of mixed particle sizes and lumps which

Calcination of Limestone
disintegrate during the process. Calcination
Balacuit, Prince Joewen
can be carried out in a fluidized bed-
Vanguardia, Glory Janereactors for materials of small and uniform
Degamo, Jude Chesterparticle size.
Gardon, Sheila Mae
Lime has been used for building purposes
since prehistory,
METE 159N: Pyrometallurgical Engineering Laboratoryas exemplified by the
lime plaster floors.discovered at Palestina
ABSTRACT and Turkey, dated 12,000 years old.

This experiment was done to determine the effects of particle size and retention time on the rate of decomposition of
CaCO3 and to observe the microstructure before and after calcining. The experiment was done by preparing 15 g of
sample for each of the particle size 40, 80, 200 and 360 mesh and roasted in 800 0 C for 45 minutes. Another 4
samples are prepared with the same range of particle size but with a retention time of 60 minutes. After calcining,
the sample were weighed for the determination of the weight loss. Microstructure of each samples were taken by
using microscope before and after calcining. Data shows that with the decrease of particle size ther is an increase
of reactivity of the limestone. The microstructure taken at different magnification shows that raw sample has a white
granular grain and after it shows that the lime have been burned with the presence of black particles. After
calcining the structure are distorted with crack edges in the grains as a manifestation of calcination. It goes the
same for every particle size. The degree of distortion of the samples calcination run of 45 min to 60 min are similar.
It also shows that increasing the retention time decreases the surfaceToday,
which islime is usedby in
manifested theagriculture, food
increase of grain
size and pore size. processing, disinfecting and disease
control, water treatment, flue-gas
I. INTRODUCTION desulfurization, producing steel, plastic
Calcination is the thermal decomposition and glass, and sugar refining. For these
of solids by heating of solids to a high applications accurate control of
temperature typically done in the absence decomposition of calcium carbonate is
of air for the purpose of removing volatile necessary to achieve a high quality product
substances. It is widely used unit operation meeting certain properties. Numerous
in process metallurgy. factors are to be considered in calcination:
The decomposition of carbonates such as the characteristic of the limestone, particle
calcium carbonate or calcite (limestone) to size, shape of the particles, temperature
form lime AND Carbon Dioxide is a profile in the calcining zone and the rate of
typical example of calcination. The heat exchange between the gases and the
reaction is highly endothermic and particles.
consumes large amount of thermal energy.
II. OBJECTIVE OF THE STUDY
CaCO3 = CaO(s) + CO2(g) The objective of the experiment is to
conduct calcination of calcite in the muffle
In the calcination of limestone temperature furnace and compare the crystallographic
is adjusted to achieve desired product is orientation of the calcite of different
obtained. Soft burnt lime, which is more particle size analysis, prior and after the
porous, with a large surface area and thermal decomposition process of the
enhanced reactivity, is obtained by material.
calcining limestone at 750–850 °C.
Calcination at 1200–1300 °C results in a
less reactive product in which the particles III. SIGNIFICANCE OF THE STUDY
are found to have undergone sintering. The significance of the study is to
Three different types of furnaces are understand the calcination of lime and the
generally in use for calcination including factors that affects its properties
shaft furnaces, rotary kilns, and fluidized specifically the particle size, residence
bed reactors. Calcining coarse limestone time, grain size and pore size.
are conducted in Shaft Furnaces. Rotary
kilns type are used for handling materials IV. METHODOLOGY
Sample Preparation was achieved, it was hold at this
temperature for about 45-minutes to allow
Using analytical balance, 500 grams of
the sample to be calcined. After
limestone was weighed then placed in a
calcination, the muffle furnace was
basin and washed to remove foreign
stopped and cooled down. The crucibles
materials. It was soaked with tap water for
containing the calcined samples were
about 30-minutes and dried in the oven at
weighed. This procedure was repeated for
temperature of 110oC for 1 hour. Using the
1 hour calcination.
mortar and pestle, the dried limestone was
crushed. Then, the crushed limestone was Microstructure Analysis
sieved through a series of screens (40, 80,
A double-sided tape was placed on the
200 and 325 mesh sieves) to obtain about
glass slide. The raw sample was placed
50-g undersize of each of the four fraction
into it making sure that it covers the entire
sizes (-40, -80, -200 and -325-mesh). The
glass slide. It was then observed under the
limestone was dry sieved to obtain the -40-
microscope at different magnification. The
mesh sample while the undersize of 80-
procedure was repeated for the calcined
mesh was wet sieved to obtain the -80, -
product of the 45 and 60-minutes retention
200 and -325-mesh samples.
time.
Specific Gravity
The pycnometer with cover was washed V. RESULTS AND DISCUSSION
with water and dried using the blower. It
Table 1 – weight loss, grams
was later cooled down and weighed.
mesh Time, minutes
Approximately 3-g sample of -200 mesh
size 45 60
limestone was weighed and placed inside
-40 5.331 g 5.475 g
the pycnometer. The pycnometer was half- -80 5.601 g 5.577 g
filled with water to completely soak the -200 5.75 g 5.55 g
limestone and was carefully swirled to -325 5.812 g 5.462 g
ensure that no air bubbles were trapped. It
was then filled with water up to its brim
and covered, making sure that the capillary 5.9
of the cover was completely filled with 5.8
weight loss

water. The exterior surface of the 5.7

pycnometer was wiped and then it was 5.6
weighed. The pycnometer was then 5.5
5.4
emptied and cleaned thoroughly. The same
5.3
procedure was done but this time, only 0 100 200 300 400
with water. The pycnometer with water mesh size
was weighed and recorded. This procedure
was repeated for the three remaining 45 minutes 60 minutes
fraction sizes.
Figure 1 – weight loss of the calcined product
Calcination
First, four crucibles were weighed using
analytical balance. Then, four limestone
samples of different particle size (-40, -80,
-200 and -325-mesh) were obtained and
placed in the weighed crucibles. The
samples were then placed into the muffle
furnace and preheated for about 1 hour and
30 minutes or until the temperature reaches
at 800˚C. Once the desired temperature
Table 3 – Microstructure of raw and after 60 -
minutes of calcination
Raw ore 60 minutes at 800 0C

-200 mesh 10 x -200 mesh 20 x

-40 mesh 5x -40 mesh 5x

325 mesh 10x 325 mesh 5x

-80 mesh 20x -80 mesh 5x A. Effect of Particle Size

The effect of the particle size is shown in
table 1 and figure 1. This experiment was
conducted under 800 C for 45 and 60
minutes. The lime is being preheated at 800 C
since theoretically, calcium carbonate
thermally decomposes at 850 C.
-200 mesh 10x -200 mesh 10x CaCO3  CaO + CO2
∆G = 178,300 – 159.1T
The calcite was grinded and mechanically
sieved to 40, 80, 200 and 325 mesh. It is
shown that the weight loss increases as the
particle size decreases which follows the
-325 mesh 10x -325 mesh 20x theory that the diminution of particle sizes in
the same mass causes the overall surface area
of the particle to be larger. Since calcination
is highly endothermic it requires high
Table 2 – Microstructure of raw and after 45
enthalpy (178,300 J/mol) or thermal energy
minutes of calcination
hence as the surface area increases the
Raw Ore 45 minutes at 800 0C
diffusion of heat also increases thus more
particles reaches the activation energy needed
for the calcination of calcium carbonate
(calcite) also it increase the reactivity of the
lime. This behaviour is attributed to the
40
-40mesh 5x
mesh 5x 40
-40mesh
mesh5x
5x influence of heat and mass transfer effect.
A decrease of weight loss with residence time
x of 60 minutes was obtained from the
experiment. The factor of this error is
probably due to the impurities.

80 mesh
-80 mesh20
20x
x -80 mesh 20x
B. Effect of Retention Time
Observe in table 2 and 3 that the grains of the
sample are round and granular. The black
 granular particles are the burnt CaCO3 at the
surface.
At temperature 8000 C and retention time of
45 minutes, different particle size shows
different images under microscope due to
different magnification but nevertheless show
same granular or approximately spherical
shape of the grains in the raw ore. However,
after calcination run of 45 minutes the smooth
grains are distorted with crack edges and
signifies that the grains reacted with heat
inside the muffle furnace.
VII. REFERENCES
For table 3, sample show same structure of
raw ore but the end result after the calcination
run of 60 minutes under the same temperature
of 8000 C are nearly the same with the 45
minutes residence time. The end results show
some finer grains and distorted edges. Even
though it is expected that the more time the
sample heated inside the furnace the better the
reaction of limestone, as of this experiment
only 15 minutes is the interval from the two
run thus the product shares nearly the same
structure.
Increasing the retention time it is expected
that the grain size and porosity would
increase as time increases. Theoretically and
experimentally, calcining at higher
temperature slow nucleation rate occurs hence
coarse grains and large pore size are produced
but at a lower temperatures (below 900 C) the
nucleation rate is faster hence producing a
finer grain size but the data provided by the
experiment is not enough to explain the
crystalline growth with respect to temperature
but it can be compared with respect to time.
Increasing the residence time increases the
grain size and pore size hence with increasing
the residence time also increases the pore size
and grain size which decreases the surface
area. The reactivity of lime is inversly
proportional to the surface area of the
particleso with an increase of residence time
there is a decrease of reactivity.
VI. CONCLUSION
With decreasing particle size, the reactivity of
the lime increases and the activation energy
decreases. This behaviour is This behaviour is
attributed to the influence of heat and mass
transfer effect.
The residence time and temperature is directly
proportional with pore size and grain size
which implies that as pore and grain size
increases the surface area decrease. The
reactivity on the other hand is inversely
proportional with the surface area so as the
surface area increases with temperature and
residence time the reactivity also decrease.
Criado, J. M., & Ortega, A. (1992). A study of
the influence of particle size on the thermal
decomposition of CaCO3 by means of
constant rate thermal analysis.
Thermochimica Acta, 195, 163–167.
Valverde, J.M., Medina, S. (2015),
Crystallographic transformation of limestone
during calcination under CO2, Phys. Chem.
Chem. Phys., 2015, 17, 21912
Hughes J, Corrigan M (2009), Microstructural
expression of temperature and residence
time in laboratory calcined limestone, 12th
Euroseminar on Microscopy Applied to
Building Materials
Lime Calcination, G.S. Kumar, A.
Ramakrishnan, and Y.T. Hung. Handbook of
Environmental Engineering, Volume 5:
Advanced Physicochemical Treatment
Technologies. The Humana Press Inc.,
Totowa, NJ.
Wuladari W, et.al ,Performance of Dolomite
Calcination in a Bench-Scale Rotary Kiln,
Department of Chemical Engineering, Faculty
of Industrial Technology, Institut Teknologi
Bandung, Jalan Ganesa No.10 Bandung
40132, Indonesia 2