H I S T O R Y O F C E M E N T 1

1. Introduction to Cement
In the most general sense of the word, cement is a binder, a substance which sets
and hardens independently, and can bind other materials together. The name ʺcementʺ
goes back to the Romans who used the term ʺopus caementitiumʺ to describe masonry which
resembled concrete and was made from crushed rock with burnt lime as binder. The
volcanic ash and pulverized brick additives which were added to the burnt lime to obtain a
hydraulic binder were later referred to as cementum, cimentum, cäment and cement.
Cement or Portland cement, is the basic ingredient in concrete, as used in
construction industry, is a fine powder which when mixed with water and allowed to set
and harden can join different components or members together to give a mechanically
strong structure.

A view of “Pioneer Cement Limited” situted at Chenki at a distance of 40 Km from

Khushab and 34 Km from Jauharabad designed by F.L. Smidth of Denmark is used for cement
manufacturing.

Cement can also be defined as any substance which can join or unite two or more
pieces of some other substance together to form a unit mass. In this study only cements
used in construction industry will be discussed. Construction of houses for shelter is one of
the oldest industries in human civilization, and cement of one kind or another has been
used from prehistoric times for construction purposes. Lime and/or lime mixed with clay
matter, burnt or otherwise, have been used for bonding of bricks and stone masonry for at
least a millennium, and various theories have been propounded from time to time to
account for the setting and hardening properties of lime mortars. It will be too much for a
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work of this size to go into the details of these theories to show how cements of improved
properties have been developed. It was just 150 years ago that ‚Cement‛ as we know it
today was developed or invented. ‚Joseph Aspdin‛ of England first patented the
manufacturing of a very improved type of cementations material for building construction
in 1824, and named it ‚Portland Cement‛, because the hardened stone from his cement
resembled Portland stone found in England.
However, others also claim to have made similar cement earlier or later and contributed to
improvements in its properties. Each of them used a process of his own. It is only since the
end of the 19th century that the process of manufacture of Portland cement, as we know it
today, was adopted.

1.1, History Of Cement

Throughout history, cementing materials have played a vital role. They were
used widely in the ancient world. The Egyptians used calcined gypsum as a cement.
The Greeks and Romans used lime made by heating limestone and added sand to make
mortar, with coarser stones for concrete.

The Romans found that a cement could be made which set under water and this
was used for the construction of harbours. The cement was made by adding crushed
volcanic ash to lime and was later called a ‘pozzolanic’ cement, named after the village
of Pozzuoli near Vesuvius.

In places such as Britain, where volcanic ash was scarce, crushed brick or tile was
used instead. The Romans were therefore the first to manipulate the properties of
cementitious materials for specific applications and situations.

Hadrian's Wall, England, a few miles east of Housesteads.

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Marcus Vitruvius Pollio, a Roman architect and engineer in the 1st century BC
wrote his "Ten books of Architecture" - a revealing historical insight into ancient
technology. Writing about concrete floors, for example:

"First I shall begin with the concrete flooring, which is the most important of the polished
finishings, observing that great pains and the utmost precaution must be taken to ensure its
durability".

"On this, lay the nucleus, consisting of pounded tile mixed with lime in the proportions
of three parts to one, and forming a layer not less than six digits thick."

And on pozzolana:

"There is also a kind of powder from which natural causes produces astonishing results.
This substance, when mixed with lime and rubble, not only lends strength to buildings of other
kinds, but even when piers are constructed of it in the sea, they set hard under water."

(Vitruvius, "The Ten Books of Architecture," Dover Publications, 1960.)

His "Ten books of Architecture" are a real historical gem bringing together
history and technology. Anyone wishing to follow his instructions might first need to
find a thousand or so slaves to dig, saw, pound and polish...

After the Romans, there was a general loss in building skills in Europe,
particularly with regard to cement. Mortars hardened mainly by carbonation of lime, a
slow process. The use of pozzolana was rediscovered in the late Middle Ages.

The great mediaeval cathedrals, such as Durham, Lincoln and Rochester in

England and Chartres and Rheims in France, were clearly built by highly skilled
masons. Despite this, it would probably be fair to say they did not have the technology
to manipulate the properties of cementitious materials in the way the Romans had done
a thousand years earlier.

The Renaissance and Age of Enlightenment brought new ways of thinking,

which for better or worse, led to the industrial revolution. In eighteenth century Britain,
the interests of industry and empire coincided, with the need to build lighthouses on
exposed rocks to prevent shipping losses. The constant loss of merchant ships and
warships drove cement technology forwards.

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Smeaton, building the third Eddystone lighthouse (1759) off the coast of
Cornwall in Southwestern England, found that a mix of lime, clay and crushed slag
from iron-making produced a mortar which hardened under water. Joseph Aspdin took
out a patent in 1824 for "Portland Cement," a material he produced by firing finely-
ground clay and limestone until the limestone was calcined. He called it Portland
Cement because the concrete made from it looked like Portland stone, a widely-used
building stone in England.

While Aspdin is usually regarded as the inventor of Portland cement, Aspdin's

cement was not produced at a high-enough temperature to be the real forerunner of
modern Portland Cement. Nevertheless, his was a major innovation and subsequent
progress could be viewed as mere development.

A ship carrying barrels of Aspdin's cement sank off the Isle of Sheppey in Kent,
England, and the barrels of set cement, minus the wooden staves, were later
incorporated into a pub in Sheerness and are still there now.

A few years later, in 1845, Isaac Johnson made the first modern Portland Cement
by firing a mixture of chalk and clay at much higher temperatures, similar to those used
today. At these temperatures (1400C-1500C), clinkering occurs and minerals form which
are very reactive and more strongly cementitious.

While Johnson used the same materials to make Portland cement as we use now,
three important developments in the manufacturing process lead to modern Portland
cement:

Development of rotary kilns

Addition of gypsum to control setting

Use of ball mills to grind clinker and raw materials

Rotary kilns gradually replaced the original vertical shaft kilns used for making
lime from the 1890s. Rotary kilns heat the clinker mainly by radiative heat transfer and
this is more efficient at higher temperatures, enabling higher burning temperatures to
be achieved. Also, because the clinker is constantly moving within the kiln, a fairly
uniform clinkering temperature is achieved in the hottest part of the kiln, the burning
zone.

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The two other principal technical developments, gypsum addition to control

setting and the use of ball mills to grind the clinker, were also introduced at around the
end of the 19th century.

1.2- Types of Portland Cement

The cements coming under the category of Portland cements are also known as
‚Hydraulic Cements‛, because they, when mixed with water, have the property of
setting and hardening under water. Hydraulic calcium silicate possesses the ability to
harden without drying or by reaction with atmospheric carbon dioxide. The reactions
involved in the hardening of cement are hydration and hydrolysis. There are various
types of Hydraulic Cements or Portland cements, a brief description of which is given
below (these five types are also mention in
ASTM):Type-I: Regular Portland Cements (or Ordinary Portland Cement
OPC) are the usual products for general construction. This type of cement develops
enough compressive strength at 3 days,7 days & 28 days to be suitable for all types of
modern civil engineering constructions. There are other types of this cement, such as
white, which contains less ferric oxide, oil-well cement, quick- setting cement, and
others for special uses. As all these classes particularly have the same method of
manufacturing; they vary only in chemical composition to impart the desired properties
of a particular type

Type-II: Portland cement, when mixed with water and allowed to hydrate,
generate considerable heat which is not desirable for mass concrete work; thus all ordinary
portland cements are not suitable for mass concrete work. By changing the chemical
composition of the cement somewhat, the heat of hydration can be lowered, and this type
of the cement is called Moderate –Heat-of-Hardening, this Portland Cement is of use where
moderate heat of hydration is required or for general concrete construction exposed to
moderate sulfate action. This type of cement is also some what more Sulphate resistant
than OPC. The heat evolved from these cements should not exceed 295-335J/g after 7 and
days, respectively.

Type-III: as said in Type-I above, ordinary portland cement develops the

desired strength at 3 days, 7 days, 28 days; but sometimes a cement is required which
should gives as high a strength in 24 hours as is required as is gives by Ordinary Portland

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at 3 days; this type of cement is called High- early strength (HES) cements (or Rapid-
Hardening Cement). It must not be confused with Quick Setting Portland Cement, say,
within a few minutes, but the ultimate strengths attained are not higher. The setting time of
Rapid Hardening Cement is the same as that of ordinary portland cements. These are made
from raw materials with a lime-to-silicate ratio higher than that of Type-I and are ground
finer than Type-I cements. They contain a higher proportion of tricalcium silicate (C 3S).
This, with the finer grinding, causes quicker hardening and a faster evolution of heat.
Roads construction from HES cement can be put into service sooner than roads
construction from regular cement.

Type-IV: Low Heat Portland Cements (LHPC); As all the above three types of
cement have fairly high heat of hydration. For larger mass concrete work in dams, piers,
etc., it is necessary to have a much lower heat of hydration, so that chances of developing
construction cracks later are minimized. This can be done by either adding some
pozzolanic material or granulated blast furnace slag to the cement while girding or by
changing its chemical composition of the cement in such a way that the heat of hydration is
reduced.

LHPC contains a lower %age of C3S and tricalcium aluminate (C3A), thus lowering
the heat evolution. Consequently, the %age of tetra calcium aluminoferrite (C 4AF) is
increased because of the addition of Fe2O3 to reduce the amount of C3A. Actually, the heat
evolved should not exceed 250-295J/g after 7 and 28 days, respectively, and is 25-35% less
than the heat of hydration of regular or HES cements. Thus the chemical composition of
Low Heat Portland Cement is so modified as to give a heat of hydration lower than the
maximum specified.

Type-V: concretes and construction made with all the types of Portland
cement described above deteriorate in strength to some degree on prolonged contact with
soils and water rich in Sulphates. Studies have been made to find out the cause of such
deterioration and it has been established that when the cement used has more than 5%
tricalcium aluminate (C3A), the cement is prone to deterioration under sulphatic
environment. Thus, a portland cement with less than 5% C3A & high content in C3AF is
highly resistant to sulphatic action and is known as Sulphate resisting cement. Sulfate-
Resistant Portland Cements are those which are those which, by their composition or
processing, resist sulfates better than other four previous types. So this Type-V is used
when a high sulfate resistance is required.

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Along with these types there are also some others specials cements as Oil-Well
Cement, White Cement, Blended Portland Cements (like Portland Blast Furnace Slag
Cement, Portland, and Masonry Cement etc.) and Special Cements have very special
properties and uses like Expansive Cement or Shrinkage Compensated Cement,
Superhigh-Strength Cement, and Alinite Cement (a special low energy cement process has
been developed in which more than 5% calcium chloride is added to the raw mix while
grinding.) and a special High C2S cement. All the above types of cement are covered by
stringent ‚standard specifications‛ and the product must conform to all the clauses in
every respect.

2. Chemistry of Raw Materials

Cement is a manufactured product made by blending different raw materials and
firing them at a high temperature in order to achieve precise chemical proportions of lime,
silica, alumina and iron in the finished product, known as cement clinker. Cement is
therefore essentially a mixture of calcium silicates and smaller amounts of calcium
aluminates that react with water and cause the cement to set.

Mainly two types of raw materials are necessary for the production of Portland cement:

one that is rich in calcium (calcareous) such as lime stone, chalk, Marl, sea-shell and
sand etc., and
One rich in silica (argillaceous) such as clay, Shale, Laterite, Bauxite, Sandstone etc.
Formerly a large amount of cement was made from argillaceous limestone, known as
Cement Rock founded at different places. In addition to natural materials, some plants use
blast-furnace slag and precipitated calcium carbonate obtained as a by-product in the alkali
and synthetic ammonium sulfate industry.

Finished cement is produced by finely grinding together around 95% cement clinker with 5%
gypsum (or anhydrite) which helps to retard the setting time of the cement.

Lime stone (As a source of CaO component )

Clay

Sand

Iron ore (As Ferric Oxide Source)

Gypsum (CaSO4.2H2O) (As an additive for OPC)

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Auxiliary Components (as impurities like excessive alkalis (Na2O, K2O, MgO, SO3 (or
Sulfur), Chloride, Fluoride, P2O5, Mn2O3)).

2.1- Limestone (Calcareous Material):

Limestone is the most common form of calcium carbonate and is used extensively
for the manufacturing of cement. Limestone is one of the most abundant materials in
nature. It is the rock formed under extreme pressure. Calcium carbonate of all geological
formations qualifies for the production of Portland cement.

Fig: Limestone
The requirement for calcium is met by using high calcium limestone (or its equivalent
calcareous raw material), and the limestone which is use normally found in Pakistan it is the
main raw material and there is no record of any cement industry in Pakistan that is using
other calcareous raw material. Limestone is very hard and Sio2, Al2O3, Fe2O3, CaO, MgO,
k2O, Na2O and So3 are present in it. And the percentage of calcium oxide is round about
50% in it.

Magnesium carbonate, which may be present in limestone, is the main undesirable

impurity. The level of magnesia (MgO) in the clinker should not exceed 5% and many
producers favour a maximum of 2% as also in accordance with the Pakistani environment;
this rules out dolomite or dolomitic limestones for cement manufacture.
Table-1 Calcareous Raw Materials
Components Limestone % Sea-Sand % Sea-Shell % Marl % By-Product (I) % Sludge (II) %

SiO2 1-15 1-10 0.5-2 10-20 2-4 2-1

Al2O3 1-6 1-3 0.5-1 2-6 1-2 1-2

Fe2O3 0.2-5 0.5-2 0.1-0.5 1-5 1-2 1-2

CaO 40-55 45-55 53-55 35-45 50-53 46-52

MgO 0.2-4 0.2-2 0.5-1 1-4 0.2-1 1-2

Alkali’s 0.2-1 1-1.5 0.3-0.5 0.5-1 1-3 0.5-1

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Chlorides (Cl) Tr.-0.1 1-2 0.2-0.5 Tr. Tr. Tr.

Sulphates (SO3) Tr.-3 0.5-1 0.1-0.3 Tr. Tr. 1-4

L.O.I. 35-44 38-44 42-45 30-38 40-45 40-43

2.2- Clay (Argillaceous Material):

The only argillaceous portion of the raw mix in Pakistan is clay. Clay is a sediment of
the same origin and nature as sand but more fine-grained, with particles size less then 2
microns. Clay contains a high proportion of alumna because the heavier silicates are
deposited during migration. Clayey raw material accounts for between 15–25%, although
the precise amounts will vary. Some times small proportions of iron ore, bauxite or
sandstone are also added to bring the silica modulus of the raw mix to a desired range.
Table-2 Argillaceous Raw Materials
Components Clay % Shale % Laterite % Bauxite % Iron-Ore % Sandstone %

SiO2 40-70 40-80 10-30 5-15 5-10 85-95

Al2O3 15-30 15-30 20-40 40-54 2-5 2-5

Fe2O3 3-10 3-10 20-40 2-10 85-95 1-3

CaO 1-10 1-10 2-4 2-4 Tr. 1-3

MgO 1-5 1-5 1-2 1-2 Tr. 1-3

Alkali’s 1-4 1-4 Tr. Tr. Tr. 1-2

Chlorides (Cl) Tr. Tr. Tr. Tr. Tr. Tr.

Sulphates (SO3) Tr.-2 Tr.-2 Tr. Tr. Tr. Tr.

L.O.I. 5-15 2-5 15-25 20-30 0-5 2-5

TiO2 ----- ----- 2.-5 2-6 ---- -----

In Pakistan, it is also acquired from the quarry and some-times due to presence of some
lime stone and lumps in this clay it is also crushed. Clay is transported to the crusher with
the help of dump trucks.

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2.3- Corrective Ingredients (Additives):

The above mentioned materials along with small amounts of other materials called
corrective or supplementary materials like bauxite, iron ore, mill scale, laterite, pyrite
cinder, and quartz are used to make up the lacking constituent in the final mix.

If an essential chemical component needed in the cement raw mixture is not present
in the required amount, corrective ingredients are use as additives. Thus e.g. for the
completion of the silica content, sand, high silica clay, diatomic, etc., are used as additives
or correctives ingredients. To compensate for deficiency in iron oxide, such s corrective
materials as pyrite cinders, iron ore, etc., are applied.

2.3.1- IRON ORE:

Iron occurs abundantly in several minerals mainly in the form of oxide, carbonate
and sulphide. Iron ores occur in igneous, metamorphic or sedimentary rocks or as
weathering products of various primary iron-bearing materials. It is also not always used
in raw materials but added in It (clay, limestone) when needed. Iron ore some times along
with Sand & waste bauxite, are used in small amounts to adjust the composition of the mix.

Fig; Iron ore Fig; Gypsum

2.3.2- GYPSUM:
Gypsum (CaSO4.2H2O) o its derivatives

Hemihydrate (CaSO4.1/2H2O)

Anhydrite (CaSO4)

Gypsum (4 to 5%) is mixed or crushed with the clinker in the last stages of cement
manufacturing to regulate the setting time of cement.

Most types of Portland cement clinker when ground alone and then mixed with
water, will set immediately; (flash set); this is not desirable, the initial set should not occur
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in less than 30 minutes or so. For retardation of the ‚setting time‛ gypsum is universally
used; thus, gypsum also has to be considered as a raw material. The purer the gypsum the
better it is as a retarder.

Gypsum or its derivatives is used in the slurry or raw mix to adjust the Sulphate
content for sulphatisation of alkali oxides or for modification of the C 3A phase to produce
calcium sulpho-aluminate which is an important constituent of certain types of expansive
cements.

Naturally occurring gypsum and that available as a by-product in various chemical

industries is used for the above purposes besides inter- grinding with clinker.

2.4- Fluxes & Mineralizers:

These are minor components added to the raw mix in a very small quantity. Fluxes like
iron oxide lower the temperature at which liquid phase appears whereas mineralizers
accelerate the rate of clinkerization. Calcium fluoride (fluorspar, CaF2) is considered the most
effective mineralizer. It lowers the temperature at which the liquid is formed by about 120°C
and it reduces both the sintering temperature and the free lime content. CaF 2 is normally used
in the manufacturing of white cement clinker. When using it, rapid cooling is desired to
prevent decomposition of the cement compounds.
There is no restriction in using mineralizers in cement industry as long as their presence
does not affect the setting, hardening, expansion, and other properties of the cement. The
following materials are also considered as fluxes and mineralizers;

Calcium Fluoride (CaF2)

Sodium Fluoride (NaF)
Calcium Fluosilicate (CaSiF6.6H2O)
Boric acid (B2O3)
Zinc Oxide (ZnO)
Cryolite (Na3AlF6)

Mineralizers very commonly used are CaF2 and CaSO4, or as mixture of two. Fluorides
of alkali and alkaline earth metals and Fluosilicate are also being used. It has been experienced
that by adding calcium Sulphate in the raw meal, the clinker produced has been higher
porosity which improves its grindability.

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2.5. Auxiliary Components:

Other deleterious materials include excessive alkalis (Na2O or soda, K2O, MgO & SO3)
which would be unacceptable because of durability problems with the concrete (due to the
reaction of alkalis with some siliceous aggregates to form a swelling gel (a jelly-like substance
that increases in volume with adverse effects on cement durability and strength).
2.5.1- ALKALIES:
Na2O and K2O originate from the raw materials as clay and marl, where these
compounds are present in fine dispersed feldspar, mica, and illite particles, and to a small
amount- when using coal as a fuel- from the coal ash. During the burning process in the rotary
kiln, parts of the alkalies evaporate in the burning zone, causing the so called alkali circulation.
Certain concrete aggregates, appearing in different areas around the world (like in USA,
Denmark, & Northern Germany) containing alkali sensitive components (hydrated silica),
reacting with the alkalies of the cement, which under certain unfavorable conditions can result
in an expansion phenomena (alkali expansion). As is known from experience, alkali expansion
can be prevented when using cement with low alkali content; in this case the total alkali
should not exceed 0.6-1% by weight with reference to restrictions applied in different
countries.
2.5.2- MAGNESIUM OXIDE:

The magnesium oxide combined up to 2% by weight the main clinker phases; beyond that
amount it appears in the clinker as free MgO, which with water as (MgO + H2O == Mg(OH)2)
to give Mg(OH)2 but this reaction proceeds slowly, while the other hardening reactions are
already concluded. Since the Mg (OH)2 occupies a larger volume than the MgO and is formed
on the same spot where the MgO particles are located, it can split apart the binding of the
hardened cement paste, resulting in the cement, if present in sufficient quantities will cause the
possibility of delayed expansion (expansion cracks or magnesia expansion) upon hydration &
also an unsoundness in the concrete.

2.5.3- SULFUR:

Sulfur appears predominantly as sulfide (pyrites & mareasite, FeS 3) in almost all cement
raw materials. The sulfur contents in fuel vary in wide limits, from zero in natural gas, to
about 3.5% in heavy fuel oil. Coal shows an average 1.1%. Investigations at different preheater
kilns showed that the amount of sulfur introduced with the raw mix in the range from 0.5-11
grams SO3/kg clinker, and the sulfur introduced with fuel, when using extremely high sulfur
fuel oil, showed a maximum of 6 grams SO3/kg clinker.

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As a result of the combustion, the sulfur of the raw mix and of the fuel evaporates in the
burning zone to SO2, which in kiln atmosphere combines with alkali and oxygen, generating
vaporized alkali sulfate, which condenses on raw mix particles in colder kiln zones as well as
in the preheater. With the exception of a small part which is carried away by the kiln dust, the
alkali sulfate returns with the kiln feed into the burning zone, and due to its low volatility
leaves the kiln with the clinker. If the SO2-content is insufficient to combine all alkalies, the
circulation of the medium volatile alkali carbonates or of the high volatile alkali chlorides
begins. So far as the alkali carbonates are not bound by the clinker phases, then evaporates
again in the burning zone.
In the preheater, an excess of SO2 is able to react with the CaCO3, and to return to the
kiln as CaSO4. Then in the burning zone, it decomposes again and thus increases the SO3-
circulationof the kiln gas. However, a certain part will appear in the clinker as undecomposed
CaSO4. The presence of alkalies in the raw mix in excess of the amount which is already
combined by the sulfur contained in the raw mix, allows the uses of high sulfur fuels without
emitting noteworthy quantities of SO2 by the kiln exit gases. The alkali sulfate combined by the
clinker of advantage for the early strength of the cement. On the other hand, higher sulfur
contents can result in increased SO2 emission with the exit gases, choking of suspension preheater,
as well as formation of kiln coating rings.

2.5.4- OTHERS:

Chloride, Fluoride, P2O5, TiO2 and Mn2O3 is all present in very small quantities in some
lime stones. If any of these impurities are present, great caution must be taken in selecting
such limestones as raw materials; it may be better to avoid them. Some of the impurities
present in the raw materials are harmful either to the burning or to the quality of the resultant
cement. It is very difficult to dissociate and drive of the SO3 present and sometimes
carbonaceous material may be added to help the dissociation.
The presence of P2O5 to the extent of more than 0.5% in raw mix is also very low early
strength. Similarly, the presences of fluorine to the extent of about 0.5% may be helpful as a
flux, but higher proportions tend to eat away the refractory lining of the kiln and increase
balling action in the kiln. More than about 05% of Mn2O3 in a raw mix is also undesirable; it
makes the colour of the cement very dark and affects the early strength of the cement
somewhat. Presence of TiO2 in some bauxite or laterite used as corrective material, generally
acts in the same way as silica, & it’s presences is cement is harmful in any way.
Note:” Thus, it will be seen that great care has to be taken in selecting the raw materials
for the manufacturing of cement. So there are four distinct processes of burning cement
as clinker (a) Wet, (b) Dry, (c) Semi-Wet, (d) Semi-Dry. Selection of one process or
another would sometime depend on the physical condition in which the raw materials
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are available and sometimes on the chemical composition. For example, it is easier to
grind sea-sand and coral reef in a wet condition than in a dry condition, so the wet
process has to be selected while using sea-sand, or coral reef; similarly, by-product
sludge cannot be dried conveniently and so again wet process has to be selected while
using by-product sludge.”

2.6 Impurities Of Raw Material:

Free silica Causes;
o High wear in crusher & grinding mills
o Fuel consumption increase.
o Raw meal should not contain more than 3% free silica
Raw material containing phosphate, lead and zinc and their compounds should
be avoided.
Alkali metals ( Na, K ) are present in excess quantities, causes problems because
they form volatile salts in the kiln system. These evaporate in the burning zone &
recondense in the cooler regions of the preheater, causing blockages.
If magnesia present in excessive amount in clinker, produce long term
unsoundness in the cement.
If sulfur present in excess amount causes build-up. Excess sulfur limits the
addition of gypsum in cement which may cause setting problem.
Chlorine produce very volatile slats which cause preheater blockages ( below
0.1% in raw mix

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