SUMMER TRAINING REPORT ON NUCLEAR FUEL COMPLEX ,HYDERABAD.

1. SUMMER TRAINING REPORT
ON
NUCLEAR FUEL COMPLEX
HYDERABAD
Presented by :
SHUBHAM SINGH
B.TECH,CHEMICAL ENGG.
IT ,GGV

2. CONTENT
• INTRODUCTION.
- HISTORY.
- SCOPE.
- VISION AND MISSION.
• ABOUT ZIRCONIUM AND HAFNIUM.
• PRODUCTION OF ZIRCALLOY COMPONENTS.
• FLOW SHEET OF ZIRCONIUM OXIDE PRODUCTION.
• PROCESS OF PRODUCTION.
- DISSOLUTION.
- SOLVENT EXTRACTION.
- SCRUBBING.
- STRIPPING.
- TREATMENT WITH SODA SOLUTION.
- PERCIPITATION.
- REPLUPING.
- VACCUM FILTRATION.
- DRYING.
- CALCINATION.
- GRINDING.
- BLENDING.
• PROPERTIES AND USES OF ZIRCONIUM OXIDE.

3. INTRODUCTION.
HISTORY.
• The Nuclear Fuel Complex (NFC), established in the year 1971 is a major
industrial unit of Department of Atomic Energy, Government of India.
• NFC is located near the famous shrine of Moula-ali at Hyderabad, is
spread over an area of 150 acres.
• The complex is responsible for the supply of nuclear fuel bundles and
reactor core components for all the nuclear power reactors operating in
India.
SCOPE.
• It is a unique centre in the world where Nuclear fuel and other reactor
core components are manufactured under one roof starting from ore
concentrations to finished, ready to use products thus emulating the
slogan ”ORE TO CORE UNDER ONE ROOF”.
• The complex also symbolizes the strong emphasis on self-reliance in the
Indian Nuclear Power Programme. The advanced technologies for the
production of nuclear grade uranium di-oxide fuel, zirconium.

4. VISION AND MISSION.
• Indiaispursuingathreestagenuclearpower
ProgrammelinkingthefuelcyclesofPressurized
HeavyWaterReactors(PHWR)andLiquidMetal
CooledFastBreederReactors(LMFBR).
• LightWaterReactors(LWR)havealsobeenincludedinthe
programmeinordertoachievethetargetof 20,000MWeofnuclear
powerbytheyear2020.
• Beside supplyingfuelfornuclearinIndia,it also manufactures and supplies
stainless steel core components for the Fast Breeder Reactor
programme, seamless alloy steel and Titanium tubes and other special
high purity materials for both nuclear and non-nuclear applications.
• With highly qualified and committed team of Scientists, Engineers
Technicians, resources, state of the art equipment and technology the
main objective of NFC is poised to meet challenges in the year to come.

5. INDIA’S THREE STAGE NUCLEAR POWER
GENERATION PROGRAMME.

6. ZIRCONIUM BELONGS TO GROUP IV PERIOD V, IS A
TRANSITION ELEMENT.
HAFNIUM BELONGS TO GROUP IV AND PERIOD VI, IS ALSO A
TRANSITION ELEMENT.
ATOMIC NO. OF ZIRCONIUM IS 40 AND THAT OF HAFNIUM IS
72.
AS BOTH BELONG TO SAME GROUP, IT BECOME DIFFICULT TO
SEPARATE HAFNIUM FROM ZIRCON SAND.
ABSORPTION CROSS SECTION OF NEUTRON FOR ZIRCONIUM IS
ABOUT 0.18 BARN AND THAT OF HAFNUM IS 115 BARN.
ZIRCONIUM FOUND IN NATURE IN FORM OF ZIRCON SAND (ZrSiO4) IN
WHICH HAFNIUM CONTENT VARY FROM FEW TENTHS OF 1 PERCENT
TO SEVERAL PERCENT.
WHILE NUCLEAR GRADE ZICONIUM IS USED AS CHAIN REACTION
INITIATOR, HAFNIUM IS USED TO CONTROL THE CHAIN REACTION.
ABOUT ZIRCONIUM AND HAFNIUM.

7. PHYSICAL AND CHEMICAL PROPERTIES OF ZIRCONIUM AND
HAFNIUM.
Physical Properties Zr Hf
Atomic number 40 72
Atomic weight 91.22 178.49
Melting point, 0C 1830 2222
Density, g/cc 6.49 13.01-13.09
Boiling point, 0C 2900 3100
Transition temperature,0C 862 1670
Chemical Property Zr Hf
Atomic radius,0A 1.452 1.442
Ionic radius, 0A 0.74 0.75

8. PRODUCTION OF ZIRCALLOY COMPONENTS.
ZIRCONIUM OXIDE PLANT (ZOP).
• Zirconium oxide plant (ZOP) involved in production of zirconium oxide powder
for which zircon sand is used as basic raw material having silicates and hafnium
as critical impurities.
• Zircon sand is subjected to fusion process with Caustic Soda at 650℃ followed by
series of leaching tank to remove sodium silicate.
• After leaching ,it is washed in plate and frame filter press to remove impurities
and alkalinity.
• Obtained washed feed is dried in turbo dryer and then subjected to dissolution
with nitric acid followed by solvent extraction to obtain pure zirconium nitrate
solution.
• Pure zirconium nitrate solution is then precipitated and subjected to drying and
calcination to obtain granules, which is pulverized to obtain fine powder of
zirconium oxide.
ZIRCONIUM SPONGE PLANT (ZSP).
• To produce reactor grade sponge, chlorination of zirconium oxide powder is done
at high temperature in presence of petroleum coke and starch solution.
• ZrO2 + 2Cl2 ZrCl4

9. • Starch in removed in the furnace by coking with continuous supply of cooling
water and N2.
• This briquette is chlorinated at high temperature to obtain zirconium chloride.
ZrCl4 is converted to zirconium metal by Kroll’s reduction reaction.
ZrCl4 (g) + 2Mg (l) Zr (s) + 2MgCl2 + 76 Calmole-1 (at 11500C).
• The reduced mass is vacuum treated at high temperature to distil out MgCl2 to
get pure zirconium.
ZIRCALLOY FABRICATION PLANT (ZFP).
The activities of this plant can be divided into three categories:
• INGOT MAKING: The alloys made in the melt shop are Zircalloy-2 for BWR fuel,
zircalloy-4 for PHWR fuel and Zr-Nb-Cu for a special PHWR component.
• The process involves mixing of alloying elements during briquetting, these are
welded in electro-beam welding equipment to form electrode.
• The electrode melted in furnace vacuum arc melting to make the primary ingots
which are subjected to re-melting to make a homogeneous melt.

10. • HOT EXTRUSION: The ingots are melted in two sizes viz., 300mm diameter and
350mm diameter, which are broken down in hot extrusion press to either rounds
or slabs depending on the end products.
• FINISHING OPERATIONS: Hot extruded rounds are subjected to pilgering to
produce fuel tubes. Slabs are rolled into sheets and further cold rolled to get the
final dimensions.
• These sheets are used for making PHWR/BWR fuel component or calandria
tubes by steam making.

11. THANK YOU

12. SUMMER TRAINING REPORT
ON
NUCLEAR FUEL COMPLEX
HYDERABAD
Presented by :
RATAN MONDAL
B.TECH,CHEMICAL ENGG.
IT ,GGV

14. FLOWSHEET OF ZIRCONIUM OXIDE PRODUCTION

15. PROCESS OF PRODUCTION
DISSOLUTION:(SS-304L)
Raw materials:
• Dry feed powder which is procured in 50kg bags is tested in control lab
before charged in the reactor.
• Nitric Acid (60% concentrated). Nitric acid is stored in two horizontal SS tank
of 150KL capacity.
Chemical reaction:
Zr(OH)4 + 4HNO3  Zr (NO3)4 + 2H2O

16. PROCESS DESCRIPTION.
• Required amount of nitric acid (12N) is charged in the reactor and heated
up to 60℃ by steam at pressure of 3 kg/cm2.
• Calculated amount of dry powder is added to the reactor and agitated for
2 hours followed by settling time of extra 2 hours.
• Dry powder dissolve in nitric acid and reacts to give zirconium nitrate
solution which is feed material for Solvent extraction process.
• As reaction is exothermic reaction ,temperature rises up to 85℃ which
indicates the dissolution process is completed.
• The nitrate solution is then stored in feed tanks having conical bottom
which ensures the draining of slit settles in due course time.
• Temperature should not exceed more than 85℃ ,otherwise nitrate fumes
will form and the batch is rejected.
• Free acidity should be maintained in order to extract zirconium from
zirconium nitrate solution by solvent extraction process.

17. SOLVENT EXTRACTION.
• The process of separation of components of a solution depends upon the
unequal distribution of the components between two immiscible liquids is
known as “LIQUID – LIQUID EXTRACTION”
• Solvent extraction is based on the principle that a solute can distribute
itself in a ratio between two immiscible solvents.
Raw materials:
• Zirconium nitrate solution from the feed tanks.
• Lean solvent (Tri Butyl Phosphate + Kerosene).
• Nitric acid (to maintain free acidity).
PROCESS DESCRIPTION.
• Mixer-settler (made of SS316/304L) is used for the process of extraction.
• The process involve ten stage counter current solvent extraction in which
nitrate solution is introduced in first stage and lean solvent in tenth stage.
• The solvent TBP is selected because of its tendency to extract only
zirconium at a given acidity in the nitrate medium.

18. • A digital rotameter is used in place of float type rotameter as slurries is
handled.
• Nitric acid is added accordingly to each stage after 1st stage to maintain free
acidity.
• The mixing and propagation is done by means of compressed air (air lift
mechanism).
• The principle of air lift mechanism is that when air is mixed with solution, the
density of solution decreases and it causes the solution to rise and also
enhance mixing operation.

19. SCRUBBING:(SS316)
Raw materials:
• Organic (extract) from the slurry extraction.
• Pure solution from stripping.
• Nitric acid.
PROCESS DESCRIPTION.
• Counter current scrubbing of extract is done in mixer-settler by using pure
zirconium nitrate solution obtained from stripping process.
• Mixers contain side baffles and agitator to create turbulence to provide good
mass transfer.
• After proper mixing it is sent to settling compartment where it settles and
then transfer to next stage by means of density difference.
• After ten stages of mixing and settling ,we obtain scrub raffinate and extract
which is feed for stripping process.
• The main importance of this unit is that the hafnium composition is totally
eliminated (<50 ppm).
• Scrub raffinate contain some amount of zirconium which is used for dilution in
dissolution tank to maintain free acidity.

20. Scrubbing Unit

21. STRIPPING:(SS316)
Raw materials:
• Extract pure from the scrubbing section.
• De Mineralized water.
PROCESS DESCRIPTION.
• Pure extract from scrubbing unit is counter currently mixed with
demineralised water.
• As free acidity is reduced, zirconium in organic phase transferred to aqueous
phase.
• The stripped organic solution is sent for recycling by treatment with soda
solution.
• The zirconium in aqueous phase is called Pure solution.
• Some part of pure solution is transferred to storage tank and some part is
recycle to scrubbing unit.

22. STRIPPING UNIT

23. TREATMENT WITH SODA SOLUTION:
Raw materials:
• Lean solvent from the stripping unit.
• Soda solution.
• DM water.
PROCESS DESCRIPTION.
• The Lean solvent from the stripping section is sent to mixer-settler unit in
which soda solution is passed in a counter current flow.
• The lean solution i.e., tri butyl phosphate degrades into mono butyl
phosphate and di butyl phosphate
• The aim of this treatment is to remove the mono butyl phosphate and di
butyl phosphate, which dissolve in soda solution thereby producing free
tri butyl phosphate.
• MBP and DBP have higher solubility in aqueous medium than that of TBP.
• This process is done in order to recycle TBP so that process become more
economical.
• TBP has 0.39g/l solubility in water
• DBP has 0.64g/l solubility in water
• MBP has complete solubility in water

24. THANK YOU

25. SUMMER TRAINING REPORT
ON
NUCLEAR FUEL COMPLEX
HYDERABAD
Presented by :
KANCHI AKSHITH
B.TECH,CHEMICAL ENGG.
IT ,GGV

26. PRECIPITATION:(SS-304)
Raw materials:
• Pure solution from the stripping unit.
• Ammonium hydroxide.
• Sulphuric acid.
Chemical reaction:
Zr (NO3)4 + 6NH4OH + H2SO4Zr (OH)4 + 4NH4NO3 + (NH4)2SO4
PROCESS DESCRIPTION.
• The required amount of pure solvent ,ammonium hydroxide and sulphuric
acid is mixed in precipitation tank and mixed till temperature reach 600C.
• Ammonium hydroxide is added to precipitate zirconium nitrate to zirconium
hydroxide.
• The slurry obtained during precipitation is passed through vacuum drum
filter which is maintained around 450 mm Hg.
• The filter cloth is made of polypropylene.

27. Precipitation tank (SS-304)
• The drum rotates with a speed of 1.33 revolutions per minute.
• The cake coming out contains 80-85% moisture which consists of water,
ammonium nitrate and ammonium sulphate.

28. REPULPING.
Raw materials:
• Filtered cake.
• Demineralized water.
PROCESS DESCRIPTION.
• The cake obtained from vacuum drum filter is mixed with demineralised
water in a tank and the process is called Repulping.
• The repulping process is done so that ammonium compounds dissolve in
demineralized water thereby reducing the possibility of explosion in the
drying chamber.

29. VACUUM FILTRATION.
Raw materials:
• Filtered cake from repulping.
Material of construction:
• Apart from cast iron, other materials of construction include stainless steel,
titanium and plastics such as poly vinyl chloride etc.
PROCESS DESCRIPTION.
• When the drum dips into the slurry vacuum is applied because of which the
slurry is sucked into the drum.
• When the drum comes out of the boot then air is applied to blow out the
filter cloth thereby helping the easy scraping of the cake.
• The cake is scraped using a doctor blade.
• We have to agitate the slurry during the filtration to avoid settling of any
solids in the equipment.

30. Vacuum Drum Filter

31. DRYING.
Raw materials:
• Wet cake from vacuum filtration.
Material of construction:
• High temperature drying is done to remove moisture content from 85% to
30% and to remove ammonium nitrate from cake.
Exhaust
Discharge
BLOWER
Heating
elements
FEED POINT
HOT TEMPERATURE OVEN

32. PROCESS DESCRIPTION.
• The wet cake from filtration is charged into static bed dryers which use hot
air for drying purpose.
• The temperature of oven is around 250℃ .
• Drying time : 12hours – 16 hours.
• The dry product is then charged in to calcination hopper for calcination.
CALCINATION.
Raw materials:
• Dry cake from drying section.
EQUIPMENT DESCRIPTION.
• Hollow cylindrical shell of diameter 350mm-500mm and length of 5m-8m
with axis at slight angle of horizontal.
• It is supported on rollers so that it can rotate to evenly distribute the heat
to the material.
• Materials move through dryer by virtue of its motion, heat effects and
inclination of the cylindrical shell.
• The cylindrical shell is rotated by a gear mechanism at a speed of 2-2.5rpm.

33. Chemical Reaction:
Zr (OH)4 ----------------- ZrO2 + 2H2O
CALCINATOR

34. PROCESS DESCRIPTION.
• The dried material is charged through an opening at the top and is fed into
the rotary furnace.
• The cylindrical tube is made up of SS310 and the heating elements are made
of nichrome.
• The temperature reached in a calcinations chamber is about 800OC.
• The main use of this furnace is to drive away the moisture and the other
volatile impurities to the specified limits.
• The collected zirconium oxide is sent for grinding.
GRINDING.
Principle:
• Size reduction is achieved by impact and attrition.
EQUIPMENT DESCRIPTION.
• The hammer mill consists of essentially of high-speed rotor turning inside a
cylindrical casing.
• In this mill, the particles are broken by sets of swing hammers.
• Several rotor discs each carrying 4 to 8 swing hammers is often mounted on a
single shaft.

35. PROCESS DESCRIPTION.
• The grinding section essentially consists of a feed charger, a feed rate
adjusted hammer mill, a blower and a big filter.
• The material is ground in the hammer mill.
• The ground power is pneumatically carried using a centrifugal blower.
• The product is of 325 mesh.

36. BLENDING.
• Blending is a process of mixing the ground solids in required proportion
to get the required percentage purity of zirconium oxide.
• After blending, the final composition are as follows:
Hafnium <100 ppm
Titanium <150ppm.
• The zirconium oxide thus obtained is then sent to Zirconium Sponge
Plant (ZSP) for production of zirconium metal.

37. PROPERTIES AND USES OF ZIRCONIUM OXIDE.
PROPERTIES OF ZIRCONIUM OXIDE
• High density
• Thermal conductivity (20% that of alumina)
• Chemical inertness
• Ionic electrical conduction
• Resistance to molten mass
• High fracture toughness
• High hardness Zirconium oxide (zircon) also has a high index of refraction
USES OF ZIRCONIUM OXIDE
• Precision ball valve balls and seats
• Rollers and guides for metal tube forming
• Thread and wire guides
• Hot metal extrusion
• Marine pump seals and shaft guides
• Oxygen sensors
• High temperature induction furnace susceptors
• Fuel cell membranes
• Electric furnace heaters over 2000OC in oxidizing atmospheres

38. THANK YOU