EXTRACTIA LICHID - SOLIDcadredidactice.ub.ro/gavrilalucian/files/2017/01/EXTRACT... · 2017. 1....
Transcript of EXTRACTIA LICHID - SOLIDcadredidactice.ub.ro/gavrilalucian/files/2017/01/EXTRACT... · 2017. 1....
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EXTRACTIALICHID - SOLID
Aplicatii in industria alimentara
si biotehnologii
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PRINCIPII GENERALE• Definitie:
– solubilizarea preferentiala a unuia sau maimultor componenti ai amestecului de constituenti aflat in solidul supus contactariicu un mediu lichid adecvat (solvent).
• Scopul operatiei:– obtinerea unei solutii concentrate a unui
component valoros dintr-o faza solida;– indepartarea unei faze solide insolubile
dintr-un produs.
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PRINCIPII GENERALE• Metoda de extractie depinde de:
– concentratia solutului in faza solida din care se extrage;
– distributia solutului in solid;– natura solidului;– granulometria solidului.
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PRINCIPII GENERALE• Procesul de extractie L-S decurge in
general in 3 etape distincte:– dizolvarea solutului in solvent (transformarea
de faza a solutului)– difuzia solutului dizolvat in solvent prin porii
solidului catre exteriorul particulei (difuziainterna)
– difuzia solutului dizolvat in solvent prin filmulde solvent care inconjoara granula de solid, catre volumul de solvent (difuzia externa)
• Oricare dintre procese poate fi limitativ
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PRINCIPII GENERALE• Structura celulara a solidelor
(caracteristica materialelor de originevegetala sau animala) incetineste difuzia: peretii celulari induc rezistentesuplimentare la transfer;
• Peretii celulari din sfecla de zaharimpiedica extractia unor componentinedoriti, cu mase moleculare mari [sfeclase marunteste sub forma de “taitei”, a.i. peretii celulari sa fie cat mai putin distrusi.
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VITEZA DE EXTRACTIE• Alegerea extractoarelor = functie de
factorii care limiteaza viteza de extractie;• Difuzia solutului prin porii solidului este
determinanta de viteza:– materialul solid trebuie maruntit a.i. distanta
parcursa de solut sa fie minima;• Difuzia solutului prin filmul de solvent este
determinanta de viteza:– trebuie asigurata agitarea intensa a fazei
lichide marirea vitezei difuziei externe.
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Factorii care influenteaza viteza extractiei
1. Dimensiunea particulelor solide2. Solventul3. Temperatura4. Agitarea
Factorii cei mai importanti
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Dimensiunea particulelor solide• Particule de dimensiuni mici:
– arie interfaciala S-L mare flux de soluttransferat mare
– dificil de separat de faza lichida;– retentie mare de faza lichida.
• Este de dorit ca particulele solide sa aibadimensiuni aproximativ egale toate particulelenecesita acelasi timp de extractie
• Part. cu granulometrii mult diferite: part. cu dimensiuni mici blocheaza interstitiile dintrepart. mari se impiedica patrunderea solventului
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Solventul• Selectivitate ridicata;• Viscozitate scazuta;• Caracteristicile cerute solventilor utilizati
in extractia L-L;
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Temperatura• De regula, solubilitatea materialului extras
creste cu cresterea temperaturii vitezade extractie creste;
• Coeficientii de difuziune cresc cu cresterea temperaturii viteza de extractie creste;
• Uzual, cresterea temperaturii este limitatade considerente secundare (necesitateaevitarii actiunii enzimelor la extractiazaharului, de ex.)
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Agitarea• Cresterea agitarii cresterea turbulentei
cresterea rolului difuziunii turbulentecresterea valorii coeficientilor de
transfer de masa.• Agitarea previne sedimentarea particulelor
solide utilizarea mai completa a suprafetei interfaciale L-S.
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Transferul de masa in extractia L - S• Viteza difuziei interne: greu de estimat in lipsa
unor date privind structura poroasa a solidului;• Viteza difuziei externe:
– M – masa de solut transferata in timpul t;– A –aria interfetei S – L;– b – grosimea stratului limita de lichid care inconjoara
particulele solide;– C – conc. solutului in volumul fazei lichide;– Cs – conc. solutiei saturate in contact cu particulele;– k’ – coeficientul de difuziei (aprox. egal cu coef. de
difuzie prin faza lichida, DL);
( )b
CCA'kdt
dM s −⋅⋅=
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Transferul de masa in extractia L - S• Pentru un proces discontinuu:• V = vol. total al solutiei (pp. constant)
• Timpul “t” necesar ca sol. sa se concentreze de la C0 la o val. oarecare C (daca A = ct. si b = ct.):
dCVdM ⋅=( )
VbCCA'k
dtdC s
⋅−⋅⋅
=
∫ ∫ ⋅⋅⋅
=−−
⇔⋅⋅
=−
C
C
t
0 s
0s
s0
tVbA'k
CCCC
lndtVbA'k
CCdC
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Transferul de masa in extractia L - S• Cand solventul initial este pur, C0 = 0 si:
• sau:
• sau:
• conc. solutiei se apropie exponential de conc. de saturatie.
tVbA'k
CCC
lns
s ⋅⋅⋅
=−
⎥⎦
⎤⎢⎣
⎡⋅⎟⎠⎞
⎜⎝⎛
⋅⋅
−=− tVbA'kexp
CC1
s
⎥⎥⎦
⎤
⎢⎢⎣
⎡−⋅=
⋅⋅⋅
− tVbA'k
s e1CC
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Transferul de masa in extractia L - S• In maj. cazurilor, aria interfaciala A creste
in timpul extractiei;• Daca solutul are pondere f. mare in faza
solida, poate avea loc dezintegrareacompleta a part. solide;
• Desi A creste, viteza extractiei scade = curgerea libear a solventului esteimpiedicata (creste valoarea lui “b”).
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Transferul de masa in extractia L - S• Calculul coeficientilor de transfer de masa:
• N – turatia agitatorului;• d – diametrul recipientului;• ρ – densitatea lichidului;• μ – viscozitatea lichidului;• KL = k’/b – coeficientul global de transfer de
masa.
3ag
5,0
L
62,02
L
L
32
ag
5,0
L
4,125
L
L
1067Repentru D
dN16,0D
dK
1067dNRepentru D
dN107,2D
dK
⋅≥⎟⎟⎠
⎞⎜⎜⎝
⎛⋅ρμ
⋅⎟⎟⎠
⎞⎜⎜⎝
⎛μ
ρ⋅⋅=
⋅
⋅<μ
ρ⋅⋅=⎟⎟
⎠
⎞⎜⎜⎝
⎛⋅ρμ
⋅⎟⎟⎠
⎞⎜⎜⎝
⎛μ
ρ⋅⋅⋅=
⋅ −
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Transferul de masa in extractia L - S• La valori mari ale agitarii, raportul coeficientilor
globali de transfer de masa (KL) si caldura (KT), este independent de turatia agitatorului:
5,0
p
L
T
L
cD77,0
KK
⎟⎟⎠
⎞⎜⎜⎝
⎛
λ⋅⋅ρ=
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Metode de operare si echipamente• Extractie:
– in regim nestationar:• extractie discontinua• extractie semicontinua
– in regim stationar• extractie continua
– utilaje cu contact in trepte– utilaje cu contact diferential
• Tehnici de lucru cuprinse intre doua limite:– pulverizarea lichidului deasupra solidului– imersarea completa a solidului in lichid
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Extractia nestationaraa. Solidul si lichidul se
contacteaza discontinuu in vase cu agitare (solide fine sau moi)
b. Stratul de solid esteparcurs de solventul aflat in curgere (solide tari)
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Extractia nestationara• Tehnica contactarii S - L:
– spalare simpla cu contact unic– spalare simpla cu contact multiplu– spalare in trepte in contracurent– spalare diferentiala in strat fix sau mobil, cu si
fara recirculare de lichid
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Spalarea prin percolare• Pentru
obtinereaproduselorfarm. din plante se utilizeazatancuri de 0,3 – 3 m3;
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Spalarea prin percolare• Extractia uleiului
din seminte de:– floarea soarelui– soia– rapita– palmier– alune de pamant
• cu solventi organici:– fractii petroliere
usoare– tricloretilena– acetona– eter
Corp
Gura deincarcareAgitator
Fundfals
TransmisieGura dedescarcare
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Spalarea prin percolare
Seminte
Abur
Serpentina
Produs
CondensatorDistribuitorde solvent
Solventpur
DescarcaresolideFundperforat
Deversor desolutie
Apa
Solvent si vapori de apa
Instalatie discontinua pentru extractia uleiului din seminte
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Spalarea prin percolareVase cu agitare
utilizate la extractiauleiurilorvegetale:
a) cu agitator verical si bratenecentrate;
b) cu agitator orizontal sibrate centrate;
c) cu vas rotitor.
a
c
b
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Spalarea prin percolare•Cand ∆P la curgerealichidului este mare, tancurile deschise se inlocuiesc cu tancuriinchise, sub presiune = DIFUZOARE (difuzere)•Difuzor din industriazaharului1 - corp; 2 - gura de incarcare; 3 - fund rabatabil; 4 - sitatronconica.
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Spalarea prin percolare
Percolarea sub presiune se poate realizasi in filtre presa cu rame si placi:
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Spalarea discontinua in contracurent• Scop: obtinerea unei solutii cat mai conc. in
component util si a unui reziduu solid cat mai bine spalat.
• Spalarea are loc in sistem Shanks• Sistemul poate functiona cu 6 – 16 vase
avand 4 – 12 m3, asezate:– in cerc– in lant (baterie de spalare)
• Aplicatii: – spalarea taninurilor din coji de copac
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Spalarea discontinua in contracurent• 1 … 6 – percolatoare
/ tancuri cu agitare;
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Spalarea discontinua in contracurent• 1 … 6 – percolatoare /
tancuri cu agitare;
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Spalarea discontinua in contracurent
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Spalarea stationara (continua)• Aplicatii principale:
– extractia uleiurilor vegetale din diferitematerii prime cu solventi organici:• hidrocarburi saturate – fractie C6, • solventi clorurati.
– difuzia zaharului din celulele sfeclei in apa• Denumiri consacrate:
– MISCELA – solutia de ulei in solvent– MARC (SROT) – solidul brut spalat
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Clasificarea extractoarelor continue• Dupa modul de contactare a fazelor:
– cu contact in trepte– cu contact diferential
• Dupa tipul constructiv:– tip transportor:
• orizontal: cu banda, cu cupe (cosuri),• vertical: cu cupe (cosuri), elicoidal• inclinat: elicoidal• carusel (cu celule rotative in plan orizontal)
– rotative;
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Extractoare cu banda orizontala• Extractorul De Smet• Extractorul PTK• Schema de principiu:
Material solid
Marc(Srot)
Solvent
Miscela
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Extractorul De Smet
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Extractorul PTK
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Extractoare orizontale cu cupe• Extractoarele Lurgi• Schema de principiu:
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Extractor Lurgi
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Extractoare verticale• Extractorul Bollmann• Doua circuite de
spalare:– echicurent– contracurent
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Extractoare verticale• Extractorul
Bollmann:detaliu umplere/golirecupe (cosuri)
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Extractoareverticale
• Difuzorul Olier:– 6 coloane– transportor cu lant
prevazut cu discuriperforate pt. transportul taiteilor
– viteza lantului: 0,7 –1 m/min
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Extractoareverticale
• Difuzorul BMA:– elementul de
transport: suprafataelicoidala
– turatia: 0,9 – 1,7 rpm
– viteza taiteilor: 0,25 m/min
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Extractoare verticale• Difuzorul Buchau-Wolf:
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Extractorul cu imersie totala• Extractorul
Hildebrandt:• 3 trsp.
elicoidaleperforate, cu vitezediferite
• util ptr. procesareasolidelorusoare, permeabile.
Solid
SolventExtract
Srot
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Extractorul Bonotto• Extractor
vertical tip coloana
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Extractoare inclinateExtractorul Kennedy1 - celula; 2 - rotor; 3 – palete (lopeti); 4 - stergator padela; 5 - carcasa
Extract
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Extractoare inclinate• Difuzorul DdS
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Extractoare inclinateSolid
Solvent
Srot
Extract
zona de extractie
zona de spalare
zona de desecare
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Extractoare carusel• Extractorul
Rotocel:– modificare a
sistemuluiShanks:
– tancurile de spalare suntmiscatecontinuu;
– un rotor invarte6 – 18 celuledeasupra uneisite fine care sustine solidul
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Extractorul Rotocel
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Extractorul Rotocel
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Extractoare rotative