202.05 m2/g and pore volume of
0.2821 cm3/g and Dry leaves has the lowest BET surface area 56.06 m2/g and pore volume of
0.0917 cm3/g. So, though Dry leaves has higher Fixed carbon, Jute Stick would be best for
producing Activated Carbon. In literature data Activated Carbon from Rice Straw shows good
value as activated carbon but in our thesis work it showed 72.64 m2/g BET surface area and 0.0731
cm3/g of pore volume. Due to low yield, we had limitations to analyze more for rice straw. Bagasse
also showed good value 147.45 m2/g of BET surface area and 0.1879 cm3/g.

Moreover, the granular powder had to be chemically activated for ensuring the highest level of
activation but due to shortage of time chemical activation has not done. Successful conversion of
bio-waste to activated charcoal has not only giving the solution to our waste management problem
in Bangladesh but also brings economic value of making a healthy mass population. In course with
that, further analysis and research is needed prior to commercializing the technology.

27
5.2 Future Works and Recommendations

 The characterization of bio-waste sample and the granular, activated product can be done
in different temperatures in batch-wise mode.
 Chemical activation at 450-600 ℃ temperature should be done after physical activation at
700℃. Chemical activation prevents the tar formation on the particle, hence it increases
the carbon yield.

 ZnCl2 and H3 PO4 are the main activating agent that should be used in the chemical
activation of lignocellulosic material. The use of ZnCl2 could produce higher surface area
therefore, it can produce stronger activated charcoal.
 Measurement of impregnation ratio is the ratio of weight of the activating agent to
precursor, which is one of the most important factor of chemical activation. The
measurement has significant impact on porosity development in the chemical activation
process.
 The pore size requirements of activated carbon generally depend on the types of
applications. For instance, a higher pore volume in the macropore (450 nm) range is needed
to avoid diffusing of the liquid into the mesopore (2–50 nm)and micropore (o2 nm)region.
So, it is important to measure the pore size distribution of granular particle.
 The thermal treatment has two steps- carbonization and activation, where these two steps
has basically the two different temperature range. The carbonization has temperature range
of 400-850 ℃ and the latter one has a range of 600- 900 ℃. The temperature option should
be maintained properly for achieving high quality activated carbon.

28
Reference
______________________________________________________________________________

1. Christian Riuji Lohri, Hassan Mtoro Rajabu, Daniel J. Sweeney, Christian Zurbrügg, “Char
fuel production in developing countries – A review of urban bio-waste carbonization”,
Elsevier, Volume 59, June 2016, pp. 1514-1530.
2. Cuhadaroglu D, Uygun OA., “Production and characterization of activated carbon from a
bituminous coal by chemical activation”, Afr. J. Biotechnol., 2008, pp. 3703–10.
3. Alhamed YA,” Activated carbon from dates' stone by ZnCl2 activation”, .JKAU: Engineering
Sci., Volume 17(2), 2006, pp. 75–100.
4. Campbell QP, Bunt JR, Kasaini H, Kruger DJ, “The preparation of activated carbon from
South African coal”, .JS Afr. Inst. Min Metall., 2012, pp. 37–44.
5. Hassan LG, Itodo AU, Umar UB, “ Equilibrium study on the bio sorption of malachite green
from aqueous solution on to thermo- chemically cracked ground nut shells”, J Chem Pharm
Res, 2010, Volume 2(3), pp. 656–66.
6. Sugumaran P, Susan VP, Ravichandran P, Seshadri S, “Production and Characterization of
activated carbon from banana empty fruit bunch and Delonix regia fruit pod”. J Sustain
Energy Environ, Volume 3, 2012, pp. 125–32.
7. Olafadehan OA, Jinadu OW, Salami L, Popoola OT, “Treatment of brewery waste water
effluent using activated carbon prepared from coconut shell”. Int. J Appl. Sci. Technol.,
2012, pp. 165–78.
8. Jassim AN, Amlah LK, Ali DF, Aljabar ATA. “Preparation and characterization of Activated
carbon from Iraqi apricot stones”, Can. J Chem. Eng. Technol., Volume 3, 2012, pp. 60–5.
9. Onyeji LI, Aboje AA. “Removal of heavy metals from dye effluent using activated carbon
produced from coconut shell”. Int. J. Eng. Sci. Technol., Volume 3, 2011, pp. 8238–46.
10.Abdullah AH, Kasim A, Zainal Z, Hussien MZ, Kuang D, Ahmad F, et al. “Preparation and
characterization of activated carbon from Gelam Wood Bark (Melaleuca cajuputi)”. Malays.
J. Anal Sci., Volume 7, 2001, pp. 65–8.

29
11. Wan Nik WB, Rahman MM, Yusof AM, Ani FN, Adnan CMC, “Production of activated
carbon from palm oil shell waste and its adsorption characteristics”, Proceedings of the 1st
international conference on natural research and engineering technology, 2006.
12. Harris PJF, Lie Z, Suenaga K, “Imaging the atomic structure of activated carbon”. J Phys.
Condens. Mater.2008, pp. 1–5.
13.Chiang HL, Huang CP, Chiang PC., “The surface characteristics of activated carbon as
affected by ozone and alkaline treatment”. Chemosphere 2002, pp. 257–65.
14.Qureshi K, Bhatti I, Kazi R, Ansari AK. “Physical and chemical analysis of activated carbon
prepared from sugarcane bagasse and use for sugar decolorisation”, World Acad. Sci. Eng.
Technol., .2007, pp. 194–8.
15. Puziy AM, v Poddubnaya OI, Socha RP, Gurgul J, Wisniewski M., “XPS and NMR studies
of phosphoric acid activated carbons”, Carbon, 2008, pp. 2113–23.
16.Li L, Quinlivan PA, Knappe DRU, “Effects of activated carbon surface chemistry and pore
structure on the adsorption of organic contaminants from aqueous solution”. Carbon, 2002,
pp. 2085–100.
17. Gaur V, Shankar PA. “Surface modification of activated carbon for the removal of water
impurities”. Water Cond. Purif., 2008, pp. 1–5.
18. Chohfi, Cortez, Luengo, Rocha, and Juan Miguel, "Technology to Produce High Energy
Biomass Briquettes." Techtp.com. Web. 30 Nov. 2010
19. Dr. Axe., “Top 10 Activated Charcoal Uses & Benefits” ,
Available at: https://draxe.com/activated-charcoal-uses/, [Accessed 4 September 2017]
20. Hu Z, Srinivasan MP. “Mesoporous high-surface-area activated carbon”, Micro Meso
Mater, 2001, pp. 267–75.
21. Hayashi J, Horikawa T, TakedaI, Muroyama K, Ani FN, “Preparing activated carbon from
various nut shells by chemical activation with K 2 CO3 ” , Carbon, 2002, pp. 2381–6.
22. Ioannidou O, Zabaniotou A. “Agricultural residues as precursors for activated carbon
production – a review”, Renew Sustain Energy Rev, 2007, pp. 1966–2005.
23. Ketcha JM, Dina DJD, Ngomo HM, Ndi NJ, “ Preparation and characterization of activated
carbons obtained from maize cobs by zinc chloride activation” , Am Chem Sci. J, 2012, pp.
13660.

30
24. Williams PT, Reed AR., “High grade activated carbon matting derived from the chemical
activation and pyrolysis of natural fibre textile waste”, J Anal Appl. Pyrol. 2004, pp. 971–
86.
25. McNaught AD, Wilkinson A.” IUPAC compendium of chemical terminology”, Oxford
(UK): Blackwell Science, second ed., 1997.
26. Antal MJ, Gronli M. “Threat, science, and technology of charcoal production”, Ind. Eng.
Chem. Res. 2003, pp. 1619–40.
27. ‘Test Methods for Activated Carbon”, European council of Chemical Manufacturers’
Federations, April 1986.
28. Duku MH, Gu S, Hagan EB, “Biochar production potential in Ghana—a review”. Renew
Sustainable Energy Rev., 2011, pp. 3539–51.
29. Tsai WT, Chang CY, Wang SY, Chang CF, Chien SF, Sun HF,“ Cleaner production of
carbon adsorbents by utilizing agricultural waste corn cob”, Res. Conserv Rec, 2001, pp.
43–53.
30. Williams PT, Reed AR., “Development of activated carbon pore structure via physical and
chemical activation of biomass fibre waste”, Biomass Bioenergy, 2006, pp. 144–52.
31. Williams PT, Reed AR., “High grade activated carbon matting derived from the chemical
activation and pyrolysis of natural fibre textile waste”, J. Anal. Appl. Pyrol., 2004, pp. 971-
86.
32. Li W, Yang K, Peng J, Zhang L, Guo S, Xia H., ”Effects of carbonization temperatures on
characteristics of porosity in coconut shell chars and activated carbons derived from
carbonized coconut shell chars”, Ind. Crops Prod , 2008, pp. 190–8.
33. Ahmadpour A, Do DD, “The preparation of activated carbon from Macadamia nutshell by
chemical activation”, Carbon, 1997, pp. 1723–32.
34. Houache O, Al-Maamari R, Al-Rashidi B, Jibril B, “Study of date palm stem as raw material
in preparation of activated carbon”, J. Eng. Res. ,2008, pp. 47–54.
35. Mohammad Asadullah, “ Adsorption Studies on Activated Carbon Derived from Steam
Activation of Jute Stick Char”, Journal of Surface Science and Technology- January 2007,
PP. 73-80

31
36. Boonpoke A, CHaiarakorn S, Laosiripojana N, Towprayoon S, Chidthaisong A,
“Synthesis of activated carbon and MCM-41 from bagasse and rice husk and their carbon
dioxide adsorption capacity” , J Sustain Energy Environ, 2011; PP.77-81

37.Mohammad Asadullah, Israt Jahan, Mohammad Boshir Ahmed, Pasilatun Adawiyah, Nur
Hanina Malek, Mohammad Sahedur Rahman, “Preparation of microporous activated carbon
and its modification for arsenic removal from water”, Journal of Industrial and
Engineering,Chemistry 20 (2014) 887–896
38.Oh GH, Park CR. Preparation and characteristics of rice-sraw-based porous carbons with high
adsorption capacity. Fuel 2002;81:327–36.
39. Ahmed Humayun Kabir Topu, “ Time for jute stick too to earn forex”, The Daily Star, 12:00
AM, November 20, 2016 / LAST MODIFIED: 03:26 AM, November 20, 2016

32
Appendices
______________________________________________________________________________

Figure A.1 BET surface area & Pore Volume data for Activated Carbon from Rice Straw

33
Figure A.2 BET surface area & pore volume data for Activated Carbon from Bagasse
34
Figure A.3 BET surface area & pore volume data for Activated Carbon from Jute Stick
35
Figure A.4 BET surface area & pore volume data for Activated Carbon from Dry Leaves
36