TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Extraction with Supercritical Fluids:Extraction of Liquid Mixtures

Thomas Gamse

Ass.Prof.Univ.Doz.Dipl.-Ing.Dr.techn.

Department of Chemical Engineering and

Environmental Technology

Graz University of Technology

Inffeldgasse 25/C, A-8010 Graz

Tel: ++43 316 873 7477

Fax: ++43 316 873 7472

Email: Thomas.Gamse@TUGraz.at

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Extraction of Liquid Mixtures

Advantages compared to Solid Materials

continuous process no dead times

higher throughput

fractionation of products

Fundamentals

Design

Applications

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Liquid-Liquid Extraction SCFE

no pressure influence pressure changesdensityviscositysurface tensionphase equilibriumdensity difference

solvent regenerationdistillationre – extractionà energy intensive

simple solvent regeneration

Fundamentals

Design

Applications

Extraction of Liquid Mixtures

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

E 1

Feed

SCF 1

S 1

R 1

EX 1

G 1

Single Stage Extraction

Fundamentals

Design

Applications

Extraction of Liquid Mixtures

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Multi-Stage Cross-Flow Extraction

E 1Feed

SCF1

S 1

E 2

R 1

S 2

E 3

SCF 3R 2

SCF 2

EX 1

EX 2

EX 3

E n

SCF n

S n

EX n

R n-1

R n

G 1

G 2

G 3

G n

S 3

Fundamentals

Design

Applications

Extraction of Liquid Mixtures

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Multi-Stage Cross-Flow Extraction

adjustment ofpressuretemperaturesolvent to feed ratio

for each step

accurate fractionation of substances

Fundamentals

Design

Applications

Extraction of Liquid Mixtures

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

SCF

Feed

Extract

Raffinate

Gas (low P)

Multi-Stage Counter-Current Extraction

Fundamentals

Design

Applications

Extraction of Liquid Mixtures

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Multi-Stage Counter-Current Extraction

SCF

Feed

Extract

Raffinate

Gas (low P)

Reflux

StrippingSection

EnrichingSection

Liquefied Extraction Gas

Fundamentals

Design

Applications

Extraction of Liquid Mixtures

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Multi-Stage Counter-Current Extraction

influence parameters

pressure

temperature

solvent to feed ratio

dispersed – continuous phase

drop size and drop size distribution

amount of reflux

Fundamentals

Design

Applications

Extraction of Liquid Mixtures

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Columns without internals

SCF

SCF + Extract Feed

Raffinate

Spray column

Design of Extraction Columns

Fundamentals

Design

Applications

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

liquidsupercritical fluid

plate with openings

phase contact

Plate Columns

Design of Extraction Columns

Fundamentals

Design

Applications

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Packed Columns

different kind of internals

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

structured packings

Packed Columns

different kind of internals

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Columns with Energy Input

pulsating sieve plate column

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

pulsating column with internals

Columns with Energy Input

pulsating sieve plate column

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

swinging plate column

pulsating column with internals

Columns with Energy Input

pulsating sieve plate column

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

A

19

extract 1 extract 2feedraffinatemodifier

DV

DV

CO 2-tank

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Fundamentals

Design

Applications

Design of Extraction Columns

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

High pressure extraction

Distillation

Distillate (Alcohol)

Raffinate

Extract (aroma substances)

WINE

Alcohol free Raffinate

Alcohol reduced Wine

Applications

Fundamentals

Design

Applications

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Vacuum- distillation

High Pressure

Extraction

Extract = Aroma

Raffinate

Distillate = Aroma + Ethanol

WINE

Ethanol

Alcohol reduced Wine

Fundamentals

Design

Applications

Applications

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

wineCO2 + ethanol

+ aroma

ethanol

CO2 + aroma

aroma

raffinatealcohol reduced

wineCO2

Hig

h P

ress

ure

Ext

ract

ion

Co

lum

n Sep

arat

or

1

Sep

arat

or

2Fundamentals

Design

Applications

Applications

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

0

1

2

3

4

5

6

7

8

9

10

80 90 100 110 120 130 140 150 160 170 180

pressure [bar]

eth

ano

l-co

nce

ntr

atio

n in

raf

finat

e [v

ol %

]PR = 5no reflux

PR = 7,5no reflux

PR = 15no reflux

PR = 30no reflux

PR ... Phase Ratio [kgCO2/kgFeed]

PR = 30with reflux

Fundamentals

Design

Applications

Applications

TUG SOCRATES Intensive Course, 11.SOCRATES Intensive Course, 11.--23.7.2004, Barcelona23.7.2004, Barcelona

Fundamentals

Design

Applications

separation of fatty acids

separation of tocopherols

separation of fish oil esters

fractionation of orange and citrus oil

separation of aromas from whiskey and cognac

Further Applications

Applications