Chemical Engineering Department

EXPERIMENT NO.

CRYSTALLIZATION

EXPERIMENT:-

CRYSTALLIZATION

Chemical Engineering Department

CRYSTALLIZATION
INTRODUCTION:Crystallization is an important operation in processing as a method o !oth p"ri ication and o pro#iding crystalline materials in a desired size range$ In a crystal% the constit"ent molec"les% icons or atoms are arranged in a reg"lar manner &ith the res"lt that the crystal shape is independent o size and% i a crystal gro&s% each o the aces de#elops in reg"lar manner$ The presence o imp"rities &ill% ho&e#er% "s"ally res"lt in the ormation o an irreg"lar crystal$ 'enerally large reg"lar crystals are a g"arantee o the p"rity o the material% thro"gh a n"m!er o pairs o materials orm (mi)ed crystals*$ In recent years% techni+"es ha#e !een de#eloped or gro&ing per ect crystals &hich are "sed in the prod"ction o semicond"ctor de#ices% laser !eams% and arti icial gems$ In an energy,conscio"s en#ironment% crystallization can o er s"!stantial sa#ings as a method o separation &hen compared &ith distillation% e#en tho"gh it is more costly to achie#e cooling rather than heating$ This is attri!"ted to the act that the enthalpy o crystallization is m"ch lo&er compared to Enthalpy o #aporization$ The crystallization process consists essentially o t&o stages &hich generally proceed sim"ltaneo"sly% !"t &hich can to some e)tent !e independently controlled$ The irst stage is the ormation o small particles or n"clei% &hich m"st e)ist in the sol"tion !e ore crystallization can start% and the second stage is the gro&th o n"clei$ I the n"m!er o n"clei can !e controlled% the size o the crystals "ltimately ormed may !e reg"lated% and this orms one o the most important eat"res o the crystallization process$ N"clei may orm spontaneo"sly i conditions are s"ita!le% !"t in many cases small seed crystals may !e added and small +"antities o imp"rities may also at as n"clei$ The rate o gro&th o a crystal in a sol"tion is dependent on the temperat"re and concentration o the li+"id at the crystal ace$ These conditions are not generally the same as those in the !"l- o the sol"tion !eca"se a concentration gradient is necessary or the trans er o sol"te to&ards the ace% and a temperat"re gradient or the dissipation o the heat o crystallization$ The pro!lem th"s in#ol#es !oth heat and mass trans er% thro"gh in most cases the heat trans er may !e negligi!le. ho&e#er in the case o melts% the pro!lem is one o heat trans er alone$ Yield of Cryst ls:CRYSTALLIZATION

Chemical Engineering Department

The yield o crystals prod"ced !y a gi#en cooling may !e estimated rom the concentration o the initial sol"tion and the sol"!ility at the inal temperat"re% allo&ing or any e#aporation% !y ma-ing sol#ent and sol"te !alances as ollo&s/ 0or the sol#ent% "s"ally &ater% the initial sol#ent present is e+"al to the s"m o the inal sol#ent in the mother li+"or% the &ater o crystallization &ithin the crystals and any &ater e#aporated or/ &1 2 &3 4 y5R,167R 4 &1E 516

8here% &1 and &3 are the initial and inal masses o sol#ent in the li+"or y is the yield o crystals R is the ratio 5molec"lar &eight o hydrate7molec"lar &eight o anhydro"s salt6 And E is the ratio 5mass o sol#ent e#aporated7mass o sol#ent in the initial sol"tion6 0or the sol"te/ &1c1 2 &3c3 4 y7R 536 8here% c1 and c3 are the initial and inal concentrations o the sol"tion in the terms o mass o anhydro"s salt per "nit mass o sol#ent$ 0rom e+"ation 516/ &3 2 &1 51,E6 , y5R,167R 596

and in e+"ation 536 &1c1 2 c3 :&1 51,E6 , y5R,167R; 4 y7R 5<6 rom &hich the yield% y 2 R&1 :c1,c3 51,E6;7:1,c35R,16; 5=6

>roadly% crystallizes may !e classi ied according to &hether they are !atch or contin"o"s in operation% and contin"o"s crystallizers may !e di#ided into linear and stirred types &hich are re erred to later$ Crystallizer may also !e classi ied according to &hich the s"per sat"ration is achie#ed$ In e#aporati#e crystallizers conditions are appro)imately isothermal% and s"per sat"ration is achie#ed as a res"lt o the remo#al o sol#ent$ In cooling crystallizers% s"per sat"ration res"lts rom lo&ering o the temperat"re o the sol"tion% and this can !e e ected either !y means o e)change o sensi!le heat or !y e#aporati#e cooling. in the latter case% there is a small loss o sol#ent$ E#aporati#e crystallization m"st o co"rse !e "sed &here the sol"!ility sho&s little #ariation &ith temperat"re$

CRYSTALLIZATION

Chemical Engineering Department

The main eat"re o the crystallizer is the method !y &hich the size o the prod"ct is reg"lated% and this is almost entirely dependent on the control o the n"cleation process$ In general% slo& cooling &ill res"lt in the ormation o relati#ely e& and large crystals !eca"se spontaneo"s n"cleation is they ormation o relati#ely e& and large crystals !eca"se spontaneo"s n"cleation is then red"ced% and rapid cooling &ill res"lt in a high rare o n"cleation and a n"m!er o size o crystal$ Crystallizers are generally simple in constr"ction% the only mo#ing part !eing agitators and the scrapers &hich are "sed to -eep the heat trans er s"r ace ree o solids$ The simplest and cheapest type o crystallizer consists o an o!e" t "#$ &hich can !e "sed either as an e#aporati#e or as a cooling crystallizer$ In small scale o !atch processing% s"ch crystallizers are +"ire con#enient !eca"se o their lo& irst cost% simplicity o operation and le)i!ility$ They are too &aste "l o la!or and gi#e too "ne#en prod"ct to !e attracti#e or large scale contin"o"s processing$ AIM:To st"dy the yield o crystals o Sodi"m S"l ate rom its sat"rated sol"tion &ith and &itho"t seeding "sing open tan- type !atch crystallizer$ EXPERIMENTAL SETUP: Open tan- !atch crystallizer &ith ?ac-et 593= mm @ and 1== mm depth% 9 mm thic- ?ac-et ann"als 33$= mm and 3= mm thic- glass &ool ins"lation &ith Al"min"m Cladding6 e+"ipped &ith Remi ma-e gear motor stirrer 5stirring rod 1A mm6% speed reg"lator and sie#e$ 0acility or heating7cooling the content o crystallizer consisting o necessary #al#es% steam trap and piping$ Control Banel consists o Reg"lator or the stirrer$ PROCEDURE: Ta-e a!o"t =,C liter o &ater in the crystallizer$ Start s"pply o steam in the ?ac-et o the crystallizer to heat this &ater and heat it "p to a!o"t CAoC$ A ter achie#ing temperat"re o &ater in the crystallizer in the range o ==,CA oC% slo&ly start adding the Na3SO< and allo& it to dissol#e completely$ Add total o a!o"t =AA,CAA gm o Na 3SO<$ Stop s"pplying the steam to the ?ac-et$ No& start s"pplying the cooling &ater instead o steam to the ?ac-et$ The cooling shall !e achie#ed in the slo&est possi!le manner to limit the n"cleation rate$

CRYSTALLIZATION

Chemical Engineering Department

A ter the content o the crystallizer reaches the temperat"re aro"nd 1A oC% stop circ"lation o the cold &ater and drain the &ater rom the crystallizer "sing drain #al#e$ 0ilter and then 8eigh the &ater collected$ Collect the crystals rom the crystallizer "sing the scraper$ Dry them and &eigh$ Repeat the e)periment in the same manner% !"t add seeds 5 ine po&der6 o Na3SO< &hile cooling operation$

O%SER&ATION:

CRYSTALLIZATION

Chemical Engineering Department

Initial &eight o &ater ta-en 5&16 Initial &eight o Na3SO< added 5m16 2 Temperat"re at &hich dissol"tion ta-es place 0inal &eight o &ater collected 5&36 0inal &eight o Na3SO< collected 5m36 0inal cooling Temperat"re 2

2 gm 2 gm 2 2

gm
o

gm o C

DATA:Dolec"lar &eight o hydrate Na3SO<% 1AE3O 2 933 -g7-gmol Dolec"lar &eight o anhydro"s salt 2 1<3 -g7-gmol Sol"!ility o the anhydro"s salt at 1A oC 2 F$G -g71AA-g &ater CALCULATION:R 2 593371<36 2 3$3H c1 2 5m17&16 2 -g7-g &ater c3 2 A$AFG -g7-g &ater at 3F9oI E 2 &1,&3 Calc"lated y "sing e+"ation5=6$ RESULT/, Yield o crystal &itho"t seeding Yield o crystal &ith seeding 2 2 -g -g

CRYSTALLIZATION