MANUFACTURING OF PHOSPHORIC ACID Presented By Sagar Mahajan Aniket Mali Exam No. B120215939 Exam No. B120215940 BE Chemical Under Guidance of Prof. H L Kamble Department of Chemical Engincering AISSMS College of Engineering, Pune-O1Cer aA Se PP Ses CONTENTS Literature Survey Introduction Selection of Process Process Description Material Balance Energy Balance Equipment Design Cost Estimation Plant Layout Safety Conclusion ReferencesINTRODUCTION > In this project, we are going to analyze the production of phosphoric acid by wet process > Phosphoric Acid is made from Phosphate Rock Figure 1: Structure 3USES >Food-grade phosphoric acid is used to acidify foods and beverages such as various colas »Teeth whiteners to eliminate plaque. >As a chemical oxidizing agent for activated carbon production » As a cleaner by construction trades to remove mineral deposits, cementations smears, and hard water stains > As a pH adjuster in cosmetics and skin-care products >As a dispersing agent in detergents and leather treatmentLITERATURE SURVEY Patent Title Table 1: Literature Surve: Author Patent No Larere ety AE Cry oy Process of manufacturing phosphoric acid Method of manufacturing wet process phosphoric acid Casimer ¢ Wet LegalJr US2504544 Process Pasadena etal Asalchi Matsubar US3416887 Wet aNoshito Process Yasutake Sulphuric acid & phosphate rock Phosphate rock H,SO, P,0,=33% Ca0=45,79% Compasition:- Fluorine=3.66% Moisture=0.70% Conversion = 98% P,0,=40% $0,=2-2.5% H,S0,=15-50%LITERATURE SURVEY continued Paper Title TT a a) Cnr COM Cr Ce Method of Feng Wet Decomposing. Lig-solid ratio-2.3-2.7 preparing wet US7I72742 Process phosphate rock SO; -0.099/1. process etal B2 in sulphuric HsPO,-33-39wt% phosphate acid acid P,0,-30-35% Production=80% Phosphoric M.Gopal PageNo Wet. Phosphate Rock Phosphate Rock- 2.5T Acid Rao 150-153 Process FSO, H,SO, —2.0T (Dryden's CaSO, -2.7T Outline of Chemical Technology, 3"! Ed.)PROPERTIES OF H,PO, > Phosphoric Acid: * Molecular formula : H,PO, * Molecular weight : 98 gm/mole * Melting point : 42.4°C * Boiling point : 213°C * pH: 1.5 (0.1 N aq. sol)SELECTION OF PROCESS » Different process are needed because of different rock and gypsum disposal systems »Two general types of processes are used > Wet Process »>Thermal processWET PROCESS » The processes that use phosphated minerals which are decomposed with an acid, are known as ‘Wet Process’ » There are 3 Types of Wet Processes: > Nitric > Hydrochloric > Sulphuric » The process using sulphuric acid is most common and particularly used for fertilizer grade phosphoric acidREACTION > Main Reaction: 3CaO + P30; — Ca,(PO,), Ca,(PO,), + 3H,SO7—3CaSO, + 2H,PO,SIDE REACTIONS *SO,+H,O — H,SO, *2Ca0+2F, —+ 2CaF, +0, * CaF, +H,SO,+2H,O —~ 2HF+CaSO,.2H,0O * 6HF + SiO, — H,SiF, +2H,O + CaO +H,O — Ca(OH), * Ca(OH), + H,SO, —- CaSO,.2H,O « Al,O, +3H,SO,—- AL(SO,), + 3H,0 + Fe,0,+3H,SO, —-+ Fe,(SO,),+3H,O *CO,+H,O — H,CO,PROCESS FLOW DIAGRAMPROCESS DESCRIPTION » Phosphate Rock: Ground to 200Mesh > Reaction Time: 4 — 6 Hr > 98% conversion >» By-Product: Gypsum(CaSO,.2H,O)MATERIAL BALANCEBASIS FOR MASS BALANCE » 1000 kg/day of Phosphoric Acid > Batch of 8hr > Slurry Feed ratio 1:2.5 > Excess H,SO, =1.4 >98% Ca;(PO,), conversionCOMPOSITION OF ROCK % by mass Table 2: Rock P05 32 CaO. 49 SiO, 3 F 4 Al,O, 2 Fe,0, 2 co, 1 so, a Moisture 1720.05 Kg Rock * = 1925.13 Kg Water t Vent REACTOR 70 — 80°C = 734.67 Kg H,SO, Table 3: Material Balance for Reactor STREAM INPUT ovrper 1 2 3 4 compoxe 20. mae 7 = = P.O: 2464171 = : = Si; 38.5027 7 = F 30.8021 = = ‘ALO: 154011 7 = FeO. 154011 «i 7.005 = = 505 18.4011 = = 10 77008 1925.1933 | 1718 5130 7 1:50. = 734.6667 3.7734 ‘CayPOo, = = 10.7411 = CaS042H:0 = 118.3379 CaF 7 = = o og HPO. HSiFs AlNSOup = = 51.6389 FexS0.) = 38.5027 Fe = = CaAOH: = = 770.0533 __| _2659.8000 serra: 3490-6533 To Filter avce, ==> FILTER Liquid to Sedimentation Tank Table 4: Material Balance for Filter = Gypsum + ‘Waste Assuming 85% Filter efficiency STREAM INPUT OUTPUT 3 5 6 COMPONE! SiO» 22.2910 20.062 2.229 10. 1718.5130 257.777 1460.736 HySO. 3.7734 3.396 0377 Ca3(POs)2 10.7411 9.667 1.074 CaSO..2H20 188.3379 1069-504 118.834 HsPOs 333.3274 = 333.327 H)SiF 38.9080, 38.908 = Al(SO.)3 51.6389) 51.639 = Fe3(SOx)s 38.5027 38.5027 = '3406.0333 1489.456 1916.578 TOTAL '3406,0333 3406.0333 38From Filter To Evaporator Table 5: Material Balance for Sedimentation Tank STREAM INPUT OUTPUT 6 7 8 COMPONEN SiO 2229 2229) 720) 1460.736 20.436 440.300 H3SO; 0377 0377 ‘Cax(PO4)> 1.074 1.074 (CaSOs.2H30 118.834 118.834 HPO. 333.327, S 333.327 1916578 142.950, 173.628 TOTAL 1916578 1916578 19Water Vapours, To 10 Evaporator I From, Sedimentation Tank 483.29 Kg Erp, I u 9 483.29 Kg Table 6: Material Balance for Evaporator 1 STREAM INPUT OUTPUT % STEAM 9 10 1 compo HO 7440.300 = 996.496 | 443.805 = HPO. 333.327 = 333.327 = = STEAM = 483.2913 ms = 483.2513 Terma | 4832013 | 10823 | aas.a0s | aan 2913Water Vapours To 13 Evaporator IL From Evaporator I 483.29 Kg == I 14 42 483.29 Kg Table 7: Material Balance for Evaporator I STREAM INPUT OUTPUT 9 10 12 13 14 COMPO! 120 996.496 _ 552.026 444.470 a H3PO: 333.327 = 333.327 = = VAPOURS. = 443,805, = = 443.805 iaas3 | aas.a05 | 685353 | aaaa7o | aan.aosWater Vapours, To 16 Condenser From Evaporator II 444.47 Kg == mI 17 15 444.47 Kg Table 8: Material Balance for Evaporator I STREAM INPUT OUTPUT iby 13 Is 16 17 éaieraien 70 ssn026 = nxn [wasn | H3PO4 333.327 sae 333.327 ue ma VAPOURS, = 444.470 = - 444.470 885.353 444.470 444.437 440.917, 444.470THERMODYNAMIC PROPERTIES Table ‘Component ‘ABE ‘Specific Heat (KS/Kmol) | (&I/Kmol K) CaQ -635.09 42.09 POs -1506.25_ 60.25 SiO: -909.47608 44.57 Fr. oO 31 ALO; 1669.8 89.76 Fe,0s 824.248 103.7 CO; -413.7976, 37.12 SOs ~441.03544 37.12 HO -285.82996 75.348 H:SO« -813.9972 131,32 Cas(PO»): 410.8216, 277.8 CaSO,. 2H:;0 -2022.62928 99.7 CaF: 1214.6 68.63 Or 0 14.688 HF -271.1232 29.14 HPO, -1271.66 150.3 AL(SOy)s -3440.9 259, Fex(SO,)s -2581.528 272.68 H,COs 699.65, 27.98 Ca(OH); 986.1683 87.5 2BGIBBS ENERGY OF REACTION Ca,(PO,), + 3H,SO, +H,O ——+ 3CaSO,.2H20+ 2H;PO, » Formula: AGrg = Y(pi X AGfi)product — L(t X AGfi)reactant where AGg; = Gibbs free energy of i'* component Pj = Stoichiometry of Product + AGra = [(3 X-1797.44) + (2 x -1111.68)] — [(1 x -3884.84) + (3 x -690.06) + (6 x —237.18)] * AGrR = -237.58KJ/Kmol * Reaction is feasibleENERGY BALANCE > Base Temperature : 298 KHEAT OF REACTION Table 10: Total Heat of Reaction for 1 Batch Reaction ‘Heat of Reaction RL -1230.873, R2 ~567.022 R3 “16.774 SL ~469.741 S2 “955.854 S3 123.22 S4 -28.17463284 SS, -16.63 ed “0.004 s7 “65.015, Ss -221.664 -3448.529 +. —AHp = 3448.526 KI 26t Vent 2k EZ REACTOR —, ook mp, 70°C “x Table 11: Total Heat of Reaction for | Batch STREAM INPUT (KJ) OUTPUT (KJ) 1 214536.982 = 2 24611.333 = 3 = 595476.564 4 ~ 176.187 ring 3448528087 242596.844 596652.751 Heat to be Added by Jacket = 354055.907 KJ Steam of 105°C is used at 0.64 Kg/min-batchGypsum From . — ==: FILTER =» 343K 339.5 K Assuming 5% 339.5 K Energy Loss Liquid to Sedimentation Tank Table 12: Energy Balance for Filter STREAM INPUT (KJ) OUTPUT KJ) 3 595476 564 — 5 = 120294.879 6 = 445407.856 TOTAL 595476564 565702.735 28From Filter 339.5 To TANK Pre-Heater J 337.5 K Assuming 3% 8 Energy Loss 337.5 K Table 13: Energy Balance for Sedimentation Tank STREAM INPUT (KJ) OUTPUT KD) 6 445407.856 = 7 = 421882858 3 = 10162.763, TOTAL 445407856 432045.621MULTIPLE EFFECT EVAPORATOR First Effect: WA, + Wp(t-t,) = WA, Second Effect: W,A, + (W;-W, )(t,-t) = WA, Second Effect: W,A, + (W)-W)-W,)(t-t:) = W3A; W-W,-W,-W; = Wp Table 14: Energy Balance for MEE Effect_| Steam Chest Pressure aP ‘Temperature & Vapours Out Bar Bar c KJ/Kg Kg 1 1.84 117.8 | 2207.37 | 443.80 2 1.27 0.57 106.7 | 2235.29 | 444.47 3 0.70 0.57 90.0 2281.81 | 440.92 |Condenso1 0.13 0.57 51.7 2377.172 Steam Supplied: 483.2913 Kg Vapours Out: 1329.191 Kg Average Heat Transfer Area Required = 36m? Steam Economy: 2.75DESIGN OF EQUIPMENTSDESIGN OF REACTOR >We calculated the total volume of input material > Volume of reactor is taken in 10% excess > Diameter, Height and Thickness of reactor sk assuming > = 1.5 > Various stability checks >Total weight of the reactor> Volume of cylinder = 7R?H >Weight = 1DHtp >Tangential Stress = f, = a . PXD; »Stress due to Internal Pressure = f, = ~ . w » Stress due to Weight = f2 = TbeDx Pfa=fith > fe = LA? — fifa + fa” + 3f,7)°°REACTOR SPECIFICATIONS Table 15: Design of Reactor Volume (in°) 27.096 Height (mm) 4266 Di (mm) 2844 D. (mm) 2850 t (mm) 6 Fx (mm?) 13.09 Fa (N/mm) 13.13 Weight (Kg) 2133.89DESIGN OF SLUDGE SEPARATOR » Calculated the total volume of input material >» Volume of tank is taken in 20% excess »Calculations same as for reactor > Diameter, Height and Thickness of tank assuming —=1.5 DSLUDGE SEPARATOR SPECIFICATIONS Table 16: Design of Sludge Separator ‘Volume (m*) 2.03 Height (mm) 1800 Di (mm) 1200 D, (mm) 1206 t (mm) 6 Fx (N/imm') 13.61 Fa (N/mm) 13.97 ‘Weight (Kg) 324.81DESIGN OF EVAPORATOR > We calculated number of tubes required. > Pitch of tube: 75mm (Triangular) mann p=09 > Area of Central down-take = 40% of CSA (Tubes) » Diameter of Tube Sheet > Thickness of Calendria > Thickness of Tube Sheet — _Fsxts(Do-ts) _ K eK = E,XNexty (Det) a= aj 24+3(K) >tys = F X Dy x — A=> Area of Drum >Rg =—4 — Ry =0.8 0.0172 » Thickness of Vapour Space. > Design for all 3 evaporators will remain same > As the heat transfer area required is equal.EVAPORATOR SPECIFICATIONS Table 17: Tubes and Calendria Specifications Heat Transfer Area Required (im?) 36 Tube OD (mm) 50 Tube Thickness (mm) 15 Tube Length (mm) 1220 No of Tubes 197 Weight of Tubes (Kg) 475.44 Tube Sheet Pitch (mm) 75 (Triangular) Central Down Take OD (mm) 450 Tube Sheet Area (m?) 1.225 Tube Sheet Diameter (mm) 1250 Tube sheet Thickness (mm) 20 Weight of 2 Tube Sheets (Kg) 385.1, Calendria Calendria Thickness (mm) 10 Calendria Length (mm) 1300 Weight of Calendria (Kg) 400.5Table 18: Vapour Space and Head Specifications Vapour Space Vapour Flow Rate (m°/sec) 0.1 Volume of Vapour Space (m') 0.22 Ra 0.8 1. Cylinder Diameter (mm) 630 Length (mm) 350 Thickness (mm) 14 2. Frustum Radius (R) (mm) 1250 Radius (©) (mm) 315 Height (mm) 153 Thickness (mm) 14 fy (Kg/cm?) 79.80 Top Head Thickness (mm) 14 Height (mm) 265 Weight (Kg) 30.1 Bottom Head Thickness (mm) 14 Height (mm) 575 Weight (Kg) 192.4yh FEDS FRQRMACED AG MM RA AAA Gh Figure 2: CFD — Geometry of EvaporatorCOST ESTIMATIONEQUIPMENT COST Table 19: Material Cost Material see Se | Low Carbon Steel Brass Cost per Kg 250 175 350 Table 20: Equipment Cost Equipment Cost (in 3) Reactor 736190 Sedimentation Tank 130736.50 Multiple Effect Evaporators 1741596 Rotary Vaccum Filter 250000 Total 2858522.5 Final Equipment Cost is 30% excess for supports, pumps, etc. Therefore, FCE = 1.3 x 2858522.5 = 3716079.3TOTAL CAPITAL INVESTMENT > Fixed Capital (FCI > Working Capital (WCI) TCI = FCI + WCI = 24773862 +17279693 = & 4,20,53,555TOTAL PRODUCT COST > Manufacturing Cost >General Expenses TPC = Manufacturing Cost + General Expenses = 24773862 +17279693 = & 1,50,93,453INCOME » Selling Price of H,PO,(SP)= = 80 » Operating Time = 330 Days/Year »Capacity of Plant= 1000 Kg/Day >Taxes = 30% of GP Income = SP X Capacity x Cycles = 80 x 1000 x 330 = 2 2,64,00,000 Gross Profit (GP)= Income — TPC = & 1,13,06,547 Net Profit = GP — Taxes = % 79,14,583RATE OF RETURN & PAYOUT PERIOD Rate of Return: Net Profit r= ———__—_——_ x Total Capital Investment = 4583 100 = 18.82% ~ 42053555.8 enemas Pay-out Period: Total Capital Investment ~ Net Profit + Depreciation = 5.08 YearPLANT LAYOUT> After the process flow diagrams are completed and before detailed piping, structural, and electrical design can begin, the layout of process units in a plant must be planned > This layout can play an important part in determining construction and manufacturing costs > Must be planned carefully with attention being given to future problems that may ariseThe principal factors to be considered are :- > Operational convenience and accessibility > Economic distribution of utilities and services > Type of buildings and building-code requirements > Health and safety considerations > Waste-disposal requirements > Auxiliary equipment > Space available and space required » Roads and railroads > Possible future expansionRew Materia Storage si Howse ‘SalfParking Main Plant | uopesisncopy ‘Visors Parking Figure 3: Plant LayoutSAFETY» Keeping the number of incidences and accidents zero > Having a robust and dynamic safety program > Major Hazard is Fire > Using inherently safe equipment > Carrying out independent audit from competent organizations » Abide by all the Govt. laws and hold sacred all the engineering ethics > Regular training and drill of the employees and workers > Creating safety policies > Developing and monitoring safety programsCONCLUSIONS * Wet process was selected for the production of Salicylic Acid. * Production capacity was selected as 1 Ton/Day after studying supply and demand data. * From analysing the residence time of the process, three batches per day were selected. * Energy balance was done for entire process. * Design of the equipments was done. * Costing of equipments was done. * Plant layout is drawn.REFERENCES > R K Sinnott , “Chemical Engineering Design,” 4" ed., Elsevier Butterworth-Heinemann (2005) > J P Holman, “Heat Transfer”, 6" ed., McGraw Hill Book Company (1986) > Donald Q Kern, “Process Heat Transfer,’ McGraw Hill Book Company (1988) > Robert H. Perry, “Perry's Chemical Engineers' Handbook,” 8" ed., McGraw Hill (1934) > V. V. Mahajani and S. B. Umarji, “Joshi’s Process Equipment Design”, 5" edition, Trinity Publications.THANK YOU