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ABSTRACT

Ore processing through the extraction process is classified into several methods, among others:
Pyrometallurgy, Hydrometallurgy, and Electrometallurgy. Among the three methods, the
extraction process through the pyrometallurical method is the most widely used process
compared to hydrometallurgy and electrometallurgy. Pyrometallurgy is the most widely used
because of its economically process and compatible for create an industry scale.
Pyrometallurgy is a branch of extractive metallurgy. It consists of the thermal treatment of
minerals and metallurgical ores and concentrates to bring about physical and
chemical transformations in the materials to enable recovery of valuable metals. Before the ore
is fed to the pyrometallurgy reaactor / furnace, the ore will be crushed and agglomerated. This
aglomeration process aims to agglomerate and homogenize the size of the ore so that it its good
to be processed in the furnace. Materials used in agglomeration process are Lateritic nickel ore,
Wood charcoal, Na2SO4 powder, Tapioca, Aquades. Equipments used in agglomeration
process are Compaction tools, Drying oven, Crusher, Screen with 50 mesh standard size,
Digital scales, and Measuring cup. Materials used in carbothermic direct reduction are Nickel
briquettes, Coals, Limestone, and LPG. Equipments used in carbothermic direct reduction are
Muffle Furnace, Crucible, Thermocouple, and Blower.The procedures to do agglomeration
process are Lateritic nickel ores and charcoals are crushed using crusher. The lateritic nickel
ores and charcoals are sieved using 50 mesh standars sieve. The lateritic nickel ores out from
the sieve are mixed with wood charcoals and sodium sulphate (Na2SO4) with a mass ratio of
100 : 12 : 12 (ore : charcoal : Na2SO4) Tapioca mixed with water of 100 mL, and heated in
boiling water until slightly thickened. The mixture of lateritic nickel ores, wood charcoal, and
Na2SO4 are added with tapioca which has slightly thickened and stirred until evenly
distributed. The mixture is formed into a pillow briquette using a mold. Then the briquettes
which have been compacted are then dried at 110⁰C for 3 hours using the drying oven.The
briquettes measured their mass after drying and calculated mass changes before and after
drying. The procedure to do carbothermic direct reduction are the briquettes is inserted into the
crucible which contains a mixture of coal and limestone. Crucible is placed in Muffle Furnace
and preheated to 700⁰C in 60 minutes. Then, it was holded at temperature 700⁰C for 2 hours.
Temperature was increased to temperature of 1400⁰C in 60 minutes. Then, it was holded at a
temperature of 1400⁰C for 6 hours. The briquette is cooled inside the Muffle Furnace for 12
hours. After that the briquette being weighed and calculate the degree of reduction and moisture
content of the briquette. From the experiment that we have done, the moisture content of bricket
1 dan 2 are 16 % and 17,857% respectively. Then the degree of reduction value is 8.94%.

Keywords: Ore, Briquettes, Direct Reduction

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DAFTAR ISI

ABSTRACT ......................................................................................................................... i
LIST OF CONTENTS ......................................................................................................... ii
LIST OF FIGURES ............................................................................................................ iii
LIST OF TABLE ................................................................................................................ iv
BAB I INTRODUCTION
I.1 Background ........................................................................................................... 1
I.2 Problem Formulation ............................................................................................ 1
I.3 Practicum Goal ..................................................................................................... 2
BAB II LITERTATURE
II.1 Direct Reduction Iron .......................................................................................... 3
II.2 Agglomeration ..................................................................................................... 3
II.3 Laterite................................................................................................................. 6
II.4 Charcoal ............................................................................................................. 10
II.5 Coal.................................................................................................................... 11
II.6 Limestone .......................................................................................................... 12
II.7 Muffle Furnace .................................................................................................. 13
II.8 Crucible Furnace ............................................................................................... 14
BAB III METODHOLOGY
III.1 Flow Sheet ........................................................................................................ 16
III.2 Materials Equipment ........................................................................................ 17
III.3 Practicum Procedure ........................................................................................ 17
III.4 Calculation ....................................................................................................... 21
BAB IV DATA ANALYSYS AND DISCUSSION
IV.1 Data Analysis ................................................................................................... 23
IV.2 Discussion ........................................................................................................ 24
BAB V CONCLUSION AND SUGGESTION
V.1 Conclusion......................................................................................................... 25
V.2 Suggestion ......................................................................................................... 25
REFERENCES .................................................................................................................... v

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LIST OF FIGURES

Figure II.1 Consequent Steps For Briquetting ..................................................................... 5

Figure II.2 Formation and ecolution of oxide and hydrous Mg silicate deposits ................ 7
Figure II.3 Lateritic profiles developed on serpentinized ultramaic rocks showing the
principal nickel laterite ores ................................................................................................ 8
Figure II.4 Nickel Laterite ................................................................................................... 9
Figure II.5 Eearly Charcoal Productions in Earth Kilns Terite Ores ................................. 11
Figure II.6 Types of Coal .................................................................................................. 12
Figure II.7 Limestone ........................................................................................................ 13
Figure II.8 Muffle Furnace ................................................................................................ 14
Figure II.9 Crucible Furnace ............................................................................................. 15
Figure III.1 Flow Sheet of Agglomeration Process ........................................................... 16
Figure III.2 Flow Sheet of Carbothermic Direct Reduction .............................................. 17
Figure III.3 Archimedes Principle for Volume Calculation .............................................. 20

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LIST OF TABLES

Table 2.1 Principal Ore Mineral in Laterite Deposits ......................................................... 9

Table 3.1 Varies the Limestone Used Between Groups .................................................... 19
Table 4.1 Moisture Content ............................................................................................... 22
Table 4.2 Degree of Reduction .......................................................................................... 22

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CHAPTER I
INTRODUCTION
I.1 Background

Ore processing through the extraction process is classifie into several methods, among
others: Pyrometallurgy, Hydrometallurgy, and Electrometallurgy. Among the three methods,
the extraction process through the pyrometallurical method is the most widely used process
compared to hydrometallurgy and electrometallurgy. Pyrometallurgy is the most widely
used because of its economically process and compatible for create an industry scale.
Pyrometallurgy is a branch of extractive metallurgy. It consists of the thermal treatment of
minerals and metallurgical ores and concentrates to bring about physical and
chemical transformations in the materials to enable recovery of valuable
metals. Pyrometallurgical treatment may produce products able to be sold such as pure
metals, or intermediate compounds or alloys, suitable as feed for further processing.
Examples of elements extracted by pyrometallurgical processes include the oxides of less
reactive elements like iron, copper, zinc, chromium, tin, and manganese. Before the ore is
fed to the pyrometallurgy reactor / furnace, the ore will be crushed and agglomerated. This
agglomeration process aims to agglomerate and homogenize the size of the ore so that it its
good to be processed in the furnace. The agglomeration process done in this practicum is the
process of briquetting and drying. One of the ore that are established in the huge amount in
Indonesia is nickel ore, which is generally divide into two classes based on the type of
impurity, I.e. nickel sulfide ore and lateritic ore (oxide). The availability of nickel ore in the
world is divided into 60% of sulfide ore and 40% of lateric ore, but ore processing in the
world is dominated by nickel sulfide ore processing which is reaches about 70%. Indonesia
is the country which is rich in nickel ore oxide resources so that Indonesian actually must be
expert in extractive metallurgy subject in order to process that ore. One of the kind extraction
method is pyrometallurgy and can be done by direct reduction furnace or blast furnace. With
direct reduction furnace this process can be done without melt the ore and only used lower
than melting temperature. In direct reduction furnace uses source gas from carbon monoxide
or nitrogen which can come from the natural gas. The advantage of using direct reduction
furnace is saving energy and also cleaner than blast furnace in its waste. In this time, the
laboratory will be done process of reduction of nickel laterite ore of lateritic nickel type by
pyrometallurgy process using muffle furnace. The reduction process aims to separate the
nickel content form its impurities.
I.2 Problem Formulation
As for the problem formulation that we used in this practicum is consist of:
1. How is the process of ore crushing and carbothermic reduction of nickel?

2. How to analyze the cause of the briquettes made is not acceptable and the cause of the
reduction results if not optimal?\

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3. How to analyze Teknologi
the relationship between Sepuluh
the form Nopember
of briquette, homogeneity of briquette
mass, pores and shatter index briquettes to the next process, i.e. reduction process and also
the relationship between reduction temperature and reduction resistant time to get a good
reduction result?
I.3 Practicum Goal
As for the goal in this practicum is consist of:
1. Understand the process of ore crushing and carbothermic reduction of nickel.

2. Being able to analyze the cause of the briquettes made is not acceptable and the cause of
the reduction results if not optimal.

3. Being able to analyze the relationship between the form of briquette, homogeneity of
briquette mass, pores and shatter index briquettes to the next process, i.e. reduction process
and also the relationship between reduction temperature and reduction resistant time to get
a good reduction result.

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CHAPTER II
LITERATURE
II.1 DRI (Direct Reduced Iron)
DRI or sponge iron refers to porous iron produced by the DR process. The DR process
is a solid-state reaction process (solid–solid or solid–gas reaction) in which removable
oxygen is removed from the iron oxide, using coal or reformed natural gas as reductants,
below the melting and fusion point of the lump ore or agglomerates of fine ore. The external
shape of the ore remains unchanged. Due to removal of oxygen (about 27–30% reduction
in weight occurs), a honeycombed microstructure develops suggesting the name Sponge
Iron. (solid porous iron; lumps/pellets with many voids filled with air).

DRI is obtained when iron oxide (generally lump iron ore or pellets) is reduced to
metallic form in solid state. Since there is no melting, the external shape is retained. Color
changes from red to black. The true density ranges from about 3.5 · 103 to 4.4 · 103 kg/m3.
The true density of pure iron is 7.8 · 103 kg/m3. Thus, there is about 45–56% reduction in
true volume and this is manifested in the formation of pores throughout the interior of
sponge iron pieces.
II.1.1 Direct Reduction Processes
Based on the types of reductant used, the DR processes can be broadly classified
into two groups:
1. Using solid reductant, that is, coal-based DR process
2. Using gaseous reductant, that is, gas-based DR process
The reactivity of the reductant is measure of its ability to react with carbon dioxide
to form carbon monoxide according to boundouard reaction :
C(s) + CO2(g) = 2CO(g) ...................................................................................... (1.1)
(Kumar, 2016, 1084)
II.2 Agglomeration
Agglomeration is processed ores formed into coherent pieces which are substantially
larger than the original particles (Babich et al., 2008). Two agglomeration methods, are
generally used: sintering for fine ores and pelletizing for concentrates. Briquetting is also
one agglomeration method, used in the iron-steel industry mainly for preparation of
materials for steelmaking (Babich et al., 2008).
II.2.1 Sintering
Sintering is agglomeration of fine mineral particles into a porous mass by
incipient fusion caused by heat produced by combustion within the mass itself
(Babich et al., 2008). Sintering aims in general to produce sintered parts with
reproducible, and if possible, designed microstructure through control of sintering
variables. Microstructural controls means the control of grain size, sintered density,

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and size and distribution of other phases including pores. The final goal is to prepare
a fully dense body with a fine grain structure (L. Kang, 2005).
Some most essential properties of sinter products are:
1. Reducibility: oxygen removal rates in gaseous reducing atmosphere.
2. Size & size distribution: should provide uniform and sufficient gas permeability
3. Strength: resistance of breakage due to impact, abrassion, compression, etc.
4. Softening behaviour: temperature of start softening should be high and range of
it should be narrow.
(Babich et al., 2008)
II.2.2 Pelletizing
Spherical agglomerates formed by balling fine ores, usually finer than 100 mm,
with various additives followed by sometimes by hot or cold bonding induration
(Babich et al., 2008).
There are 3 steps necessary to produce a pellet:
1. Preparation of raw materials
2. Formation of green pellets
3. Firing of green pellets
For relative large particles, grinding is necessary. Generally a grain size
distribution of raw materials for pelletizing must below than 0,2 mm. For full
capillary effect the ore concentrate must be sufficiently fine-grained having about
70-80% of fraction < 40 nm (Babich et al., 2008).
Some important physical and metallurgical properties of fired pellets are:
1. Cold compression strength
2. Reduction strength
3. Reducibility
4. Softening behaviour
5. Density
6. Porosity
7. Size distribution
8. Swelling behaviour
(Babich et al., 2008)

II.2.3 Briquetting
In briquetting, fine particles are compressed with partial or full controlled
forming in order to produce a solid body of defined shape. Briquetting pressure and
temperature, kind and amount of binding agents, and following secondary treatment
determine the binding mechanism. The binding is achieved through following
mechanism:

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1. Molecular attraction (Van der Waals forces)

2. Melting or sintering of single grains because of plasticity caused by temperature
or pressure
3. Recrystallization
4. Mutual penetration of absorbed adhesives or binding agent layers
5. Controlled binding
Based on the temperature, briquetting process is divided into two: cold and hot
briquetting. Cold briquetting carried out at room temperature or slightly increased
temperature. While hot briquetting takes place at temperature reaching up to 1000oC.
Some consequent steps for briquetting are as follows:
1. Closing of downside forming edge and separation of the new from old briquette.
Material is soaked from upside into hollow space by gravity or stuffing (a.).
2. Compressing of loose material (b. and c.).
3. Opening of downside forming edge before total compression. Closing of forming
edge in the upper part and compression of material (d.).
4. Slopping of briquette (e.).

Figure II.1 Consequent Steps for Briquetting (Babitch et al., 2008)

Briquetting has some advantages, these are:
1. Easy storage, handling, and transport.
2. Prevention of uncontrolled agglomeration process.
3. Generation of suitable size and form of the material for further application.
(Babich et al., 2008)
Usually, briquetting is undergo by mixing the laterites, coal and flux, with
additional composition in the form of starch. Starch is used as a binder for increasing
the strength of green briquette before the roasting process, reducing the level of
degradation of briquette before the roasting process, and reducing the level of
degradation of briquettes during transportation and handling. Because only for the
purposes before the roasting process, the binder must not have a negative effect on
the roasting process. The starch is chosen as a binder because starch is an organic
substance, which will burn out during heating (Kumar Gupta, 2003).

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II.3 Laterite
Nickeliferous laterites are residual products derived from chemical weathering of
olivine-rich cumulate rocks and their metamorphic derivatives which have primary initial
Ni contents of 0.2- 0.4%. The characteristics of a Ni laterite, including grade, tonnage and
mineralogy, are controlled by the interaction of climatic and geological factors. Thise
factors are geomorphological history, drainage, structure and lithology. The combined
effect of these individual factors in a dynamic system allows Ni to concentrate in the
regolith.
About 85% (in the world) Ni laterite resources are located in accretionary terrains,
developed in the weathered mantle of obducted Miocene and Pliocene ophiolite complexes.
These harzburgite-dunite-olivine cumulates cover thousands of square kilometres, have
marked topographic relief and account for Ni laterite deposits in, for example, New
Caledonia, the Philippines, Indonesia, Australia (Queensland), Colombia, Cuba, the
Dominican Republic, and Western USA.
Other 15% of laterite resources are located in stable cratonic platforns, developed on
komatiites and layered complexes in Archaean and Proterozoic greenstone belts. The
komatiitic lithologies, dominated by peridotites and dunites, typically have a moderate to
subdued relief. These deposits developed in many places include the Yilgarn Craton of
Western Australia and parts of Brazil, West Africa, and Ukraine.
(Brand et al., 1998)
II.3.1 Formation and Evolution of Nickel Laterite
1. Direct Formation
Many deposits formed during an essentially continuous weathering episode under
a dominantly humid savanna climate. These conditions are typical of lateritization
on cratons and less active accretionary terranes. High water-tables, fluctuating
seasonally in savanna climates, and low erosion rates favour weathering to 50–80
m. In free-draining environments, Ni released by the hydrolysis of olivine or
serpentinized olivine is largely retained and is hosted by goethite. Magnesium and
silica are leached, causing porosity to increase and density to decrease, with a total
mass loss of up to 70%. This alone can residually concentrate Ni in the ferruginous
oxide zone above the Mg-discontinuity to 0.6–1%, where it is mainly adsorbed to
goethite. In poorly drained environments, similar oxide zones develop over
serpentinized dunite, but as silica may not be fully leached, it can precipitate as
quartz in the lower oxide zone, the upper Mg-bearing saprolite and fault zones.
Mg, Si and Ni are retained in smectites in the mid to upper saprolite.

2. Multi-stage Formation
Tectonic uplift has played an important role in the formation of some deposits in
areas of originally low relief by rejuvenating the topography and lowering
previously high water-tables. In the humid tropics, this has typically led to
leaching of Ni from the oxide zones and its accumulation in hydrous Mg silicates
deeper in the saprolite. This process accounts for many high-grade

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deposits inuplifted and partly eroded plateaux and terraces. A related mechanism
may account for the formation of some hydrous Mg silicate deposits in more stable
areas of generally low relief. Relief inversion has left isolated hills of free-
draining, weathered ultramafic rocks, protected by ferruginous duricrust, in which
Ni leached from the oxide zone has concentrated in saprolite.

Figure II.2 Formation and evolution of oxide and hydrous Mg silicate deposits.

(A) Progressive development of a well-differentiated lateritic regolith under a

seasonally humid savanna climate in an area with low relief and tectonic stability.
(B) With uplift and under a similar climate, leaching and reaction/exchange of Ni
yield hydrous Mg silicates. (C) The profile is modified during a change to an arid
climate, with precipitation of magnesite and silica.

1. (Fe,Mg)2SiO4 + 5H- → 2FeOOH + H4SiO4(aq) + Mg2+

olivine geothite silicic acid
2. 2(Fe,Mg)3Si2O5(OH)4 + 3H2O → Mg3Si4O10(OH)2 + FeOOH + 2Mg2+ + 3OH-
serpentine saponite
3. FeOOH.(Ni)(OH)2 + 2H → FeOOH + Ni2+ + 2H2O
+

goethite, absorbed Ni
4. Mg3Si2O5(OH)4 + Ni2+ → (Mg,Ni)3Si2O5(OH)4 + Mg2+
lizardite Ni serpentine/né pouite/ 7Ǻ garnierite
5. 4Mg2SiO4 + Ni + 10H+ → Mg2NiSi4O10(OH)2 + 2Mg2+ + 4H2O
2+

forsterite Ni-saponite
6. (Mg,Fe)3Si2O5(OH)4 + 3H+ → FeOOH + 2SiO2 + 2Mg2+ + 3H2O
(Butt and Cluzel, 2013).

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II.3.2 Classification, Mineralogy, Grade, and Chemical Composition of Ini Laterite
Various classification schemes exist for Ni laterites, based on features such as
alteration of the host rock, climate, drainage, geomorphological history, and
composition. Based on the mineralogy of the dominant Ni host. There are three main
types of deposit:
Type A: silicate Ni deposits, dominated by hydrated Mg-Ini silicates (e.g. gamierite),
generally occurring deep in the saprolite.
Type B: silicate Ni deposits, dominated by smectitic clays (e.g. nontronite),
commonly occurring in the upper saprolite or pedolith.
Type C: oxide deposits, dominated by Fe oxyhydroxides (e.g. goethite), forming a
layer at the pedolith saprolith boundary.
The silicate Ni deposits, dominated by type A, account for 80% of global Ni laterite
resources; most Ni laterite deposits, however, contain both silicate and oxide ore in
varying proportions. Manganese oxides , enriched in Co and Ni , probably formed
during late phases of weathering, are present in each type of deposit, but account for
only a minor proportion of the total Ni.
(Brand et al., 1998).

Figure II.3 Lateritic profiles developed on serpentinized ultramafic rocks showing the
principal nickel laterite ores. (A) oxide; (B) partly silicified oxide; (C) hydrous Mg silicate;
(D) Clay silicate (Butt and Cluzel, 2013).

Table 2.1 Principal ore minerals in Ni laterite deposits. Most minerals are poorly crystalline
and variable in composition (Butt and Cluzel, 2013).
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Hydrous Mg Silicate Ore
Ni lizardite - népouite Serpentine (Mg,Ni)3Si2O5(OH)4 6-33% Ni
7Å garnierite Serpentine Variable, poorly defined 15% Ni
Nimite Chlorite (Ni5Al)(Si3Al)O10(OH)8 17% Ni
14Å garnierite Chlorite Variable, poorly defined 3% Ni
Falcondoite Sepiolite (Ni,Mg)4Si6O15(OH)2.6H2O 24% Ni
Kerolite-willemseite Talc (Ni,Mg)3Si4O10(OH)2 16–27% Ni
10Å garnierite Talc Variable, poorly defi ned 20% Ni
Clay Silicate Ore
3+
Nontronite Smectite Na0.3Fe2 (Si,Al)4O10(OH)2.nH2O ~4% Ni
2+
Saponite Smectite (Ca/2,Na)0.3(Mg,Fe )3(Si,Al)4O10(OH2).4H2O ~3% Ni
Oxide Ore
Goethite Oxide α-(Fe )O(OH)
3+
2% Ni, 0.2% Co
2+ 3+ 4+
Asbolane Oxide (Ni ,Co )xMn (O,OH)4.nH2O 16% Ni, >4% Co
4+
Lithiophorite Oxide (Al,Li)Mn O2(OH)2 1% Ni, ~7% Co

The mineralogy of type A silicate deposits is highly variable, consisting of a mixture of both
well-crystallized and poorly defined neoformed varieties of Ni-bearing hydrous silicates,
referred to as garnierite, in which the Ni content of individual minerals can exceed 20%.
Smectite-dominant type B deposits are characterized by Ni-rich nontronite and saponite,
typically containing 1.0- 1.5% Ni , with the Ni fixed between the structural laye rs or in the
octahedral layer, substituting for Fe3+.

Figure II.4 Nickel Laterite Ore (Private Documentation)

Iron oxides, commonly referred to as limonite in the Ni laterite literature, dominate the
type C oxide deposits. Similar materials also overlie silicate deposits and penetrate through
them in fractures and joint planes. Goethite and poorly crystalline Fe oxyhydroxides are the

principal Ni host minerals of type C deposits. Experimental studies have shown that goethite
may contain up to 5.4 mole %Ni, but the proportion of Ni incorporated into the lattice,
adsorbed onto the surface or present within its structure is still a matter of debate. Other Fe

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in minor quantities in theTeknologi Sepuluh
ore zone (e.g. Nopember
magnetite, lepidocrocite and hematite),
have low Ni contents.
The silicate Ni deposits have a grade of 1-2.6% Ni, with a global mean grade of 1.53%
Ni for hydrated Mg- Ni silicates (type A) and 1.21 % Ni for smectite-dominated deposits (type
B). Parts of some type A deposits (e.g. New Caledonia), however, can exceed 15% Ni and are
typically associated with faults and shear zones. Oxide deposits generally have a grade of up
to 1.6% Ni, (e.g. Goro, New Caledonia), with a global mean grade of l.03% Ni.
During weathering, some elements become leached (e.g. Mg, Ca ± Si) and others either
are secondarily enriched (e.g. Ni, Mn, Co, Zn, Y) or residually concentrated (e.g. Fe, Cr, AI,
Ti, Zr, Cu) within the profile. Both types of silicate deposit are characterized by a low Si:Mg
ratio (type A, 2-4; type B, typically <10), < 20% Fe for type A, and up to 30% Fe for type B
(depending on clay type), and are neutral to mildly alkaline (pH 7.6-8.7). The type C oxide
deposits have low Si and Mg concentrations, high Fe (>40% Fe), and are weakly acid (pH
5.2-5.7). Chromium and Al contents have been increased by relative accumulation in the oxide
zone. Only Ni and, in places, Co are significantly enriched in the supergene phases.
(Brand et al, 1998)
II.4 Charcoal
Charcoal is defined as carbonized wood used mainly as fuel or as reductant in industry,
e.g., to reduce oxidized iron ores in iron and steel production. The production of gunpowder
containing 15% charcoal was the principal driver for research on charcoal. This included
trials on different types of wood as feedstock and on production technologies overall
aiming at low ash contents to enable a clean combustion. Charcoal was
and is mainly used as a smokeless fuel for cooking, heating and steel production.
(Hagemann et al., 2018).
Charcoal is produced by heating wood in airtight ovens or retorts, in chambers with
various gases, or in kilns supplied with limited and controlled amounts of air. High-
temperature heating by all methods breaks down the wood into gases, a watery tar mixture,
and the familiar solid carbon material commonly known as charcoal. Charcoal is obtained
from all species of wood. The charcoal, or impure carbon, yielded by the various
commercial methods is usually considered adequately refined for its markets. The
carbonization, or socalled "coaling," temperatures used control the amounts of volatiles or
smoky material remaining in the charcoal. If coaling temperatures are too low, excessive
amounts of volatiles will remain in the charcoal and cause heavy smoke when it burns. The
yield of charcoal from a given amount of wood by weight is dependent upon the amount
of carbon in the wood and the carbonization conditions employed. On the average, carbon

constitutes about 50 percent of the dry weight of the wood. At least this amount is likewise
present in hardwood barks, while softwood barks contain somewhat less. (Toole et al., 1961)

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Figure II.5 Early Charcoal Productions in Earth Kilns (Toole et al., 1961)
II.5 Coal
Coal is a fossil fuel. It is a combustible, sedimentary, organic rock, which is composed
mainly of carbon, hydrogen and oxygen. It is formed from vegetation, which has been
consolidated between other rock strata and altered by the combined effects of pressure and
heat over millions of years to form coal seams. Coal is a fossil fuel. It is a combustible,
sedimentary, organic rock, which is composed mainly of carbon, hydrogen and oxygen. It
is formed from vegetation, which has been consolidated between other rock strata and
altered by the combined effects of pressure and heat over millions of years to form coal
seams. The quality of each coal deposit is determined by temperature and pressure and by
the length of time in formation, which is referred to as its ‘organic maturity’. Initially the
peat is converted into lignite or ‘brown coal’ types with low organic maturity. In
comparison to other coals, lignite is quite soft and its colour can range from dark black to
various shades of brown (World Coal Institute, 2005)
The degree of change undergone by a coal as it matures from peat to anthracite, known
as coalification has an important bearing on its physical and chemical properties and is
referred to as the ‘rank’ of the coal. Low rank coals, such as lignite and sub- bituminous
coals are typically softer, friable materials with a dull, earthy appearance. They are
characterised by high moisture levels and low carbon content, and therefore a low energy
content. Higher rank coals are generally harder and stronger and often have a black,
vitreous lustre. They contain more carbon, have lower moisture content, and produce more
energy. Anthracite is at the top of the rank scale and has a correspondingly higher carbon
and energy content and a lower level of moisture (World Coal Institute, 2005)

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Figure II.6 Types of Coal (World Coal Institute, 2005)

II.6 Limestone
Limestones have been worked for many thousands of years, initially for building stone
and agricultural lime and more recently for a wide range of construction and industrial uses.
In most industrialized countries limestone quarries represent the most visually obvious and,
in both process and landform terms, the most dramatic anthropogenic impact on karst
terrain. However, quarrying has, to date, received surprisingly little attention from karst
scientists. Research in the English Peak District suggested that the postexcavation
evolution of quarried limestone rock faces was in part a result of the methods used in their
excavation, and this led to the development of a technique designed to reduce the visual
and environmental impacts of modern quarries by “Landform replication. ” This involves
the use of controlled “restoration blasting” techniques on quarried rock slopes to construct
a landform sequence similar to that in the surrounding natural landscape. The constructed
landforms are then partially revegetated using appropriate wildflower, grass, and/or tree
species.
The earliest and simplest methods of extraction involved the use of human muscle to
remove limestone from free faces. For example, drawings of early quarries in the En- glish
Peak District show men suspended from ropes prising loose stones from valley sides. The
stone fell to the ground where it was further broken using sledgehammers. It is possible
that the characteristic form of limestone valleys in the Peak District (steep free faces above
scree slopes) may in part be a result of this early form of quarrying. Manual extraction was
largely superseded by the use of explosives in the 19 century but mechanical excavators
are still used on some weaker limestones (e.g., chalk) and saws are used to remove harder,
decorative limestones (marbles).
(Gunn, 1983)

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Figure II.7 Limestone (M. Heikal, 2000)

II.7 Muffle Furnace
Limestones have been worked for many thousands of years, initially for building stone
and agricultural lime and more recently for a wide range of construction and industrial uses.
In most industrialized countries limestone quarries represent the most visually obvious and,
in both process and landform terms, the most dramatic anthropogenic impact on karst
terrain. However, quarrying has, to date, received surprisingly little attention from karst
scientists. Research in the English Peak District suggested that the postexcavation
evolution of quarried limestone rock faces was in part a result of the methods used in their
excavation, and this led to the development of a technique designed to reduce the visual
and environmental impacts of modern quarries by “Landform replication. ” This involves
the use of controlled “restoration blasting” techniques on quarried rock slopes to construct
a landform sequence similar to that in the surrounding natural landscape. The constructed
landforms are then partially revegetated using appropriate wildflower, grass, and/or tree
species.
The earliest and simplest methods of extraction involved the use of human muscle to
remove limestone from free faces. For example, drawings of early quarries in the En- glish
Peak District show men suspended from ropes prising loose stones from valley sides. The
stone fell to the ground where it was further broken using sledgehammers. It is possible
that the characteristic form of limestone valleys in the Peak District (steep free faces above
scree slopes) may in part be a result of this early form of quarrying. Manual extraction was
largely superseded by the use of explosives in the 19 century but mechanical excavators
are still used on some weaker limestones (e.g., chalk) and saws are used to remove harder,
decorative limestones (marbles).
(Gunn, 1983)
This invention relates to a tunnel type heating furnace provided with an elongated
metallic muffle, and more particularly it relates to a muffle furnace in which pro visions
are made to prevent the deformation or warp of muffle. Various gases are employed as an
atomophere of furnaces for the deoxidation or oxygen free heating of articles in the
furnaces. In order to keep the atmosphere at a high purity, metallic muffles are often used.
How ever, such muffles which are elongated and extend sometimes as long as 10 m, are
apt to warp on account of differences of temperature produced among different portions
thereof and especially between upper and lower portions with the elevation of temperature
at their cyclic first operations and with the repeated intro duction of articles thereinto. This
warp or deformation adversely affects the normal operation of furnaces. Hence, an object
of this invention is to provide a muffle furnace in which the metallic muffle shall not be

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deformed, and by which articles in Teknologi Sepuluh
the furnace can Nopember
be uniformly heated. It is known for
those skilled in this art to control a temperature of metallic muffles in a heating furnace
under a predetermined temperature by means of programmed heating. This conventional
method can not, however, prevent the deformation of the muffles, because while it can
make the muffles be subjected to a certain temperature as a whole, it can not prevent dif
ference of temperatures existing among different por tions of muffles. Whereas, in this
invention, a muffle which is heated by a plurality of heaters is checked continuously as to
its temperature at several different portions thereof, and the muffle is continuously kept at
a predetermined tem perature or temperatures corresponding to those exist ing at one or
more of said several portions, while the temperatures of other portions are controlled so as
to be substantially equal to said predetermined tem perature(s). It shall be noted that said
predetermined tempera tures can be varied as one desires, whereby the muffle can be heated
to any desired temperature, and that temperatures working at the muffle are substantially
equal at any portion thereof, whereby muffles shall not be deformed, resulting in the
smooth operation and running of a furnace.

(Takahashi,1983)

Figure II.8 Muffle Furnace (Gao Q, 2013)

II.8 Crucible furnace
A furnace is an apparatus in which heat is generated and transferred directly or indirectly
to a molten or solid mass for the purpose of effecting a physical, chemical or metallurgical
change in the mass. Furnace is equipment isolated from the surrounding by an insulated
wall and is used to transfer heat to the material to be melted or heat treated within the
furnace .. An ideal furnace is one in which all energy produced is utilized, this practically
unachievable and there is no thermal processing equipment with efficiency of 100% . A
furnace of high efficiency is therefore a system in which energy losses are minimal
Accoding to . Furnace can be classified according to the firing techniques; direct-fired and
indirect-fired furnace. In direct- fired furnace the product of combustion has direct contact
with the surface of the workload, this workloads are affected by the product of combustion.
Indirectfired furnaces are for heating materials and products for which the quality of the
finished products may be inferior if they have come in contact with flame or products of
combustion. In such cases, the stock or charge may be (a) heated in an enclosing muffle

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(conductingTechnologyInstitut Teknologi
container) that is heated Sepuluh
from the outside Nopember
by products of combustion from
burners or (b) heated by radiant tubes that enclose the flame and products of combustion.
Crucible furnace is one of the oldest and simplest types of melting furnace unit in the
foundry. The furnaces use a refractory crucible which contains the metal charge. The
charge is heated via conduction of heat through the wall of the crucible. Crucible melting
is commonly used where small datches of low melting point alloy are required. The capital
outlay of these furnaces makes their attraction to small non-ferrous foundries. Melting of
metals is one basic industrial practice in the production of engineering products
(Atanda, P. O. 2014)

Figure II.9 Crucible Furnace (A. A. Olalere. 2015)

A pot furnace or crucible furnace is a form of muffle furnace in which the container
prevents product of combustion contact with the load. Ideally, all heat added to the furnaces
should be used to heat the charge, load or stock. In practice, however, a lot of heat is lost
in several ways. The losses include energy conversion losses, furnace wall losses, furnace
opening losses and the likes. In order to prevent these losses, materials that can retain and
conserve heat known as refractory materials are therefore used as lining materials for the
furnaces. Refractories are porous, multi-component and heterogeneous materials
composed of thermally stable mineral aggregate, a binder phase and additives.
(Gbasouzor.2018)
SiC-Based materials are attracting more and more attention within research activities in
advanced refractories across the world. This is due to its standing propertoiees, which
include mechanical strength, wear resistantance, heat conductivity, and thermal shock
resistance. These type of spesification offer these materials to be good candidate for
application involving severe working environment and different field of industries.
(Emad. 2004)

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CHAPTER III
METHODOLOGY

I.1 Flow Sheet

III.1.1. Aglomeration Process

Start

Preparation of material and equipment

Crushing / Screening lateritic nickel ores and charcoals

Sieving using 50 mesh standard sieve

Mixing with Na2SO4 with a mass ratio of 100 : 12 : 12 (Ore : charcoal : Na2SO4)

Mixing tapioca with water, then heating in boiling water

Adding the mixed tapioca with the mixture of ore, charcoal, and Na2SO4, then stirring

Molding the mixture into a pillow briquette

Measuring the briquettes

Drying the briquettes at 110⁰C for 3 hours

Measuring the dried briquettes then calculate the mass

change, and compare the mass homogenity

Measuring its bulk using Archimedes principle and calculating the pores

Testing the briquettes for fall strength using index test

Data analysis and discussion

Finish

Figure III. 1 Flow Sheet of Aglomeration Process

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III.1.2. Carbothermic Direct Reduction

Start

Preparation
Preparation of materials
of material and
and equipment
equipment

Inserting coal and 8gr limestone into

the crucible

Placement of crucible into the Muffle

Furnace

Preheating to 700⁰C in 60 minutes, then holding for 2

hours

Increasing to temperature of 1400⁰C in 60

minutes, then holding for 6 hours

Cooling for 12 hours inside the Muffle Furnace

Measuring the weight of reduction

briquette

Calculating the degree of

reduction

Data analysis and discussion

Conclusion

Finish

Figure III. 2 Flow Sheet of Carbothermic Direct Reduction

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III.2. Materials and Equipment

III.2.1. Aglomeration Process
III.2.1.1. Materials used
1. Materials used in this experiment are:
2. Lateritic nickel ore 100 g
3. Wood charcoal 30 g
4. Na2SO4 powder 30 g
5. Tapioca 6g
6. Aquades

III.2.1.2. Equipment used

Equipments used in this experiment are:
1. Compaction tools 1 set
2. Drying oven 1 set
3. Crusher 1 set
4. Screen with 50 mesh standard size 1 unit
5. Digital scales 1 unit
6. Measuring cup 1 unit

III.2.2. Carbothermic Direct Reduction

III.2.2.1. Material used
Materials used in this experiment are:
1. Nickel briquettes 1-4 pieces
2. Coals 20-70g
3. Limestone 10-45g
4. LPG

III.2.2.2. Equipment used

Equipments used in this experiment are:
1. Muffle Furnace 1 set
2. Crucible 1 set
3. Thermocouple 1 unit
4. Blower 1 set

III. 3 Practicum Procedures

III.3.1. Aglomeration Process
Procedure in this experiment are
1. Lateritic nickel ores and charcoals are crushed using crusher.
2. The lateritic nickel ores and charcoals are sieved using 50 mesh standars sieve.
3. The lateritic nickel ores out from the sieve are mixed with wood charcoals and
sodium sulphate (Na2SO4) with a mass ratio of 100 : 12 : 12 (ore : charcoal :
Na2SO4)
4. Tapioca mixed with water of 100 mL, and heated in boiling water until slightly
thickened.

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5. The mixture of lateritic nickel ores, wood charcoal, and Na2SO4 are added with
tapioca which has slightly thickened and stirred until evenly distributed.
6. The mixture is formed into a pillow briquette using a mold.
7. The existing mixture is molded with pillow shape with compaction device with a
pressure of 30 kgf/sm2. In one agglomeration process, it takes 1 piece of briquette.
8. Briquettes are measured in mass using digital scale.
9. Briquettes measured its bulk volume using the Archimedes principle.
10. The briquettes which have been compacted are then dried at 110⁰C for 3 hours using
the drying oven.
11. Briquettes are assessed from their shape visually to see if there are any cracks or
not.
12. The briquettes measured their mass after drying and calculated mass changes before
and after drying and compared the mass homogeneity between the four briquettes.
13. The briquettes after drying are measured its bulk volume using the Archimedes
principle and calculated the pores present in the briquettes.
14. Briquettes are tested for fall strength using a shatter index test. Briquette is placed
at a height of 2 meters. Briquettes are freely dropped from a height of 2 meters to a
steel plate. Briquettes are measured in size distribution (category 1: size <5 mm,
category 2: size 5-10 mm, and category 3: size >10 mm).

III.3.2. Carbothermic Direct Reduction

Procedure in this experiment are
1. The briquettes is inserted into the crucible which contains a mixture of coal and
limestone. The limestone used in the bed varies between groups according to the
table below:

Table 3.1 Varies the limestone used between groups

Group Limestone Mass

1 4g

2 6g

3 8g

4 10 g

5 12 g

6 14 g

7 16 g

And for group 3, the required limestone mass is 8 g.

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2. Crucible is placed in Muffle Teknologi
Furnace and Sepuluh Nopember
preheated to 700⁰C in 60 minutes. Then,
it was holded at temperature 700⁰C for 2 hours.
3. Temperature was increased to temperature of 1400⁰C in 60 minutes. Then, it was
holded at a temperature of 1400⁰C for 6 hours.
4. The briquette is cooled inside the Muffle Furnace for 12 hours.
5. The reduced briquette is removed from Muffle Furnace.
6. Reduction briquette is weighed.
7. Calculation of degree of reduction.

III. 4 Calculations
III.4.1. Aglomeration Process
Volume and density of briquette calculation
The briquette volume measurements were performed using Archimedes
principle. The aquadest is inserted into a measuring cup up to a size of 50 mL.
Then, briquettes are inserted into a measuring cup which has been filled with
distilled water. Once incorporated into water, the final volume is measured.
The change in volume is calculated using the equation below

ΔVol = Volfinal – Volinitial

. ........................................................ (3.1)
Volume change (ΔVol) in mL is a briquette volume.

Figure III. 3 Archimedes principle for volume calculations

Then, the density of briquette is calculated using equation below.

𝑚 𝑏𝑟𝑖𝑞𝑢𝑒𝑡𝑡𝑒
𝜌=
𝛥𝑉𝑜𝑙
........................................................... (3.2)
Then, for calculating the pores in briquettes, the calculation conducted using
below equation.

%Pores = ΔVol – Vol briquette appropriate to the mold

............. (3.3)

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III.4.2. Carbothermic Direct Reduction

The reduced briquettes then were cooled and were weighed to calculate the
reduction degree using equation below.
𝑂2 𝑟𝑒𝑚𝑜𝑣𝑒𝑑
%Degree of Reduction = 𝑥 100%
𝑂2 𝑖𝑛𝑖𝑡𝑖𝑎𝑙
.............. (3.4)

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CHAPTER IV
DATA ANALYSIS AND DISCUSSION

IV.1 Data Analysis

IV.1.1. Moisture Content
Table 4.1 Drying data
No Mass before drying Mass after drying Moisture (%)

25 gram 21 gram 16
1.

2. 28 gram 23 gram 17,857

Calculation of moisture content

Formula :
𝑚𝑎𝑠𝑠 𝑏𝑒𝑓𝑜𝑟𝑒 𝑑𝑟𝑦𝑖𝑛𝑔−𝑚𝑎𝑠𝑠 𝑎𝑓𝑡𝑒𝑟 𝑑𝑟𝑦𝑖𝑛𝑔
% moisture = x
𝑚𝑎𝑠𝑠 𝑏𝑒𝑓𝑜𝑟𝑒 𝑑𝑟𝑦𝑖𝑛𝑔
100% .................... (4.1)

Bricket 1
25−21
% moisture = x 100%
25
= 16 %
Bricket 2
28−23
% moisture = x 100%
28
= 17,857 %

IV.1.2. Degree of reduction

Table 4.2 Degree of reduction data
Degree of reduction
No Mass before DRI Mass after DRI LOI metal form

1. 23 gram 4 gram 44% Yes

Calculation of degree of reduction

Formula :
% 𝑑𝑒𝑔𝑟𝑒𝑒 𝑜𝑓 𝑟𝑒𝑑𝑢𝑐𝑡𝑖𝑜𝑛
𝑂₂ 𝑟𝑒𝑚𝑜𝑣𝑒𝑑
= 𝑥 100%
𝑂₂ 𝑖𝑛𝑖𝑡𝑖𝑎𝑙
......................... (4.2)

𝑚𝑎𝑠𝑠 𝑏𝑟𝑖𝑐𝑘𝑒𝑡 𝑎𝑓𝑡𝑒𝑟 𝑑𝑟𝑦𝑖𝑛𝑔 − (𝐿𝑂𝐼 𝑥 𝑚𝑎𝑠𝑠 𝑎𝑓𝑡𝑒𝑟 𝑑𝑟𝑦𝑖𝑛𝑔) − 𝑚𝑎𝑠𝑠𝑎 𝑙𝑜𝑔𝑎𝑚
= 𝑥 100%
𝐴𝑟 𝑂₂
𝑀𝑟 𝐹𝑒₂𝑂₃

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% wt Fe2O3 = 38,84%
% wt NiO = 2.03%
Mass after drying = 23 gram
Fe2O3 in briket = 38.83% x 23 = 8.93
NiO in briket = 2.03 x 23 = 0.47
𝐴𝑟 𝑂
Mass O in Fe2O3 = 𝑥 𝑚𝑎𝑠𝑠 Fe2O3
𝑀𝑟 Fe2O3
16
= 𝑥 8.93 = 0.893 𝑔𝑟𝑎𝑚
160
𝐴𝑟 𝑂
Mass O in NiO = 𝑥 𝑚𝑎𝑠𝑠 𝑁𝑖𝑂
𝑀𝑟 NiO
16
= 𝑥 0.47 = 0.1 𝑔𝑟𝑎𝑚
75

Mass O initial = mass O in Fe2O3 + mass O in NiO

= 0.893 + 0.1
= 0.993
Mass O loss = mass after drying – (LOI – mass after drying) – mass logam
= 23 – (44% x 23) – 4
= 8.88
8.88
%Degree of Reduction = = 8.94%
0.993
IV.2 Discussion
For this extractive metallurgy experiment session, we are doing two experiments. The
first, is agglomeration process. The objective of this experiment is to make a good
agglomerate both physically and mechanically to feed into direct reduction furnace. The
materials used are 100 g lateritic nickel ore, 30 g wood charcoal, 30 g Na2SO4 powder, 6
g tapioca, and aquades. While the equipment used are compaction tools, oven, crusher,
screen with 50 mesh standard size, digital scales, and measuring cup. The procedure is,
first we crushed the ore and charcoal, and sieved theme with 50 mesh standard sieve, then
mixed up with Na2SO4. After that, the mixture is added with tapioca and formed into
pillow briquette using compaction tools. Then, we measure the briquette’s weight before
drying, and after that the briquette is dried for 3 hours in oven. Then, we measure the
briquette’s weight after drying. The second experiment, is carbothermic direct reduction.
This experiment’s objective is to conduct a direct nickel lateritic reduction process to
increase the nickel content. The materials used are 1-4 pieces nickel briquettes, 20-70 gr
coals, 10-45 gr limestones, and LPG. While the equipment used is muffle furnace,
crucible, thermocouple, and blower. The procedure is, placing the briquette inside
crucible in muffle furnace, and it was reduced inside the furnace at temperature 1300-
1400oC. After that, the briquette is cooled inside the furnace, and them weighed to
calculate the reduction degree.
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Briquettes that we use are 2 samples with an initial weight of each 25g and 28g.
Following the drying process acquired the final mass of samples 1 and 2 with the weight
of each is 21 g and 23 g the weight decrease because of the moisture that contain in the
briquettes is evaporate. After the calculation of the percentage of moisture in a way that
reduces the initial mass with final mass divided by the initial mass multiplied by 100%.
From the calculations, sample 1 has a moisture percentage of 16% and sample 2 has a
moisture percentage of 17,857 %.
The degree of reduction influences the reaction process. The higher the degree of
reduction, the more oxygen is bound in the briquette that is released. Oxygen content, the
less oxygen content removed during agglomeration, the more efficient the process in the
Blast Furnace. This means that the higher the degree of reduction, the reaction will take
place quickly. The degree of reduction can be reduced due to the diffusion of carbon into
iron ore. The degree of reduction is affected by temperature and processing time. If the
temperature of the reduction is less than the actual temperature, the process of the
reduction process is slow and long. In this study of reduction the oxygen that bonded in
Fe2O3 and NiO will be break by the reduction then the oxygen make a bonding with
Carbon form carbondioxide, the degree of reduction shows us the amount of oxygen that
released from the fe2O3 and NiO bonds. So, in this experiment it shows 66,8% of total
oxygen is released.
(Mangarul Esaputra, 2014)
The beginning of direct reduction process is put the briquette into the crucible with
limestrone and cokes with certain composition (coke-limestone-briquette-limestone-
coke). Briquette that put into crucible furnace has 23 gram in mass. After that it is being
heated in crucible frunace with certain temperature. This process result is ferro-nickel
with 4 gram in mass and in the form of granule shape. This is the result of the direct
reduction process which does not make the metal molten first like the smelting process.
The process is just like the theory which explain that the direct reduction process is a
solid-state reaction process ( solid–solid or solid–gas reaction) in which removable
oxygen is removed from the ore, using coal or reformed natural gas as reductants, below
the melting and fusion point of the lump ore or agglomerates of fine ore. The external
shape of the ore remains unchanged. The transformation of metal through direct reduction
process consider as success procedure if the solid metal doesn’t through melt phase.

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TeknologiVSepuluh Nopember

CONCLUSION AND SUGGESTION

V.1 Conclusion
Based on the experiment that we have done, there are some conclusion such as:
1. The Process of carbothermic reduction of nickel
The process of carbothermic reduction is a reduction process that use carbon as a
reductor, based on the ellingham diagram the position of the carbon line against the
line of metal oxide formation, it can be seen the ability of carbon to reduce oxide to
metal. If the carbon line is below the oxide line, carbon can be used to reduce the
oxide to metal. So with this process the oxigen canbe separated from the metal.
3 Fe2O3 + C → 2 Fe3O4 + CO
NiO + C → Ni + CO
The ore crushing process consist of several step below,
a. Primary crushing
b. Secondary crushing
c. Terrtiary crushing
d. Grinding
2. The briquettes made process result is so depend on the every step that involved in
the process, such as the drying process, the moisture content, pressing and etc. The
Ni content tends to increase with increasing reduction process time. The higher the
addition of reducing agents, the higher the Ni and Fe content is.
One variable that greatly influences the results of the reduction process is the
reduction time. The longer the reduction process, the intensity of the peak metal
phase will also increase and the intensity of impurity will decrease.
3. Pillow form briquettes with the same volume have small miner thickness and a
larger surface area compared to the shape of the ball. This will increase the heat flux
during the heating process. Large heat fluxes will increase heat transfer so that the
reduction rate will also increase

V.2 Suggestion
Based on the experiment that we have done, there are some suggestion in order to create
a better experiment nex time, such as :
1. Precisely control the process temperature in order to create a good direct reduction
process and prevent the metal being melted.
2. Minimalize the heat loss in order to make the heat input more stable
3. Calculate and measure the composition precisely

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Hagemann, Nikolas et al. 2018. Activated Carbon, Biochar and Charcoal: Linkages and
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Direct Reduced Iron Experiment v

Laboratory of Minerals and Materials Processing Technology
2019