INDUSTRIAL TRAINING REPORT KIOCL Limited New Mangaluru Port .Panambur ,Mangaluru – 575010 Submitted by: LOKESH GUGULOTH JEEVAN KUMAR CHUKKA HASWANTH MATHANGI VISHAL NAGAR Department Of Chemica5 Engineering National Institute Of Technology Karnataka Srinivasnagar PO, Surathkal, Mangalore 575025, India INDEX Chapter Content 01 Introduction to the Company 02 Analysis Of Iron Ore 03 Page Number 01-06 2.1 Analysis Of % Of Iron Ore Sample 07-11 2.2 Determination Of Silica 12-13 2 .3 Determination Of Alumina 12-14 2.4 Loss On Ignition 15 2.5 Determination Of Phosphorus 16-18 2.6 Determination Of Sulphur 19-23 2.7 Determination Of Blaine’s Number 24-26 Analysis Of Bentonite 3.1 Free Swelling Capacity 25 3.2 Plate water Observation 26-27 3.3 Size Analysis 28 04 Blast Furnace unit 29-32 05 Capitative Power Plant 35-41 06 Safety measures at KIOCL 41 07 Snapshots 42 08 Conclusion 43 09 Acknowledgement 44 Page no 1 INTRODUCTION: KIOCL LTD. (KIOCL) - COMPANY HISTORY Kudremukh Iron Ore Company Limited (KIOCL) is a Miniratna Government of India Enterprise having its Head Office in Bangalore; it has Pelletisation and Pig Iron plant units in Mangalore. The Company was established in 1976 as 100% Export Oriented Unit to develop the mine and plant facilities. The Company is primarily engaged in the business of Iron Ore Mining Benefication and Production of high quality Pellets.The mine and plant facilities were commissioned in 1980 and the first shipment of concentrate was made in October 1981. The outstanding feature of Kudremukh ore is its low alumna sulphur phosphorous vanadium and other deleterious elements.A pelletisation plant with a capacity of 3 million tonnes per year was commissioned in 1987 for production of high quality blast furnace and direct reduction grade pellets for export.A 110 km road through ghats was built and a slurry pipeline to Mangalore port was completed. KIOCL delivered the project on time within the estimated cost of US$630 million.The company entered into Joint Venture with MECON & MSTC in order to set up a Pig Iron & Ductile Iron Spun Pipe Plant at Mangalore. KIOCL MISSION : 1.Lasting relations with customers and Vendors to ensure smooth supply chain based on trust and mutual benefits. 2.Business with ethics & integrity. 3.To thrive to improve the socio economic condition in the neighbourhood of 4.Company's production centre. 5.Continuous learning. 6.Adaptability to Technology and changing Global Scenario. h Growth, recognition and reward for employees. Operational Performance of Pellet Plant: KIOCL is producing both BF and DR grade pellets with excellent chemical & physical specifications to suite for Blast furnaces and direct reduction plants. The Company has taken up many initiatives like handling both Magnetite and Hematite types of ores through in-house R&D, sourcing from both domestic and global markets through long term contracts,100% utilization of coastal transportation, Indigenization of equipments/spares etc. Page no 3 SYSTEM DEPARTMENTS 1. Pellet plant: The pellet plant at Mangalore products high quality iron oxide pellets as following facilities. - Palletizing disc - Roller screens - Indurating Machines 2. Captive power plant: It controls by APP control system. It uses three generators. Each generators have power of 10M watts 3. Blast Furnace: KIOCL in additional to dispatch of pellet by sea route dispatch of pellets by trucks to meet the demand of small customer like coal based sponge iron manufacturers, mini - steel plants etc.The blast unit h as a blast furnace of 350 cum capacity of producing 2, 27,500MT of hot metal per annum. 4. Filter plant: KIOCL Limited at its Port Facilities departments has iron ore grinding unit, filtering unit and loading system for handling the panama vessels for cargo loading at a draft depth of 13 meters. Port Facilities: KIOCL Limited at its Port Facilities department has iron ore grinding unit, filtering unit and loading system for handling the panamax vessels for cargo loading at a draft depth of 13 mtrs. The iron ore fines received by rail and ship are subjected to grinding after primary screening. Through three nos. of Ball mills, the ore is ground by way of wet grinding process. The ore thus ground is subjected to screening and then filtration. Highly efficient screens are used for screening the ground iron ore with size separation. For filtration of the ground slurry, vacuum disc High Pressure filters are used. The filtered material will have a moisture of around 8.5-11%.This is then carried to a closed storage shed of 2 lakh tonnes capacity.From the storage shed, the ore is fed to the Pellet Plant using a bridge reclaimer. The Company has another shed for storage of Pellets. About 2.5 lakh tonnes of pellets can be stockpiled there. A bucket-wheel reclaimer is used to load the pellets to conveyors to further carry the pellets to ship, anchored in the berth dedicated to KIOCL Ltd. This can load 5000 tonnes per hour. Page no 4 Pellet Plant: A 3.5 MTPA Pellet Plant based on LURGI Straight Grate process is in operation at Mangaluru, since 1987. The process of palletization involves mixing of Iron Ore Concentrate with Limestone, Bentonite, Coke as additives for improving the Physical and Metallurgical properties of Pellets. The mixed material is fed to pelletizing discs of 7.5 meter dia for production of green pellets, which are screened on Double Decker roller screen to remove the un-sized material. The sized green pellets are fed to the indurating machine of 492 Sq meter grate area. The green pellets are dried, pre-heated fired at high temperature and cooled in the indurating machine. The pellets after screening to remove the undersized materials are conveyed to a stockpile. Captive Power Plant: KIOCL ltd has two captive power plants. One at Pellet Plant Unit and the other at Blast Furnace Unit. At Pellet Plant, there are three DG sets having maximum capacity rating of 9.36 MW each. They are run by low Sulphur furnace oil. At the BF Unit, two DG sets of 3.5 MW are run by the hot gas generated by the Blast Furnace. Blast Furnace unit: The Blast Furnace unit has a blast furnace of 350 cum capacity of producing 227500 MT of Hot Metal per annum. The end product of the Blast Furnace Complex is foundry grade Pig Iron. The following raw materials are used in the process : A special feature of blast furnace process is that by using a feed of 100% Iron Ore pellets from KIOCL's Pellet Plant, 650 Tons per day of Hot Metal can be Page no 5 produced. For the present however, calibrated iron ore lumps of 10 - 30 mm size is being used as feed to the furnace. The principle involved in Blast Furnace iron making is the thermo-chemical reduction of iron oxide ore by Coke into liquid iron at around 1500 degree C. The unwanted materials are removed in the form of liquid slag by addition of suitable fluxes. Raw materials are changed from blast furnace top and hot air is sent up from the bottom resulting in these thermo-chemical reactions. The major raw materials used in the Blast Furnace operation are Iron Ore, Coke, Manganese Ore, Lime Stone, Quartizite and Dolomite, the last three being fluxes. The raw materials are received and stacked material wise in the stockyard. The materials required for the day's usage are then transferred into day bunkers by use of a conveyor system. The materials from the day bunkers are screened and weighed to the required size and quantity in batches. The undersize materials in the screening process are transferred into the fines bunkers for storage. The weighed batches are discharged into a conveyor in a pre-determined sequence and are transported to the blast furnace top for charging into the blast furnace. The Blast Furnace top charging system is equipped with a double bell system to maintain the blast furnace top pressure. The raw materials are evenly distributed by using a rotary chute. The charging is carried out in batches as per a pre-determined sequence. The stock level indicator measures the level of raw materials inside the furnace and gives feed back for charging inputs. The entire charging system from screening to charging is fully automated. The hot air required for the chemical reactions are blown into the furnace at an average rate of 43000 Nm3/hr by 2 HT motor driven blowers. The air before entering into the blast furnace is heated up to 1100 degree C using 3 stoves. The stove refractory checkers, which store heat, are heated by combustion of air and blast furnace gas inside stoves at optimum proportions. Blast Furnace gas is a by-product the furnace and carries around 20% CO which makes it a cheap and efficient fuel. The heat thus stored is passed onto the cold air blown by the Page no 6 blowers raising its temperature to 1100 Degree C making it suitable for use in the blast furnace. The counter current movement of blast air and raw materials facilitates the reduction reaction of iron ore. The liquid iron (Hot Metal) produced collects at the bottom of the furnace above which liquid slag, which is higher, is collected. Both slag and hot metal are drained out through a top hole at regular intervals in Cast House. The hot metal is collected in 35 T capacity ladles where as the slag is granulated into powder form in a Slag Granulation Plant. The Blast Furnace gas generated inside the furnace is cleaned of dust at Dust Catcher and Gas Cleaning Plant (GCP). Gas is washed of dust in GCP by water spray and the stoves and captive power plant use the cleaned gas as a cheap source of fuel. Any excess gas is bled off to the atmosphere after flaring. Dedicated water pumping arrangements provides cooling water for the different cooling members inside the furnace. Cooling is essential in view of the refractory and shell life of the furnace. Another pumping system caters to the water requirements of the GCP. The ladles carrying hot metal are transferred to a Pig Casting Machine (PCM) using a 50 Ton EOT crane. In the PCM, the hot metal is cast into 'Pig Iron' of max 8 Kg weight. The arrangement for this includes a double strand casting chain carrying 298 moulds in one strand. The strands are driven by an electric drive. The ladle is tited using the EOT crane and the hot metal is directed into the moulds by a runner system. Air-cooling and water-cooling is provided for the casting chain. The pig iron generated by the PCM is collected in three wagons from where it is lifted by electro-magnetic crane and transported to the pig storage yard and stacked grade wise for dispatch to customers. The Pig Iron thus produced is sold to various customers all over India as per their specified requirements. The Pig Iron thus produced is sold to various customers all over India as per their requirements.The Captive Power Plant(CPP) with two nos.each of 3.5MW Steam Turbine Generators Page no 7 SPECIFICATION OF IRON ORE FINES a) Fe : 64% Guaranteed [Fe above 64% will be accepted with bonus [Fe below 64% and up to 63% will be accepted with penalty. [Fe below 63% and up to 62% will be accepted with penalty. [Fe below 62% and up to 61% will be accepted with penalty. [In case Iron ore fines are supplied with Fe content less than 61%, the same shall not be returned to the supplier and a token payment of Rs.1/- Per WMT (Rupees One only per WMT) will be made by KIOCL to the supplier. b) SiO2 + Al2O3 : 6% max (Al2O3-2% max) [Al2O3 above and up to 2.5% will be accepted with penalty. c) Moisture : 5% max [Above 5% moisture, to the extent it exceeds 5% limit, acceptance will be at corresponding reduction on quantity supplied. d) Sulphur : 0.01% max. e) Phosphorus : 0.04% max f) Size : (-) 10mm g) Tolerance : (+) 10mm : 5% max (-100mesh) : 15% max DETERMINATION OF MOISTURE: For determining moisture content, samples from the loaded tippers at KIOCL, Pellet Plant weigh Bridge will be collected and the same will be analyzed by a registered assayer acceptable to both KIOCL and the supplier. The results obtained thereof are binding on both the parties and shall be final for payment besides all applicable clauses in this tender. During this analysis, the supplier shall ensure deployment of his representative for witnessing the tests, if required. Page no 8 ANALYSIS OF % OF IRON IN THE IRON ORE SAMPlE Determination of iron (Fe) Theory: In ores and minerals of iron it generally appears in a mixed form as ferrous or ferric compounds. In order to determine the iron content volumetrically, the ferric form is reduced to ferrous form quantitatively and the whole of ferrous iron is oxidized to ferric form. From the standard oxidizing agent consumed during the reaction, the amount of iron present is calculated. Most of the iron ores are brought into solution by digesting with concentration hydrochloric acid and reduced to ferrous state using stannous chloride as reducing agent. 2Fe3 + Sn² à 2Fe² + Sn The solution containing iron in the ferrous state is titrated with the standard potassium dichromate solution, which oxidizes whole of ferrous iron to ferric iron, using diphenylamine as indicator. 6Fe²+ +14H à 6Fe+ 2Cr₂³ +7H₂O Solution preparation:1. Standard K₂Cr₂O- solution of approximately 0.1343N: Exactly 65.86gm of dry Potassium dichromate was placed in a 10 liter carboy & diluted to the mark with distilled water. Iml of this K-Cr₂O solution is equivalent to approximately 1.5% Fe. The above potassium dichromate stock solution was standardized with the help of a standard iron ore sample. Based on the volume of potassium dichromate consumed a FACTOR is established. Factor= (Fe in the standard sample)/(Volume of dichromate) 2) Conc. Hydrochloric acid (11.3N): 3) Reducing solution (SnCl, solution): Weighed out 7gms pure, dried SnCl, salt into a 250ml beaker. About 10 to 15ml dil 1:1 HCI acid was added, stirred and kept on a hotplate for digestion until the solution turns clear. Cooled the solution to room temperature & diluted it to 100ml with distilled water & preserved it in an air tight glass bottle, after adding a few pieces of granulated tin to maintain the strength. 4)Saturated Mercuric chloride (HgCl2) solution: Page no 9 About 100ml of distilled water was taken in a beaker and mercuric chloride was added with constant stirring until the solution is saturated. (Till HgCl2, is left at the beaker). 5)Barium diphenylamine sulphonate indicator: Weighed out 0.3gm of the indicator into a 250ml beaker. 10-20ml of water & 5drops of 1:1 HCI were added and kept it for digestion on a low heat for 30minutes. After cooling, 2-3 drops of conc. Sulphuric acid was added and filtered the solution & made up to 100ml with distilled water. 6)Acid mixture: Exactly 3.40 liters of distilled water was taken in 5 liters beaker & placed it in a cold water bath. To this 750ml of conc. H3PO4, acid was added with constant stirring and also750ml of conc. H2SO4 acid was added to the same with constant stirring. After cooling 100ml Barium diphenylamine sulphonate indicator was added. Procedure: Well mixed, finely grounded Iron ore powder is dried at 105°C for one hour and brought to room temperature in a desiccator. Exactly 0.5gms of the sample was weighed out in an analytical balance & transferred it to a 250ml tall form beaker. About 15-20ml of conc. HCI acid was added & digested on a hotplate without boiling the solution. When the sample was completely dissolved (which was ensured by the disappearance of black particles), then the hot solution was reduced by SnCl₂ solution which was added drop by drop from a dropping bottle till the yellow color disappears. 2-3 more drops were added. Then the solution was cooled rapidly under cold water and diluted with distilled water. To this 10ml of saturated mercuric chloride solution was added, a silky white precipitate appears. About 20ml of acid mixture with indicator solution was added. The solution was then titrated with standard K2Cr2O7 solution, the color changes from deep green to a stable purple or violet and the titre value was noted down. Factor for Potassium Dichromate used =1.4471 %Fe =Titre value * factor Page no 10 Titre Value %Fe Sample Trial 1 Trial 2 1. 44.3 44.4 64.2 2. 43.7 43.7 63.2 Page no 11 DETERMINATION OF SILICA IN THE IRON ORE:SAMPLE: Theory: Here gravimetric method of estimating silica was carried out. The soluble silicates were converted into insoluble silicates and these insoluble were filtered and the residue was treated with HF acid which vaporizes the silica as silicon tetra fluoride leaving behind other impurities associated with silica. SiO2 + HF à H2[SiF6] + 2H₂0 H2[SiF6] à SiF4 + 2HF The loss in weight therefore represents the amount of pure SiO₂ present in the sample. Solutions required: a) Conc. Hydrochloric acid (HCI) (11.3N). b) Cone. Nitric acid (HNO3). c) Perchloric acid (HClO4) -70% d) Hydrofluoric acid (HF)-48% e) Sodium carbonate salt (Na2CO3) f) Conc. Sulphuric acid (H2SO4) (18.0 N) g) Potassium pyrosulphate (K2S2O7). Procedure: Well mixed & finely powdered iron ore sample was taken and dried at 105°C for one hour and cooled in a desiccator. The sample was placed in a desiccator and brought to room temperature. Exactly 1gm of sample was placed into a 250ml short form beaker and covered it with a watch glass. About 20ml of conc. HCI was added & kept for digestion on hot plate. When the sample was nearing to dissolution: 5-6 drops of conc. HNO3 were added. The solution was allowed to digest on a hotplate for 10 minutes till the brown fumes of HNO3 escapes. About 7ml of HCIO4 was added and hydrated till thick white fumes appear. It was then cooled and extracted the dehydrated mass with 1:1 HC1 & heated for 5 minutes. The contents were filtered through No. 40 whatman filter paper into a 250ml standard flask. The residue was washed with 1:1 HCI Page no 12 followed by hot water till the yellow color on the filter paper disappears or the filter paper is acid free. Now the filtrate was preserved for further analysis. The residue was ignited in a platinum crucible at 950°C to a constant weight. It was then cooled & the residue with the crucible was weighed (W₁). After this residue in the Pt crucible was moistened with 2-3 drops of water. And about 2-3 drops of H2SO4 & about 15ml of HF were added. The contents of this crucible were to evaporate over a low heat. After the complete evaporation the crucible was ignited in a muffle furnace at 950°C to a constant weight (W₂) the residue was fused with potassium pyrosulphate or sodium carbonate. The fused mass was dissolved in dilute HCI and this was then added to the main filtrate for further analysis. Calculation: % Silica = (W1-W2) /(weight of the sample) x 100 Weight of crucible residue before hydrofluorization = W1 g Weight of crucible+ residue after hydrofluorization = W2g Weight of the sample = 1g Sample W1(g) W2(g) %SiO2 1 20.5872 20.5423 3.59 2 20.4338 20.3982 3.54 Page no 13 DETERMINATION OF ALUMINA IN THE IRON ORE:- Outline In this method an unknown Aliquot of solution from silica filtrate was pipetted out. Iron voice separated out by adding NAOH solution, and after filtration, aluminum in the filtrate was complexED with access EDTA. The access EDTA was titrated with zinc solution using xylenol Orange indicator. Solutions required: 1.Sodium hydroxide (NaOH) solution (10% w/v): 2.100gm of NaOH was placed in a beaker & dissolved in distilled water & made up to 1000ml. 3. Ammonium fluoride (NH, F) solution (10% w/v): 100gm of Ammonium fluoride was taken in a beaker dissolved in distilled water & made up to 1000ml. 4. Xylenol orange indicator: About 0.25 gm of xylenol orange indicator was weighed into a beaker. About 100ml of distilled water was added to it. And 2-3 drops of 1:1 HCI was added with constant stirring. The solution was filtered and the filtrate was stored. 5. Methyl red: 0.5 gm of methyl red was dissolved in 100ml ethanol. 6. Ethylenediaminetetraacetic acid disodium salt (EDTA): Exactly 3.7724 gm of EDTA was dissolved (which was dried at 80°C) for Ihr. into a one litre standard flask. The solution was made up to the mark Page no 14 it with distilled water. It was then standardized against 0.0IM.Strength of EDTA was calculated. Exactly 0.6538gm of granulated zinc was weight into a 250ml beaker to this 5-6ml of conc. HCI acid was added and dissolved it. It was then cooled and made the volume to 1 litre with distilled water. It was standardized by titrating against std. EDTA solution of known strength using Xylenol orange as the indicator. Color changes from orange to pink. This solution was used for calculation. Procedure: Exactly 25ml of aliquot was pipette out from the silica filtrate stock solution into a beaker. About 10 to 20ml of NaOH (10%) solution was added till no further precipitation at supernatant solution. About Igm of sodium carbonate was added and warmed on a hot plate for 15-25 minutes. It was then filtered through No 4 filter paper into a 500ml conical flask. The residue was washed thoroughly with hot water & the washings were collected in the conical flask. The residue was discarded. The solution was then neutralized with 1:1 HCl using 2-4 drops of methyl red indicator. About Sml of 0.01M EDTA solution was added and shaken thoroughly. About 1-2gms of ammonium acetate was added and the color becomes yellow. The solution was boiled for 5 minutes. The solution was then cooled to room temperature and titrated against std. 0.01M zinc solution using xylenol orange indicator and the end point is orange to pink. About 5-10ml of ammonium fluoride was added and boiled for 5 minutes. The solution was cooled to room temperature and 1gm of ammonium acetate, 2 drops of xylenol orange indicator were added and the liberated EDTA was titrated against standard zinc solution. Color changes from lemon yellow to pink. The volume of zinc solution consumed was noted down. Calculations: Volume of Zinc solution consumed-X ml Strength of Zine solution prepared 0.01M Factor for Al,O,-1.88 1ml of 1M EDTA= 1ml of IM Zn=1ml of AI 1ml of IM EDTA= 1ml of A=(27/1000) g A = 0.027 g of Al Page no 15 =0.00027mg of Al. %Al2O3=0.00027 x 250 x 100 X 1.88/25 Total: Alumina + Silica = 6% max Sample Volume of Std. Zn Soln 5Al2O3 (ml) Total= Alumina+Silica Trail 1 Trail2 1 3.6 3.7 1.8527 5.442 2 3.8 3.7 1.9035 5.443 Page no 16 Loss On Ignition Procedure: Exactly 1gm of the sample was weighed into a previously weighed platinum crucible. Heated it gradually raising the temperature and finally ignited at 1000°C for half an hour. Calculations: Loss On Ignition (%) = Weight of crucible + sample before ignition = W₁ g Weight of crucible + sample after ignition W₂g Weight of the sample taken = 1g Sample W1(g) W2(g) L.O.I 1 21.0193 20.9940 2.53 2 21.1433 21.1130 3.03 Page no 17 DETERMINATION OF PHOSPHORUS (P): Principle: Phosphorus in iron ore/pellets was determined by precipitating phosphorus as phosphor molybdate and dissolved in excess standard sodium hydroxide and back titrated with standard nitric acid. Solutions required: 1) Standard sodium hydroxide soln. (NaOH)-0.1482 N. 2) Standard nitric acid solution (HNO,)-0.1482 N. 3) Phenolphthalein indicator (alcoholic 1:1)-0.10%. 4) Hydrochloric acid-concentrated & dilute (1:1). 5) Nitric acid-concentrated &dilute. 6) Ammonium Hydroxide concentrated (NH₂OH). 7) Potassium nitrate (KNO,)-1.0%. 8) Ammonium molybdate solution - 4 liters. Procedure: Exactly 2gm of the sample was weighed out and brushed into a 250 ml beaker. Approximately 25 ml of conc. HCL was added and covered it with a watch glass and digested until the soluble minerals are in solution. About 1-2 ml of conc. HNO, was added and boiled for a few minutes. The total mass was heated and brought to dryness on a low hot plate. It was then baked for 10 minutes. It was then cooled and approximately 25 ml of dil.HCI 1:1 was added and digested it until the salts are in Page no 18 solution. The solution was filtered using filter paper No. 40 into a 500 ml Stoppard conical flask. It was alternatively washed with dilute HCI and water until the iron strain is no longer noticeable. For soluble phosphorus proceed with step 9. For insoluble phosphorus, the acid insoluble residue was ignited, fused with Na CO,. dissolved in dil. HCI, dehydrated, and the solution was filterer and combined with the filtrate from step 6. It was neutralize with NH,OH until the hydroxides are completely precipitated and there should be a slight excess of NHOH. This point was easily detected if the flask was swirled gently on the just dissolved. The solution was dark brown at this point. About 5ml of addition of NH,OH. Concentrated HNO, HNO, was added in excess. The solution was then warmed to 60-70 C and was added until the precipitate is about 50 ml of molybdate solution was added. Shaken it well and let it to stand on a warm plate for 10 minutes. It was then remove from the hot plate and let to stand at room temperature until the ammonium phosphor molybdate precipitate has settled. Then it was filtered using filter paper No. 42. The flask was washed with 1.0% HNO, until all of the precipitate was collected on the paper. Then the paper was washed with 1% KNO;. The paper was washed well until all the acid was washed out from the paper. Washing is completed when a strip of blue litmus paper placed on the end of the filter funnel does not turn pink. The flask was rinsed out well with water. The filter paper was placed in the flask, and approximately 25 ml water of water was added. Then exactly 10 ml of standard NaOH was added. Stoppered the flask and shaken well to break up the paper and dissolved the precipitate. The stopper was removed and washed down the sides of the flask. Few drops of phenolphthalein solution were added. Finally back titrated with standard HNO, to the end point. Calculations: Page no 19 Strength Of NAOH = 0.149N Sample Volume Of HNO3 Consumed Trail 1 %P Trail2 5488 4.1 4.2 0.0588 5470 4.2 4.3 0.0578 Page no 20 DETERMINATION OF SULPHUR Aim And Theory: For determination of the amount of Sulphur in iron ore samples, the Ripper method is used.The Ripper Method, developed in 1898, is an analytical chemistry technique used to determine the total amount of sulfur dioxide (SO2) in a solution. This technique uses iodine standard and a starch indicator to titrate the solution and determine the concentration of free SO2. This in turn, gives the percentage of sulphur in the given sample. Apparatus Used : 1) Supply of oxygen using medical oxygen cylinders. 2) Leco High Frequency Induction furnace consisting of one combustion unit for determination of sulphur. 3) Oxygen purifying train 4) Accelerators - Iron chips to Tin metal. 5) Crucibles - leco#IH-10-800 with #IH-10-950 crucible cover. Each crucible and cover is used for one combustion only. 6) Sulphur apparatus - leco sulphur determinator consisting of a burette stand, KIO₃ automatic burette calibrated 0.000 - 0.200% sulphur titration vessel and 2 way stopcock for filling burette and vessel. Reactions involved: I. Sulphur in the sample + oxygen → sulphur dioxide (upon heating) In the induction furnace, 100% of the sulphur is converted to sulphur dioxide. II. Potassium Iodate and potassium iodide react with hydrochloric acid to liberate Iodine gas. III. Sulphur dioxide reacts with iodine gas to liberate sulphuric acid and hydroiodic acid. ➢ S + O₂ → SO₂ ➢ KIO₃ + 5KI +6HCl → 6KCl +3H₂O +3I₂↑ ➢ SO₂ + I₂ +2H₂O → H₂SO₄ + 2HI Page no 21 Preparation of Solutions : 01. Potassium Iodate solution : Exactly 0.222 gm of potassium iodate was dissolved in distilled water and diluted To one liter in a volumetric flask. A solution of this strength will titrate up to 0.2% sulphur in a 0.5 gm sample. If sulphur content is greater than 0.2% , then the quantity of potassium iodate is increased in initial solution making. Exactly 0.444 gm potassium iodate is dissolved in water and diluted in 1 liter to titrate 0.4% sulphur in 0.5 gm sample. 02. Starch Indicator solution : About 100ml of distilled water was boiled and 1.8 gm of arrowroot starch was added, stirred and boiled and cooled later after which 3.0 gm of KI was added. The indicator solution gives a blue color but if it gives a reddish tinge then the solution should be discarded and a new solution is prepared. 03. Hydrochloric acid solution : About 15ml of hydrochloric acid is added to 1 liter of water and diluted. Procedure: About 0.5 gm of the sample of iron is weighed, transferred to a combustible crucible and the proper accelerator( tin) was added. The titration vessel was filled with HCl solution. Exactly 2 ml of starch solution was. Burette is filled with potassium iodate solution. The color formed is light blue. Initial end points with dark color affects the inaccuracy as the eye cannot detect small changes in dark solution. The crucible was placed with cover in place on a pedestal and raised into a combustion tube without engaging the power switch. The flow of oxygen was adjusted to 1 LPM. The combustion begins after 1 or 2 mins. Sulphur will not begin to burn until the sample temperature reaches 260 degree celsius. sulphur dioxide is given off and reacts with iodine in titration vessel bleaching the color from blue to colorless, while undergoing titration with potassium iodate solution. When all the sulphur dioxide formed is absorbed, the blue color no longer fades. The solution color brings us to the endpoint and the readings are noted. Calibration Procedure: Steps: 1) Flow of oxygen is regulated for every test. 2) Titrator is cleaned once in a day. 3) Starch indicator is prepared afresh to ensure no damping property. 4) Daily once, standard rings of known sulphur which is supplied with the instrument from LECO CORPORATION, USA is checked. Page no 22 Calculation: Sample % sulphur 5488 0.007 5470 0.009 Page no 23 DETERMINATION OF BLAINE NUMBER Principle of operation: The sub-sieve sizer operates on the air permeability principle for measuring the average particle size of the Iron ore powder. The principle is based on the fact that a current of air flows more readily through a bed of coarse powder than through an otherwise equal bed of fine powder that is equal in shape of bed, apparent volume. The basic operating principles of the instrument are relatively simple. The air pump builds up air pressure to constant head in the pressure regulator stand pipe. Under the pressure head, the air is conducted to the packed powder sample contained in the sample tube.The flow of air through this packed powder bed is measured by means of a calibrated manometer in which the level of the fluid indicates the average diameter of the powder particles directly on the calculated chart. The average particle diameter may be expressed in terms of Sw; equal to this specific surface of the powder in square centimeters per gram of dry powder, or in terms of So equal to the specific surface of the dry powder in square centimeters per c.c of equal solid materials. These relationships are expressed in the equation; Sw = (6× 10⁴) / (dm ×P) So = (6 ×10⁴) / dm Where dm-Average diameter in Micron taken from calculator. P -Chart density of material from which the powder was made. Sw-Specific surface area in square centimeters per gram of material. So-Specific surface area in square centimeters per CC of solid material. Page no 24 Apparatus used: Fisher sub-sieve sizer model no. 95 Measuring particle size Procedure: Plug the line cord and power switch on and allow the instrument to warm up for 20 minutes to give it a chance to stabilize.While allowing the unit to warm up,perform the Steps..Lay a paper disc over one end of the sample tube, then with the perforated surface of the plug against the surface of the paper disc push one of the two porous plugs about 1/2 inches into the tube, forcing the paper to crump around the edges. Vertically placed the tube in the supplied sample tube stand with the open end up. Weigh out a sample of dry iron ore concentrate equal in grams to the true density of the sample. Transfer the weighted sample into the sample tube. Tap on this side of the tube to settle the Iron ore concentrate. Lay a second paper disc over the open top of the sample tube and force the other porous plug and paper disc down into the tube. Place the sample tube on the brass post with the lower plug touching the upper end of the post .Using the rack and pinion control, lower the rack until the flat bottom end touches the upper plug. Move the calculator chart to the right until the pointer is set at the porosity of 0.80 . using the rack and pinion control, lower the rack until the tip of the pointer on the rack is set on the sample height curve on the chart. Without moving the chart, raise the rack and remove the sample tube, being careful not to disturb the sample. Mount the sample tube between the rubber cushioned supports just to the right of the brass post and twist the clamp assembly control to the right until the tube is locked into place making an airtight seal at both the ends of the tube. Adjust the pressure control selector until the bubble rises in the pressure regulator standpipe at the rate of 2-4 per second. The water level will rise above the water level marks as observed through the water level observation window. This is normal in addition: the liquid level in the manometer tube will rise slowly and reach a maximum height within 30 seconds to several minutes depending on particle size. Page no 25 After the liquid in the manometer reaches its maximum level and without disturbing the calculator chart, turn up the rack until the upper edge of the cross bar coincides with the liquid meniscus in the manometer. Read the particle size of the chart and record the reading. The size is indicated by the location of the tip of the pointer with relation to the curves on the chart. Calculations : Blaine number = 60000/ (avg particle size× specific gravity) Sw = 60000/ (Dm× P) Sample - 5470 %Fe = 63.20 Specific gravity of the sample with 63.2%Fe is 4.5360 Average particle size dm = 11.5 microns Blaine number = 60000/(11.5 * 4.5360) = 1150.2018 4.5360gm of the sample can be spread over 1150.218 sq. cm. area with each particle distinctly separated. Page no 26 METHODS OF TEST FOR BENTONITE 3.1. FREE SWELLING CAPACITY: Procedure: Accurately 2.00g of dried Bentonite powder sample was weighed and sprinkled it slowly with the help of a vibrating spatullar into a graduated cylinder containing 100ml of distilled water (pH=7.0).Care was taken to see that every particle of bentonite is wetted and settled while sprinkled cach time till all the sample has been taken over. Generally time taken for completing the test was 1 to 2 hours. The initial level was recorded after 1 hour and final reading after 24 hours. The volume of gel formed was noted down. This is the Free Swelling Index (FSI) of the Bentonite Calculation: Amount of sample taken =2g Sample 1: Free swelling =27ml Sample 2: Free swelling =29ml Page no 27 3.2. PLATE WATER ABSORPTION TEST: Equipment: Sintered Aluminium Oxide plate 12" x 12"x 1’’ standard medium coarse plate, permeability 19 unit per plate, approximate pore size 164 microns approximate particle retention 68 u.Shallow plastic pan 15" x 18" x2" Glass covers 20" x 22" with a sponge rubber seal strip to a seal against the pan, Hardened filter paper (whatman 50), 9 mm diameter Drying oven controllable to 105c. Balance of 0.001gm sensitivity. Tarred watch glasses 10cm diameter. Thermometer of 0.1c sensitivity.Distilled water. Setting of the equipment: The alumina plate was centrally located in the pan supported by the 1/4" thick inner pads and levels the top of the plate. The pan was filled with distilled water prior to each test to the 1/4" of the top of the plate measuring to the water plate contact. The glass cover was placed on the pan for complete coverage. Inscribe 5cm circles centered on the 9cm filter paper. Noted down the temperature. Procedure: Exactly 2.000gm of processed bentonite was placed, previously dried at 105C for 1 hours, onto the tarred, dry filter paper and spreaded evenly within 5cm circle inscribed upon the 9cm diameter paper. Noted down the temperature (T₁®C). The paper and bentonite was placed on the alumina plate. Upto 6 samples can be placed on the plate at one time. After 18 hours, temperature (T₂® C) was recorded and surface condition of the bentonite. Carefully the filter paper was lifted and placed on a pre weighed watch glass. The watch glass + hydrated paper + hydrated bentonite was weighed. The net weight of the hydrated bentonite was determined by subtracting the watch glass weight and average weight of the hydrated filter paper from the total weight. The moisture absorption as the percent weight gain over the dry bentonite weight was calculated and reported using the calculation below with correction for temperature effects Page no 28 Calculations: Plate Water absorption =(((Ww-W1)/Wd)*100 )-[K (Ta-Tr)] Wd= weight of the sample taken Ww=weight of hydrated sample Page no 29 Ta=average room temperature =22°C Tr=reference temperature =20 °C Sample Trial No. Wd(in gm) W1(in gm) W2(in gm) Ww= (W1-W2) in gm) Plate water bsorption Mean BGS 1 2 1.5050 16.0098 14.5048 618.63 606.48 2 2 1.5050 15.5234 14.0184 594.32 1 2 1.5050 14.2812 12.7762 532.21 2 2 1.5050 14.0275 12.7085 528.825 4177 530.825 Page no 30 SIZE ANALYSIS: Procedure: Exactly 50.00 gms of the dried Bentonite powder was weighed and passed it over the 200# sieve thoroughly with the help of a brush.The sample remaining on the screen was weighed. Calculation: Weight of the sample taken (a)=50 g Weight of the sample remaining on the sieve (b) (200#)=x g Size i.e -200# (%) =( (a b)/50)*100 Weight of sample taken= 50g Sample 1: BGS Page no 31 Blast Furnace Unit Blast Furnace Process The blast furnace is a counter-current gas/solids reactor in which the descending column of burden materials [coke, iron ore and fluxes/additives] reacts with the ascending hot gasses. The process is continuous with raw materials being regularly charged to the top of the furnace and molten iron and slag being tapped from the bottom of the furnace at regular intervals. Page no 32 Key steps of the process are as follows: ● upper part of the furnace - free moisture is driven off from the burden materials and hydrates and carbonates are disassociated. ● lower part of the blast furnace shaft - indirect reduction of the iron oxides by carbon monoxide and hydrogen occurs at 700-1,000°C. ● Bosh area of the furnace where the burden starts to soften and melt - direct reduction of the iron [and other] oxides and carbonization by the coke occurs at 1,000-1,600°C. Molten iron and slag start to drip through to the bottom of the furnace [the hearth]. Between the bosh and the hearth are the tuyeres [water cooled copper nozzles] through which the blast - combustion air, preheated to 900-1,300°C, often enriched with oxygen - is blown into the furnace. Immediately in front of the tuyeres is the combustion zone, the hottest part of the furnace, 1,850-2,200°C, where coke reacts with the oxygen and steam in the blast to form carbon monoxide and hydrogen [as well as heat] and the iron and slag melt completely. Molten iron and slag collect in the furnace hearth. Being less dense, the slag floats on top of the iron. Slag and iron are tapped at regular intervals through separate tap holes. For merchant pig iron production, the iron is cast into ingots; in integrated steel mills, the molten iron or hot metal is transferred in torpedo ladle cars to the steel converters. Slag is transferred to slag pits for further processing into usable materials, for example raw material for cement production, road construction, etc. Page no 33 Blast Furnace principal reactions are: 2C + O2 → 2CO C + H2O → CO + H2 CO2 + C → 2CO 3Fe2O3 + CO → CO2 + 2Fe3O4 Fe3O4 + CO → CO2 + 3FeO FeO + CO → Fe + CO2 When charging the blast furnace, burden materials are added in layers. Charging is done either with an elevator in which a bucket is lifted up and set down on the top of the furnace o be emptied directly into the furnace [bell system] or by conveyor belts to the top of the furnace where materials are charged into a bin fixed to the top of the furnace [bell-less system] and from there into the furnace. By means of a rotating chute it is possible to achieve very uniform distribution of the charge materials across the furnace. The bell-less system has the additional advantage that less energy rich blast furnace gas is lost during charging. The additives and fluxes serve to convert the waste or gangue materials in the charge [mainly silica and alumina] into a low melting point slag which also dissolves the coke ash and removes sulfur. For example: Page no 34 CaCO3 → CaO + CO2 CaO + SiO2 → CaSiO3 FeS + CaO + C → CaS + FeO + CO The blast furnace itself is a steel shaft lined with fire resistant, refractory materials. The hottest part of the furnace - where the walls reach a temperature >300°C - are water cooled. The whole structure is supported from the outside by a steel frame. The blast furnace gas that leaves the top of the furnace is a mixture of carbon dioxide, carbon monoxide, hydrogen and nitrogen and has a calorific value between 3,200 and 4,000 kJ/m³. After cleaning, it is used for a variety of purposes, including heating of the hot blast stoves [“cowpers”], in iron ore agglomeration plants and for electricity generation. The credit for this gas is an important factor in keeping blast furnace operating costs low. BLAST FURNACE AT KIOCL Blast Furnace Unit of KIOCL Ltd. (formerly known as KISCO) was initially promoted as a joint venture by KIOCL Limited, the country's largest 100% EOU located in Karnataka, MECON Limited and MSTC Limited, all Public Sector Undertakings of the Government of India, it was incorporated in June 1995 to give shape to KIOCL's vision to diversify its operation and go into production of value added products. The Plant is situated at 740 50 E Longitude and 120 56' N Latitude and is adjacent to the east boundary wall of Mangalore Chemicals and Fertilizer (MCF) plant. It is erected on Plot No.456 and 457, Baikampady Industrial Area, Panambur, Mangalore-575 010 in a land area of 153.87 Acres. Page no 35 The Blast Furnace Unit commissioned in February 2001, has an annual manufacturing capacity of 2, 16,000 MT of Foundry Grade Pig Iron. The Blast Furnace incorporates state of art technology from M/S Mannesmann Demag, Germany. It was erected and commissioned by their subsidiary M/S INDOMAG Steel Technology Ltd., a member of SMS DEMAG Group, with the detailed engineering support from M/S MECON Limited, India. Activities of the Blast Furnace Unit: BFU produces a premium grade of foundry Pig Iron which is for the production of superior grade and high precision castings. It also produces low phosphorus low sulfur pig iron (SG grade). BFU uses Iron ore from mines of areas like Bellary, Tumkur, Chitradurga and LAM coke from China. The imported coke is transported from NMPT at Panambur to BFU Stock yard by Tippers. The other raw materials like Dolomite, Quartzite, Manganese etc. are sourced from Karnataka. The Plant is equipped with modern facilities to provide safe working conditions. Adequate investments have been made towards environmental control measures to conform to the environment regulation norms. Technological Parameters of Major Equipment Blast Furnace: • Useful volume 350 M3 • Gross hot metal production: 2,25,000 MT/y(with CIO) • Pig iron : MT/y • Specific productivity: 1.85 t/M3 /d(with CIO) • coke rate(dry & net): 650 kg/THM Page no 36 • Slag rate: 231 kg/THM • Hot blast temperature: 10000c • Blast rate:2242 NM3/THM • Top gas kg/cm2 • BF gas / Blast: 1.4 • Furnace shell cooling is by external •water spray with box coolers Page no 37 Captive Power Plant: • Generation capacity: 7 MW (3.5 MW x 2 No.) • Provision for synchronization with grid and also to cater maximum plant load island mode • Steam boiler(2 no.): 25 TPH @ 42 kg/cm2, 4500c • Main fuel: BF gas • Flame stabilization: by LDO/fo • Generator(2No.): 3.5 @ 6.6kv • De-mineralisation plant: 3 streams, 5 M3/hr/stream • Cooling tower: 3 cells,2400 M3/hr • Fuel storage tanks: 170 kl x 2 Top Charging Equipment: Rotating hopper distributor with two bell systems and pressure balancing/relief valves. Bells and valves are operated by a winch-rope drive system. Page no 38 Hot Blast System: Stoves: 3 Nos,Hoogovan type, with vertical ceramic burner, parabolic shaped dome, hexagonal checkers with a high heating surface, which gives 1000 degree centigrade temperature. Hot blast main with isolation valve and bustle main connecting to 12 (twelve) Tuyres (dia. 110 mm) supply blast to the furnace. Hot Metal Tapping: Pneumatically operated rotary drilling system for tap hole opening and hydraulically operated piston/barrel type mud gun for closing the tap hole Slag: Slag is granulated using water jet in granulation system Ladles (8 nos): 35 MT capacity refractory lined ladle to collect & carry hot metal from cast house to pig casting machine. Handled by EOT crane (55/25 MT). Pig Casting Machine: Capacity: 2 no 1000 T/day, with additional new unit of 600 T/day ● Weight of pig: 5-6 kgs/piece ● Ladle tilted with the help of EOT crane at old rn/c and hydraulic tilting in the new M/c. ● Lime splashing system for mold coating ● Water cooling system for pig cooling ● Pig knocking system at new M/c ● Pig collection by wagon at old M/c and tipper collection at new M/c. ● Magnetic crane for unloading the wagon Page no 39 Air Blower (2 no.): Make: Mannesmann Demag ● Capacity: 31500 nm3/hr@ 2.2 kg/cm2 ● Drive: induction motor of 2.25 MW @6.6 KV, 1500 rpm BF Gas Cleaning: ● Cyclonic dust separator ● 2 stage venturi type wet scrubber ● Thickener for sludge removal BF Cooling Water System ● CWPH/MWPH etc. ● Plant automation and control is through PLC (ABB MP 280/1) ● Process Control Laboratory has x-ray spectrometer for metal analysis Main Power Supply & Distribution System: ● Power supply: 110 KV from Mescom grid ● Sanctioned demand: 10 MVA ● Contracted demand: 5 MVA ● Distribution: 110 KV to 6.6 KV by 2 Nos. 16 MVA power transformers ● Power distribution to load centers sub-stations: 415 V ● Inter connected with Captive Power Plant Pig Iron Grades Generally Produced At This Plant: Basic: Si Gp2 : Si 1.25-1.74% Gp3: Si 1.75-1.99% Page no 40 Gp4: Si 2-2.24% Gp5: Si 2.25-2.74% Gp6: Si 2.75-3.24% High Silicon: Si>3.25 Off Grade: Or Mn > 0.70 Weigh Bridge: 2 Nos. of 60t weighbridge of M/S AVERY make Plant Security: At present the plant security is manned by Central Industrial Security Force. SAFETY MEASURES KIOCL is trying its level best for the safety of the workers and engineers working in all departments of the company. Following are the steps taken by the company for the safety of the employees: 1. Compulsory use of the hand gloves while working in repair units. 2. When the repair of any machine in the plant is undertaken, compulsory shut down of the entire plant so as to avoid untoward incidents for working personnel who are repairing the machinery 3. A number of slogans regarding safety is put up everywhere in the campus. For example "PRODUCTION IS MUST, BUT SAFETY IS SUPER MOST". 4. Warning boards are put tip near every machine to avoid hazards. - A fire brigade is always kept ready to fight fire accidents. 5. In case of accidents, a first aid center is made available in the plant for immediate treatment. 6. Compulsory wearing of the helmets in all sections of the industry. Adopting these safety measures, the company is able to reduce the number of accidents in the working area very efficiently. A separate department has been set aside to oversee the proper implementation of safety measures and thus reducing the no of accidents in the plant. Page no 41 SNAPSHOTS : 1) Grinding & Filtration process 2. Palletization process: Page no 42 CONCLUSION: the project carried out at KIOCL Ltd Mangalore, raw materials were analysed for the percentage composition of their constituents. Iron ore and bentonite are two of the component utilized for the manufacture of iron ore pellets. During this training period, we understood that the raw materials like iron ore,bentonite. Coke or coal and the limestone are tested as per prescribed standards like IS, ISO, and ASTM, At different stage of the entire process it is necessary to test these raw materials to estimate its physical and chemical composition for controlling the process and to maintain the product quality as per the standard specification. We got exposure to the basic laboratory techniques and also learnt the good laboratory practices, safe handling of chemicals, personal safety, place safety. we also visited the blast furnace and got to know how it works. In summary, it was a very fruitful experience of getting a chance to work especially in the esteemed industry like KIOCL Ltd. Page no 43 ACKNOWLEDGEMENT The Industrial visit to KIOCL was an excellent and rewarding experience. We have been able to understand the working of an Industry. Before this visit we had never imagined walking around in an industrial plant. sincerely thanks to Mr. Prakash B. V, Head of the Department, (Process Control Dept.), KIOCL, Mangalore, for his interest with our work during our project work and his invaluable guidance and encouragement throughout the time of the training period. I am immensely grateful to Mr. K. Shivaraju, Manager, (Training and Safety) for scheduling our training sessions in a symmetric manner and giving us permissions to carry out our project. Heartily thanks to Mr.Akshay sir(Pellet plant department),Mr.Raveendra sir(Mineral processing department),and Mr.Prashant sir(process control department) for their guidance in industrial training project and kind cooperation during the entire training period for helping us gain procedural knowledge in the company. I wish to express sincere gratitude to Professor P.E. JagadeeshBabu, Head of the Department of Chemical Engineering, National Institute of Technology Karnataka, for providing us an opportunity to undergo Industrial Training at KIOCL, Mangalore in the field of Iron ore pellet making and inspiring us to do this training Page no 44