DEWAS & PITHAMPUR (M.

P)
VOCATIONAL TRAINING REPORT
ON
PRODUCTION PROCESS OF RANEY NICKEL & OTHER CHEMICALS

Submitted to: Submitted by:

HARDIK JAIN
(Chief Manager H.R.D.) CHEMICAL ENGINEERING
I.P.S. INDORE (M.P.)
 VISION

“To be the leader in manufacture and distribution of Raney Nickel Catalyst and allied products”

MISSION

“A dynamic organization committed to serve the scientific community and other

customers to their total satisfaction through timely & perfect quality supply of Catalysts
and other products.”

ACKNOWLEDGEMENT

I take this opportunity to express my gratitude towards all the persons who were deeply
involved in my training period.
During this period guidance and valuable information which was given by my guide was
remarkable and will be fruitful in my future days.
I am also obliged to staff members of production department for their cordial support.
Lastly, I thank to my parents without their trust and support this assignment would not be
possible.
I am proud to express my sincere thanks to Mr. D. C. Jain(Director) for facilitating me during the
training.
I specially thanks to Mr. Mohit Jain(senior manager)

ABSTRACT
In this report, we discuss about all the technical aspects which we are getting during our
training duration at Namokar Speciality Chemicals Pvt. Ltd.
This report revolves around Nickel catalysts, alloy production & Other chemicals, their
applications of and all the technical details related to them.
Industrial training is one of the most vital part of syllabus of chemical engineering, which is not
only teaches about industrial operations, the equipments and other technical aspects but also
teaches discipline, interaction with various people on the field and importance of team work.
It develop an awareness of industrial approach to problem solving, based on broad
understanding of process and mode of operation of organization.
 COMPANY PROFILE
Namokar Speciality Chemicals Private Limited an ISO 9001:2008 certified company a registered
MSME unit established in 1992, is engaged in manufacturing of the following:

1. Raney Nickel Catalyst (for bulk drug and pharmaceutical companies)

2. Raney Copper Catalyst
3. Nickel & Aluminium Alloys & Alloy Powder
4. Nickel powder
5. Sodium Aluminate Solution (Caustic Lye)
6. Ferrous Sulphate

other allied products.

MANUFACTURING PLANTS
Namokar has two units:-
1. Dewas (M.P.) – Raney Nickel Catalyst, Ni-Al Alloys, Ni Powders
2. Pithampur (M.P.) – Bulk Drugs, Intermediates and Fine Chemicals
Clients:

1. Cadila Pharmaceutical,
Ankleshwar
2. Vijayasri Organics Ltd,
Hyderabad
3. High Rise Chemicals,
Taloja
4. Jubilant Organosys,
Mysore
5. The Sukhjit Starch Ltd,
Phagwara
6. Glenmark Generics
Ltd, Ankleshwar
7. Tagros Chemicals
India Ltd, Chennai
8. Natco Pharma Ltd,
Hyderabad
9. Divis Laboratories Ltd,
Hyderabad
10. Ind-Swift Laboratories Ltd
Chandigarh

PRODUCTION & SUPPORT FACILITIES

The plant is provided with excellent manufacturing setup. It includes various reactors and associated
infrastructure, well equipped for its products processing. The engineering section has support facilities
like D.M. water plant, RO Plant, two-stage evaporating unit, D.G. boiler and modern office automation
system, training facilities, etc. . Fully Equipped Laboratory is also there to test the qualities of the
finished products.

RANEY NICKEL CATALYST

Product Overview :

Raney Nickel catalyst was developed in 1926 by American engineer Murray Raney as an alternative
catalyst for the hydrogenation of vegetable oils in industrial processes. More recently it is used as a
heterogeneous catalyst in a variety of organic synthesis, most commonly for hydrogenation reaction.
Raney Nickel is produced when Nickel aluminium alloy is treated with concentrated Sodium Hydroxide.
This treatment, called "activation", dissolves most of the aluminium out of the alloy. The porous
structure left behind has a large surface area, which gives high catalytic activity.
The more general term is "skeletal catalyst" or "sponge-metal catalyst" may be used to refer to catalysts
that have physical and chemical properties similar to those of Raney Nickel.

Raney Nickel is used in a large number of industrial processes and in organic synthesis because of its
stability and high catalytic activity at room temperature.

Process

The formation of nickel-aluminium alloy at a certain ratio takes place in this furnace. The
working of this induction furnace is based on the concept of eddy currents so the temperature
of 1400 degrees centigrade is achieved 70 volts only. The alloy from furnace is spread to cool it
under room temperature and solidify. These cold pieces are the send to grinding section.

In Grinding section large plates of Al-Ni alloy are fed to jaw crusher, and further grinding is done
in pulverizer to get particle size of around 200 mesh. The pulverizer is attached with a cyclone
separator to discard unwanted particles. After which the particles are screened to get a fine
powder,and the large particles are recycled to pulverizer.

The powdered alloy is treated with concentrated solution of sodium hydroxide in batch
reactors.

2Al + 2NaOH + 6H2O → 2Na[Al(OH)4] + 3H2

According to the reaction mentioned sodium aluminate is formed along with release of
hydrogen gas, leaving behind nickel in an activated state. This activated nickel settles down at
the bottom of reactor. This is the Raney Nickel Catalyst. To prevent its oxidation, its stored as
slurry with demineralized oxygen free water.

The solution of sodium aluminate is sent to evaporation unit. The unit has a Multi-Effect
evaporator working on steam. From here concentrated solution of sodium aluminate is
obtained. The Byproducts of the process like Nickel powder, Ni-Al alloy powder, sodium
aluminate, hydrogen is sold to other industries.
RANEY COPPER CATALYST
Activation of alloy to Raney copper catalyst, needs a change only in reactor section

To activate a 50:50 copper aluminum alloy is performed using a semi-batch fixed bed reactor
constructed from three-fourth inch outside diameter, 20 BWG tubing. The reactor is provided
with a nitrogen purge inlet, a burette for caustic addition, a Circulation of the leaching solution
is accomplished by using an agitator. After the alloy is placed in the basket mounted in the
reactor flask, 6 gms of deionized water per gram of alloy is added to the reactor and the
agitator is set for about 120 r.p.m. Heating to a reaction temperature of 105 F. is undertaken
concurrently with a 30 minute nitrogen purge. When the flask reaches 105 F. and the 3 purge is
completed, a 50 weight percent sodium hydroxide solution is added continuously over a 380
minute period to the system until 3.022 kg of sodium hydroxide per kg of alloy have added,
while control ling the temperature within 2 F. with external cool ling. The hydrogen evolution
rate averages 0.0041 moles hydrogen per mole aluminum initially in the alloy particles per
minute during the sodium hydroxide addition period. The hydrogen evolution rate
subsequently de creases to a low level as conversion of aluminum approaches 80%. After
completing addition of sodium hydroxide, the reaction is continued until an estimated amount
of about 80 to 90 weight percent of the total aluminum present in the starting alloy has been
leached. The reaction rate is monitored by measuring hydrogen evolution every 15 to 30
minutes. Thereafter, the product catalyst is immediately removed from the leaching solution
and placed into a large excess of deionized water. The product catalyst is rinsed with deionized
water until the pH of the rinse water approaches 7.0 after which the product catalyst is stored
under deionized water to prevent oxidation thereof.

Ferrous Sulphate - Iron(II) sulfate or ferrous sulfate denotes a range of salts with the
formula FeSO4·xH2O. These compounds exist most commonly as the heptahydrate (x = 7) but
are known for several values of x. The hydrated form is used medically to treat iron deficiency,
and also for industrial applications. Known since ancient times as copperas and as green
vitriol (vitriol is an archaic name for sulfate), the blue-green heptahydrate (hydrate with 7
molecules of water) is the most common form of this material. All the iron(II) sulfates dissolve
in water to give the same aquo complex [Fe(H2O)6]2+, which has octahedral molecular
geometry and is paramagnetic. The name copperas dates from times when the copper(II)
sulfate was known as blue copperas, and perhaps in analogy, iron(II) and zinc sulfate were
known respectively as green and white copperas.
FERROUS SULPHATE PRODUCTION PROCESS
Stage 1 - Solid iron in the form of scrap steel is continuously fed as small fragments via a belt
into a feed chute which discharged into a first reaction vessel. Dry ferric compounds (ferric
oxide or ferric sulphate) are added to the conveying system in a controlled manner to produce
a consistent blend of iron compounds feeding the reaction. An aqueous solution of about 35%
wt/wt sulphuric acid is provided in a first circulation tank and circulated into the reaction vessel
in order to contact the acid with the iron. Stoichiometric amounts of acid is added, with about
300 m/hr of the acid being circulated around about 2 tonnes of Scrap steel. The process liquor
is circulated around the reaction vessel from the circulation tank using high capacity pumps,
and fed through a distribution plate at the bottom of the reaction vessel to produce a fluidised
bed of iron/iron compound particles within the reaction vessel, allowing the reaction to take
place between the iron and Sulphuric acid. The liquor is then returned to the circulation tank.
The liquid in the reaction vessel was agitated to allow the hydrogen evolved from the process
to separate from the liquid in the reaction vessel. The hydrogen is then collected under partial
vacuum. The temperature in the vessels is controlled to be from 50° C to 70° C.

Stage 2 - The liquor from the circulation tank of the first stage is passed into the circulation tank
of the second stage. It is then circulated into a second reaction vessel where it is contacted with
ferric ions, provided by the addition of a low-grade dry ferric product. The temperature in the
vessel is controlled to be from 50° C to 70° C . Once a low acid strength aqueous solution
(between 0% & 20% (wt/wt) sulphuric acid) is obtained, the liquor is an acidic ferrous Sulphate
solution that could be used in the next stage.

Stage 3 - The acidic ferrous sulphate solution is filtered using a vibrating sieve to remove
detritus & unreacted Solid material. The filtered ferrous sulphate solution is then transported,
using an export pump, to the next stage of the process.

Stage 4 - The filtered, slightly acidic, ferrous sulphate solution is combined with a stream of
concentrated Sulphuric acid (from 95 to 98 (wt/wt) in a mixing tank. The temperature before
the acidic ferrous sulphate solution is combined with the concentrated sulphuric acid is in the
range of 60 to 80° C. The acidic ferrous sulphate solution is combined with the concentrated
Sulphuric acid to give a concentration of acid in the mixing vessel in the range 15% to 45%
(wt/wt). The dilution of the concentrated sulphuric acid act firstly to heat the solution and
secondly to increase the acid strength of the process liquor. This caused the liquor to self
crystallize, forming ferrous sulfate monohydrate. The resulting slurry, containing both
crystallized and soluble ferrous sulfate, is then transferred to the next stage of the process.
Stage 5 - The slurry is thickened to generate a high Fe concentration slurry using a gravity
thickener. The clarified acidic liquor generated as the overflow from the gravity thickener is
used as acidic feedstock to the first circulation tank in stage 1.

Stage 6 - The thickened slurry is filtered to produce a solid monohydrate product. The filtrates
are then recycled back to stage 1 of the process. The thickened slurry has from 20% to 40% by
wt. monohydrate crystal. The end product obtained are 25-28% Fe(II), 28-30% total Fe and
approx. 5% -10% sulphuric acid. The particle size range of the obtained product is
approximately 20 um-55um.
INTRODUCTION

Sodium Silicate (Na2SiO3) is formed by melting sand and Sodium Carbonate (Soda Ash). The industrial
name of it is water glass. It is extensively used in the manufacturing of Detergents, Silica Gel, Card-board,
Paper, Textiles, Paints, Adhesives, Pottery, Sanitaryware, Refractories, Foundry and Wood Processing
Industries because of it’s very good binding, adhesive, bleaching and sizing properties respectively. It is
also used as electrolyte in keeping fine particles in suspension (of water) without allowing them to settle
down.

TECHNICAL ASPECTS:

Process of Manufacture

Silica sand and Sodium carbonate are the two principal raw materials used in the manufacture of
sodium silicate. The proportions of these two raw materials will vary depending on the ratio of Na2O
and SiO2 required in the final product. Processed quartz with a particle size distribution of –20 and +80
BS Sieve can also be used in place of natural silica sand. Sodium carbonate, also called soda ash, is
available in two forms: dense and light. Only dense variety of sodium carbonate is used for manufacture
of sodium silicate. The raw materials are charged from a charging end, which is called a dog house, into
a continuous glass-melting furnace operated at 1200 C to 1400 C. The exact melting temperature will
depend on the batch constituents. There will be weight loss of approximately 10% in the weight of the
charge to the weight of finished fused melt drawn from the furnace due to loss of gases and
volatilization of alkali oxides. The fused melt is drawn from the discharging end of the furnace
continuously or periodically as a thin stream. This melt will be solidified by passage into a moving chilled
conveyor of steel moulds, in which the melt cools to a semi-transparent solid. If the hot melt is sprayed
with a stream of cold water, it is shattered into fragments. The fragments are either charged into
grinding and screening equipment to yield solid sodium silicate (granular) or are passed into a rotary
dissolver. In the rotary dissolver, the solid material is dissolved by superheated (80 psi) steam.
Alternatively, the fused melt is directly passed into water, in which it is dissolved with steam. The
resulting solution is clarified by settling in a tank and is adjusted to the desired specific gravity. Specific
gravity of sodium silicates range from 22 to 69 Be with 40 Be being the most common. Dry, powdered
sodium silicates may be produced by taking liquors of proper specific gravity and forcing them through a
very fine opening into a solidification chamber. The chamber is swept by a rapid current of cold air,
which carries off the moisture. The desired sodium silicate is obtained by varying the ratio of the raw
materials charged as well as the working up of proper solution.

Quality Specifications:
As per BIS publication following standards are
IS:6773-1978,
IS:9601-1980, &
IS:381-1995

Grades: The material shall be of two grades, Neutral & Alkaline. The material of both grades shall be in
one of the following two forms:
i) Liquid: It shall be thick (viscous), translucent mass of water white or slightly grey colour.
 ii) Solid: It shall be in the form of glassy lumps of pale grey to green colour.

PROCESS FLOW CHART:

Raw Material Storage —> Batch Preparation —> Mixing —> Charging —> Melting —> Discharging —>
Quenching —> Dissolving —> Bleaching —> Testing —>Sorting —> Packaging —> Despatching

PRODUCTION CAPACITY:
i) Quantity (MT) : 200

MOTIVE POWER REQUIREMENT: 20 KWH

POLLUTION CONTROL NEEDS: In the batch house cyclonic dust collector is recommended to be used.
However, exhaust and proper ventilation is required to be produced in every section, Since the product
mix contains soda ash, only CO2 would be expelled out of the chemicals along-with the exhaust.

ENERGY CONSERVATION: In comparison to conventional coal fired furnaces, Furnace Oil/ LDO/
Natural Gas Fired Modern Tank Furnace with heat insulation is more energy efficient
Other Equipments

DeMineralising Water System

Demineralized Water also known as Deionized Water, Water that has had its mineral
ions removed. Mineral ions such as cations of sodium, calcium, iron, copper, etc and
anions such as chloride, sulphate, nitrate, etc are common ions present in Water.
Deionization is a physical process which uses specially-manufactured ion exchange
resins which provides ion exchange site for the replacement of the mineral salts in
Water with Water forming H+ and OH- ions. Because the majority of Water impurities
are dissolved salts, deionization produces a high purity Water that is generally similar
to distilled Water, and this process is quick and without scale buildup. De-mineralization
technology is the proven process for treatment of Water. A DM Water System produces
mineral free Water by operating on the principles of ion exchange, Degasification, and
polishing. Demineralized Water System finds wide application in the field of steam,
power, process, and cooling.

Principle
Raw Water is passed via two small polystyrene bead filled (ion exchange resins) beds.
While the cations get exchanged with hydrogen ions in first bed, the anions are
exchanged with hydroxyl ions, in the second one.

Process
In the context of Water purification, ion-exchange is a rapid and reversible process in
which impurity ions present in the Water are replaced by ions released by an ion-
exchange resin. The impurity ions are taken up by the resin, which must be periodically
regenerated to restore it to the original ionic form. (An ion is an atom or group of
atoms with an electric charge. Positively-charged ions are called cations and are usually
metals; negatively-charged ions are called anions and are usually non-metals).
The following ions are widely found in raw Waters :
Cations

 Calcium (Ca2+)
 Magnesium (Mg2+)
 Sodium (Na+)
 Potassium (K+)

Anions

 Chloride ( Cl-)
 Bicarbonate (HCO3-)
 Nitrate (NO3-)
 Carbonate (CO32-)
Ion Exchange Resins
There are two basic types of resin - cation-exchange and anion-exchange resins. Cation
exchange resins will release Hydrogen (H+) ions or other positively charged ions in
exchange for impurity cations present in the Water. Anion exchange resins will release
hydroxyl (OH-) ions or other negatively charged ions in exchange for impurity anions
present in the Water. The application of ion-exchange to Water treatment and
purification. There are three ways in which ion-exchange technology can be
used in Water treatment and purification : first, cation-exchange resins alone can
be employed to soften Water by base exchange; secondly, anion-exchange resins alone
can be used for organic scavenging or nitrate removal; and thirdly, combinations of
cation-exchange and anion-exchange resins can be used to remove virtually all the
ionic impurities present in the feedWater, a process known as deionization. Water
deionizers purification process results in Water of exceptionally high quality

Deionization
For many laboratory and industrial applications, high-purity Water which is essentially
free from ionic contaminants is required. Water of this quality can be produced by
deionization.The two most common types of deionization are :
• Two-bed deionization
• Mixed-bed deionization
Induction Furnace

An induction furnace consists of a nonconductive crucible holding the charge of metal to be melted,
surrounded by a coil of copper wire. A powerful alternating current flows through the wire. The coil
creates a rapidly reversing magnetic field that penetrates the metal. The magnetic field induces eddy
currents, circular electric currents, inside the metal, by electromagnetic induction.[9] The eddy
currents, flowing through the electrical resistance of the bulk metal, heat it by Joule heating.
In ferromagnetic materials like iron, the material may also be heated by magnetic hysteresis, the
reversal of the molecular magnetic dipoles in the metal. Once melted, the eddy currents cause
vigorous stirring of the melt, assuring good mixing.

1 - Melt
2 - water-cooled coil
3 – yokes
4 - crucible
Conclusion

Our two week industrial attachment with Namokar speciality Chemicals Pvt Ltd has been one of
the most interesting, productive and instructive experience in my life. Through this training, we
have got the new insight and more comprehensive understanding about the real industrial
working condition and practice, it is also improved my soft and functional skill. All these valuable
experiences and and knowledge that we have gained were not only acquired through direct
involvement in task but also through other aspects of training such as : work observation,
interaction with colleagues, supervisors and other people related to field. We are sure that
industrial training program has achieved its primary objective. As a result of this training we are
more confident to build our future career.