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    Crystallization Handout

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    Crystallization Handout

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    crystallization handout

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    Crystallization Handout

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    pacoto livingstone

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    of 8
    EE LILLE NSE SNE Ug used, The dried solids are taken out from the bottom Of teeta screw conveyer. The exhaust gases are fed into a cyclone wpm, any fines, Advantages include short drying times (2-20 s) er hheat sensitive products, control of particle size, rapid ty disadvantages are low solids content, maintenance of atom ee ‘product build-up on interior walls. mm Unto /-— Spray chamber X Exhaust gas ~~ tomas —e : \ Te By ‘ ef mL \ Vy) = dy prodvet Fig.6.33 Spray dryer 6.26.4 Drum Dryer Drum dryers are suitable for handlin and for solutions. A drum dryer ¢ hheated internally by steam. The rl slurries or pases of sli fine supensic insists of One or more mal lls which 2 ls are usually 0.6-3.5 m iniameter and 0¢ 5 m in length. The material is died on the outside surface of he drum, 1? contact time between the solid material and hot metal is 61S se, The dys is finally recovered by a kaie scraper from the slowly revoling ll The see of rotation is 1 to 10 rpm. The drum acts partly as an evapenor and party 4 dryet. Such dryers are not used for solutions of salts with lated soli for sluries of abrasive solids that have the tendency to settles and rea hig pressure between the drums. 6.27 CRYSTALLIZATION Crystallization refers to a.soid-tigui are formed within a homogeneous pha\Jt can occur as (I)fomation of so particles in a vapour, (2) formation of sol i particles from abi met nd oxmation of solid crystals from a solution, tion process in which slid particle Film — Seam heated drum Spreader a —=——Feea knife scraper Fig.6.34 Drumdiyer Dry product ‘The process usually involves \wo Steys: concentration of solution and cooling Of solution until the solute conc tratiin becomes greater than its solubility at ‘hat temperature. Then the solute Semés out ofthe solution in the form of pure crystals. Crystallization from solution Ys important industrially because the crystals formed age pure. Itis more convenigst use any material in the erystalline form because it facilitates packaging ay stofge. In commercial crystallization, the 6.28 CRYSTAL GEOMETRY A crystal is a highly organized type of matter, the constituent particles of which are arranged in an orderly and repetitive manner. The constituent particles may be ‘toms, molecules or ions. They are arranged in orderly three dimensional arrays called space lattices. Crystals appear as polyhedrons with sharp comers and flat sides or faces. In case of crystalyaf the sme material, the relative sizes of the faces and edges of different crystals\nay/be different to a very large extent, but the angles between the correspondiny aces of all cyrstals are equal and are characteristics of that material. Hence cn{stals ofa particular material are classified on the basis of the arrangement of the/a2s to which the angles are referred. The seven classes of erysials are cubic, tetyégona) onhorhombic, hexagonal, monoclinic, ticlinic, and trigonal. Depending an the cOvditions under which crystallization orewrs, 8 given material may form crystals ONwo or more diferent classes, 6.29 SUPERSATURATION {Let us consider an equilibrium solution ofa solid and liquid phase. If the equilibrium 's disturbed either by cooling the solution or evaporating some Gf the lguid, the Smount of dissolved solids will exceed the equilibrium concentration and the ‘94m will ry to attain equilibrium by rEhovihg excess solids present in it. The esutting process is called crystalfzation ffnjn solution and the concentation sradiete driving force is called supersaturaiidn<$upersaturation is a measure of Mass, parts solvent paris soute/100 parts : Darts Solote at equiibrium/100 pasts solvent ol fi Crystallization cannot occur without supersaturation, There are Ve basic me, of generating supersaturation. (iii) Vacuum cooling By flashing of feed solution adiabat HCAMY 10 & lower temperature and inducing crystallization by simultaneous cooling ang evaporation of the solvent. Gv) Reaction By chemical reaction with a thiré substance. () Salting Bs 'Y the addition of a third component to change the solubility, relationship. £30. MECHANISM OF CRYSTALLIZATION PROCESS as sign and operation of erystalizing equipment Fequire a knowledge of the Sram at bY Which erytalstprtyand prow, There ae cee Dasic steps in the len eroeeSS Of crystallization fiom a supersanated solution, 7, ‘nucleation and (b) crystal growih, Nif the solytion ist and crystal growth do not occur solution, Nucleation ma Y Occur in three different heterogeneous, s mechanisms: homogeneoug ondary or contact, any, oo Prat 1 Fapid local Mtuatong on cleation Occurs Of the crystals’ such as : wall in mixing, or/foreign Patticles. This 1, eB On the intensity of Ye ot sation, r Seionsryrleaton ecu doy, " Presence of crystals of Ube erystatining etl Brow sa ayer.by ayes i" Sole BREEN yal ne 8 occas in two sep 9), Solute into the crystal lace a (2) surface reaction for absy US inthe presen, the surhices of wane oo" gy MATERIAL AND HEAT BALANCED In (ya sumerac™"* na majority of industrial crystallization processes, the mother liquor (solution) ig the solid crystals are allowed to make contact with each other for along time antcach equilibrium, s0 thatthe mother liquor is saturated a he final temperate rahe process, The final concentration of the solute in the solution, there be obtained from the solubility curve. The yield of crystals from a cr¥* process is then calculated from the ncentration of the sotute, the final temperature, and the solubitity at the final temperature. Jp We Cee of av viscous solution, or if the surface of the crystals exposed to the sol the rate of crystal growth is very slow. This results if a lower ¥! id of cr than expected. When the soh very simple, But when the crystals are hydrated, takes into account some of the water present inthe crys ‘The material balance equation is Pob+ crystals are anhydrous, the matgfial balance calculations “°° “the material balance equation tals as hydrate. (6.86) Solute batance gives Prep = La + Cro (687) where F = feed, kg or a = mother liquor, kg ke/ C= crystals, ke ot ke/h x = weight fraction sol iquid or solid phase In the case of anhydrous crystals, x¢/=\) but for hydrated crystals, xc will be less than 1. owe know that when a compound dissolves, absorption or evolution of heat ‘occurs depending ‘on how its solubility hinges with temperature. There is no heat effect on the dissolution of a compoun ‘whose solubility does not change ‘of dissol 1, at equilibrium the heat of crystallization may be assum be equal to the negative heat of Solution at the same concentration provided ihe hat of dilution from saturation in the solution to infinite dilution is very sm I. This assumption is made since in wef solution data are not commonly available. sr balance in a crystallization process is necessary in order to know the cooling requirements or to determine the final conditions. When the enthalpies for the solution and the various solid phases are available in the form of an to patpy_concentration chart, the heat balance equations oe very simple. ‘Let //; be the enthalpy of the feed sol jemperature and Hy be the enthalpy of the final mixture of crystals and mi iquor at the final perawre. If fy be the enthalpy of water vapour which is formed due to on, then the total heat ‘absorbed, g, may be calculated from the q= y+ Hy) Mh (6.88) sae Woy a ae WY We ay 1g 15 POSRIVE. I 415 NEBAME, DEATHS or given off ; 7 of NagCOy andeuer with a concen, Example 6.20 ot solution consiing 5000 by of Ne ‘ation o125 Wt % Na;CO, is cooled 1 293 K and crystals of No:COy 50 are precip any ‘81299 Ue solubility is 21.5 kg anhydrous/10) kof total wate Caleulste the pick of erst tained 31 5% of the original water in the system evapmtes on cooling 4+ Molecular Weight of NaxCO, = 106 Molecular Weight of 1011,0 = 180 Molecular weight of Na,CO,-10H,0 = 2862 Let W be the kg of water evaporated Tren W = 0.05(5900) = 250 kg Material balance in terms of water gives/ '5000(0.75) = oS 3500 = 0.82302 + 0.6296 (689, ‘Material balance in terms of salt gives stoma oh (GaptSrs) + (gS) +0 =| (eo awed sen fal ssi bd me 12> 2681.8 ig solution ‘ iarcracy Pant 23 Kis 5 te Mesoyioy ne oe average etc of ee Foe a MEK. The heat of sutra 1 sed, sate met MeSOc7H0, Calculate he yd wt eo andmke heat balance Assume a ma wn fee Sra ete + Molecular weight of’ MgSO, 120.35 Molecular weight of 78,0 = Iveta ‘Molecular weight of MgSO,7H\ = 246.49 Here w Matra balance in ems of water gives 2000(0:70) = “(ae)+ oo 100 +355) *¢| 73800 + 051170 Mati blance in terms of sl gives “(eSss)+¢ or, 1400 20004030) "ution toChemicalFrgineering 600 = 026191 + 04882C x os (691) 28 (650), we ae C= 3365 kg of MgSO47H1,0 ensias L = 16685 kg stution este the datum tempertize a8 293 K. The enhany of the feed ny = 2000298) 330 ~ 29) = 216820 3 The heat of solution is 0331x109, S110) 5a targets ‘Then heat of ery jon is +54 KUIig cr or 54(3365) = 18171 “The heat of solution data at 291 K is taken as the heat of solu absorbed, 293K. The (q = -216820 - 18171 = -234991 Since q is negative, heat must be removed. 6.32 CLASSIFICATION OF CRYSTALLIZATION EQUIPMENT ay be classified according to their mode of operation. They may 1wous operation is preferred. ns. Crystallization he method Sf generating super rf e solution with very litle evaporation— stallizers, (2) supersaturation produced by vaporization of the solvent with ne ,— evaporator erysalizers 1g evaporators and (3) supers anand evaporation in adiabaitevaportors vacuum rystalizers. Nn erystlzers producing super edu ann publty ofthe solute must increase considerably he case of common salt, 9 part of the solvent is ‘or large-scale production, supe ‘a vacuuin where the solvent flashes of evaporates such as in produce supersaturation by inducing the hot so} zag ane sotution is cooled a Since various methods OF Prod same type of equipments ¢8: Ks Sad of generating SUPT A tray also be cussified secording to the method of Suspe tion may be employed in the mn according to the ory. Crystallizers the groWing product

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