liquid-liquid extraction
TRANSCRIPT
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LIQUID-LIQUID EXTRACTION
An Introduction
4 5 E i se n h o w er D r i v e , S u i te 35 0 , P ara m u s , N J 0 76 52 | Te l : (2 01 ) 26 7 - 86 70 | F a x : ( 20 1 ) 3 68 -8 98 9 | w ww. m o d u l ar p ro c es s . c o m
2
WHO IS ?
Koch Modular Process Systems (KMPS) is a joint venture with Koch-Glitsch LP, one of the world's most prominent suppliers of mass transfer equipment. Koch-Glitsch's parent company is Koch Industries, one of the largest privately held corporations in the United States.
For over 20 years KMPS has successfully designed and constructed mass transfer systems for the worldwide Chemical Processing Industry. Our customer’s rely upon KMPS for our quality products and technical expertise.
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Hierarchy of Separation Technologies
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Typical Applications
When is it prudent to use extraction?
When you want to:• Remove products and pollutants from dilute aqueous streams• Wash polar compounds or acids/bases from organic streams• Separate heat sensitive products• Purify non-volatile materials• Process azeotropic and close boiling mixtures• Avoid a high cost distillation solution
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Industries Using Extraction Technology
Chemical •Washing of acids/bases, polar compounds from organics•Recovery of valuable chemicals from aqueous solutions
Biochemical Processing • Recovery of carboxylic acid from fermentation broths• Recovery of valuable “oil” from algae broths
Effluent Treatment • Recovery of phenol, DMF, DMAC• Recovery of acetic acid from dilute solutions
Pharmaceuticals • Recovery of active materials from fermentation broths• Purification of vitamin products
Polymer Processing • Recovery of caprolactam for nylon manufacture• Separation of catalyst from reaction products
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Industries Using Extraction Technology
Petroleum • Lube oil quality improvement• Separation of aromatics/aliphatics (BTX)
Food • Decaffeination of coffee and tea• Separation of essential oils (flavors and fragrances)
Metals • Copper production• Recovery of rare earth elements
Inorganic Chemicals • Purification of phosphoric acid
Nuclear • Purification of uranium
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Removal of Organics From Water:Distillation vs. Extraction
Organic Compound BP [°C] Water Solu.
[%]Azeotrope
B.P. [°C]AzeotropeWater [%]
Typical Reduction Level
Methylene Chloride 40 2.0 38.1 1.5 < 50 ppb
Acetone 56.2 Infinite Non Azeotropic < 50 ppb
Methanol 64.5 Infinite Non Azeotropic < 50 ppb
Benzene 80.1 0.18 69.4 8.9 < 50 ppb
Toluene 110.8 0.05 85.0 20.2 < 50 ppb
Formaldehyde -21 Infinite Non Azeotropic < 1,000 ppm
Formic Acid 100.8 Infinite 107.1 22.5 < 500 ppm
Acetic Acid 118.0 Infinite Non Azeotropic < 500 ppm
Pyridine 115.5 57 92.6 43 < 10 ppm
Aniline 181.4 3.60 99.0 80.8 < 10 ppm
Phenol 181.4 8.20 99.5 90.8 < 10 ppm
Nitrobenzene 210.9 0.04 98.6 88.0 < 10 ppm
Dimethyl Acetamide 166.1 Infinite Non Azeotropic < 10 ppm
n-Methylpyrrolidone 202.0 Infinite Non Azeotropic < 10 ppm
Disti
llatio
nEx
trac
tion
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Simple Extraction Single Stage
8
4.07.929950MF
SE
7.9299
0.250
0.8
RaffinateinSoluteConc.ExtractinSoluteConc.M
0.21.00.2
FeedinSoluteRaffinateinSoluteU
Fraction Unextracted
Distribution Coefficient
Extraction Factor
A – 99
B – 0
C – 1
100
Feed (F)
A – 0
B – 50
C – 0
50
Solvent (S)
A – 0
B – 50
C – 0.8
50.8
Extract (E)
A – 99.0
B – 0
C – 0.2
99.2Raffinate (R)
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Cross Flow Extraction
LEGEND
A, B Components in feed
C Component in solvent
Rx Raffinate from stage x
Ex Extract (made up of components B & C)
Mx Composition of two phase mixture R1R2R3
R4
E1 E2 E3E4
M1M2M3M4
B
A C
F
C C C CA + B
Feed
E1 E2 E3 E4
F + S = M1 R1 + S = M2 R2 + S = M3 R3 + S = M4
R1 R2 R3 R4
Solvent Solvent Solvent Solvent
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Countercurrent Flow Extraction
F + S = ME1 + R4 = MF + S = E1 + R4
F – E1 = R4 – S = Δ
Equations
NOTE: Extract is made up of components B and C
A
CE1
E2
E3
E4
A + B
Feed R1 R2 R3 R4
Solvent
C
R1
R2R3
R4
E1
B
A
F
ΔM E2
E3E4
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B + C
A
C
A + BFeed (F)
Solvent (S)
Extract (E):Solute Rich Stream
Raffinate (R):Solute Lean Stream
Primary Interface
Continuous Phase
Dispersed Phase
Countercurrent Extraction
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Bench Scale Test Apparatus
Variable Speed Drive
ThermometerBaffle
Tempered Water In
Drain
1 – Liter Flask
Tempered Water Out
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Simple Extraction
Solute Free Basis
𝑋𝐵𝐹=𝑋 𝐵𝐹
𝑋 𝐴𝐹
𝑌 𝐵𝐸=𝑦𝐵𝐸
𝑦 𝐴𝑅+𝑦𝐶𝐸
𝑋𝐵𝑅=𝑥𝐵𝑅
𝑥𝐴𝑅+𝑥𝐶𝑅𝑌 𝐵𝑆=
𝑦𝐵𝐹
𝑦𝐴𝑆+𝑦𝐶𝑆R’
E’
F’
S’
XBF
Graphical Solution
Y
X
YBE
YBS
XBR
Equilibriu
m Curve ->
Slope = m
Operating Line ->
Slope = F’/S’
𝑚=𝑌 𝐵❑
∗
𝑋 𝐵❑∗(Distribution Coefficienton Solute Free Basis )
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Typical LLE Equilibrium Curve
0.000 0.005 0.010 0.015 0.0200.00
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
0.09
Raffinate Composition (Wt. Frac., Solute Free)
Extr
act C
omp.
(Wt.
Frac
., So
lute
Fre
e)
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Graphical Determination of Theoretical Stages95% Solute Extraction, S/F = 1.0 mass basis
0.000 0.020 0.040 0.060 0.080 0.100 0.1200.00
0.02
0.04
0.06
0.08
0.10
0.12
Raffinate Composition (Wt Frac., Solute Free)
Extr
act C
omp
(Wt F
rac.
, Sol
ute
Free
)
1
23
(0.136, 0.114)
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Graphical Determination of Theoretical Stages98% Solute Extraction, S/F = 1.0 mass basis
0.000 0.020 0.040 0.060 0.080 0.100 0.1200.00
0.02
0.04
0.06
0.08
0.10
0.12
Raffinate Composition (Wt Frac., Solute Free)
Extr
act C
omp
(Wt F
rac.
, Sol
ute
Free
)
23
456
(0.136, 0.118)
1
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Kremser Equation
Where: n = Number of theoretical stages requiredxf = Conc. of solute in feed on solute free basisxn = Conc. of solute in raffinate on solute free basisys = Conc. of solute in solvent on solute free basism = Distribution coefficientE = Extraction factor = (m)(S/F)
ELOG
E1
E11
msy
nxm
syfx
LOG
n
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Engineering CalculationsKremser Type Plot
1.00.80.6
0.40.3
0.2
0.10.080.06
0.040.03
0.02
0.010.0080.006
0.0040.003
0.002
0.0010.00080.00060.0005
1 2 3 4 5 6 7 8 10 15 20Number of Ideal Stages
X BR/X
BF =
Fra
ction
Une
xtra
cted
E = 0.3
E = 20
E = 1.3
R’
E’
F’
S’
XB
YBS
XBF
YBE
E: Extraction FactorE = m (S’/F’)
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Typical Extraction System
(A+B)
FeedA+B
C
A+(B+C)
B+C+(A)
A (B+C) B (C)
C(A)
C(A+B)
Extraction
Raffinate
Stripping
Solvent Recovery
Solvent
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Removal of Phenol from Wastewater
ppb Phenol
Extraction
Raffinate
Stripping
Solvent Recovery
Wastewater Feed
0.1 – 8 % Phenol
Raffinate
RecycledSolvent
Extract
PhenolBiological Treatment
Or
Carbon Adsorption
< 1 ppm Phenol
Steam
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Recovery of Acetic Acid from WaterUsing a Low Boiling Solvent
Aqueous Feed
1 - 30 % Acetic Acid
Typical Solvents:Ethyl Acetate
MTBEExtraction
Raffinate
Stripping
Solvent Recovery
Raffinate
RecycledSolvent
Extract
Acetic Acid
Aqueous Raffinate
Steam
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Neutralization/Washing of Acid or Baseor Polar Compounds from Organic Stream
Extraction
Water
Water + Salts
Organic
Caustic (Mild)**
Feed (Organic + Acid) **
**Organic Feed could contain caustic. Mid-Feed would be mild acid.
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Series Extraction
Extractor #1
Extractor #2
Feed
A + B
Extract
B + C
Solvent 1
C Solvent 2
D
ProductB + D
RaffinateA
Extractor 1 & 2 May Differ In:• Temperature• pH• Solvent
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Recovery of Caprolactam
Feed From
ReactionSection
Lactam O
il Ext.
AQ Waste to Discharge
Am. Sulphate Ext.
Am. Sulph. Waste to Discharge
Re-Extraction
Lactam Oil to Recovery
WaterLactam Oil Phase65 – 70% Caprolactam
Ammonium Sulphate Phase2 – 3% Caprolactam
Extract
RaffinateSolvent
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25
Phosphoric Acid Extraction
Extraction
Raffinate to Disposal
Scrub Extraction
Re-Extraction
Phosphoric Acid to Recovery
Water
Solvent
Phosphate Rock DigesterHCL
Feed
Recycle
Scrub Solv.
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Organo-Metallic Catalyst Recovery
Water Effluent(1 ppm Cobalt)
Extraction
Feed
Makeup Organic
CatalystPreparation
Reactor
SeparatorWater Effluent
(200 ppm Cobalt)
Cobalt
Organo-MetallicCatalyst
Product
Slipstream
Organic
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Fractional ExtractionProcess Scheme
NR
NS
XAS2,XBS2
XAF,XBF
XAS1,XBS1
YAE,YBE
XAR,XBR
I2S
I1F
I1S
IE
IR(B-Rich)
(A-Rich)
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Extraction of Flavors and Aromas
Oil
Essential Extract
Extraction
Solvent 1 Distillation
Aqueous AlcoholSolvent 2
Distillation
Essential Oil
Hydrocarbon
Typical Products: Orange OilLemon Oil
Peppermint OilCinnamon Oil
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Fractional LLE – Mixed Polymer Feed
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Major Types of Extraction Equipment
Used primarily in the metals industry due to:- Large flows- Intense mixing- Long Residence time- Corrosive fluids- History
Used primarily in thepharmaceutical industry due to:- Low Volume- Short Residence time- Handles Small Gravity Diff.- History
Static Agitated
Spray Packed Tray Pulsed Rotary Reciprocating
Rarely usedUsed in:- Refining- Petrochemicals
Example:- Random- Structured- SMVPTM
Used in:- Refining- Petrochemicals
Example:- Sieve
Used in:- Nuclear- Inorganics- Chemicals
Example:- Packed- Tray- Disc & Donut Example:
- RDC- SCHEIBEL®
Example:- KARR®
Used in:- Chemicals- Petrochemicals- Refining- Pharmaceutical
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
Mixer Settlers Column Contactors Centrifugal
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Mix / Decant Tank
Characteristics• Mix – Settle – Phase separate in
a single tank• Batch Processing only• Requires multiple solvent
additions for more than one stage (crossflow operation)
• Typically used for small capacity operations or intermittent processing
Feed Inlet
Outlet
Sight Glass
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Mixer / Settlers
Characteristics• Handle very high flowrates• Good for processes with
relatively slow reactions (residence time required)
• Provide intense mixing to promote mass transfer
• Require large amount of floor space
• Suitable when few theoretical stages required
• Large solvent inventory (and losses)
Light Phase In
Heavy Phase Out
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Centrifugal Extractor
Characteristics• Countercurrent flow via centrifugal
force• Low residence time ideally suited for
some pharmaceutical applications• Handles low density difference
between phases• Provide up to several theoretical
stages per unit• High speed device requires
maintenance• Susceptible to fouling and plugging
due to small clearances
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Packed Column
Feed (F)
Solvent (S)
Extract (E)
Raffinate (R)
Characteristics• High capacity:
20-30 M3/M2-hr (Random) 500-750 gal/ft2-hr (Random) 40-80 M3/M2-hr (Structured) 1,000-2,000 gal/ft2-hr (Structured)
• Poor efficiency due to backmixing and wetting
• Limited turndown flexibility• Affected by changes in wetting
characteristics• Limited as to which phase can be dispersed• Requires low interfacial tension for
economic usefulness• Not good for fouling service
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Sieve Tray Column
Feed (F)
Solvent (S)
Extract (E)
PrimaryInterface
Raffinate (R)
Characteristics• High capacity: 30-50 M3/M2-hr
750-1,250 gal/ft2-hr • Good efficiency due to minimum back-
mixing• Multiple interfaces can be a problem• Limited turndown flexibility• Affected by changes in wetting
characteristics• Limited as to which phase can be dispersed• Not effective for high interfacial tension
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RDC Extractor
VesselWalls
Shaft
Stators RotorsLightPhase In
HeavyPhase In
LightPhase Out
HeavyPhase Out
Drive Motor
Gearbox
InterfaceControl
Interface
Characteristics• Reasonable capacity:
20-30 M3/M2-hr• Limited efficiency due to
axial backmixing• Suitable for viscous
materials• Suitable for fouling
materials• Sensitive to emulsions due
to high shear mixing• Reasonable turndown
(40%)
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SCHEIBEL® Column
Characteristics• Reasonable capacity:
15-25 M3/M2-hr 350-600 gal/ft2-hr
• High efficiency due to internal baffling
• Good turndown capability (4:1) and high flexibility
• Best suited when many stages are required
• Not recommended for highly fouling systems or systems that tend to emulsify
LightPhase In
HeavyPhase In
LightPhase Out
HeavyPhase Out
Variable SpeedDrive
InterfaceControl
Interface
VesselWalls
RotatingShaft
TurbineImpeller
HorizontalInner Baffle
HorizontalOuter Baffle
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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SCHEIBEL® Column Internal Assembly
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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KARR® Reciprocating Column
Characteristics• Highest capacity:
30-60 M3/M2-hr 750-1,500 gal/ft2-hr
• Good efficiency• Good turndown capability (4:1)• Uniform shear mixing• Best suited for systems that emulsify
LightPhase Inlet
Sparger
HeavyPhase Inlet
Sparger
LightPhase Out
Interface
Baffle Plate
Tie Rods& SpacersPerforated
Plate
DriveAssembly
InterfaceControl
HeavyPhase Out
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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KARR® Column Plate Stack Assembly
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Comparing Commercial Extractors
1 2 4 6 10 20 40 60 1000.2
0.4.06
1
2
4
6
10
20SCHEIBEL
KARR
RDC
GraesserKuhni
RZE
PFKPSE
FK
MS SE
Effic
ienc
y / S
tage
s pe
r M
eter
Capacity M3/(M2 HR)
Graesser = Raining BucketMS = Mixer SettlerSE = Sieve PlateFK = Random PackedPFK = Pulsed PackedPSE = Pulsed Sieve PlateRDC = Rotating Disc ContactorRZE = Agitated CellKARR = KARR® Recipr. PlateKuhni = Kuhni ColumnSCHEIBEL = SCHEIBEL® Col.
Key
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Column Selection CriteriaStatic Column
A static column design may be appropriate when:
• Interfacial tension is low to medium: up to 10-15 dynes/cm
• Only a few theoretical stages are required, and reduction in S/F is not an economic benefit
• No operational flexibility required
• There is a large difference in solvent to feed rates
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Column Selection CriteriaAgitated Column
Agitated columns are generally more economical when:
• More than 2-3 theoretical stages are required
• Interfacial tension is moderate to high, although low interfacial tensions may also be economical
• A reduction in solvent usage is beneficial to the process economics
• The process requires a wide turndown as well as the ability to handle a range of S/F ratios
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Column Selection CriteriaSCHEIBEL® Column
• Systems that require a large number of stages due to either theoretical stage requirements or low mass transfer rates
• Low volume applications in which a relatively small column is required
• Systems that process relatively easily, without a tendency to emulsify and/or flood
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Column Selection CriteriaKARR® Reciprocation Plate Column
• Difficult systems that tend to emulsify and/or flood easily
• Systems in which the hydraulic behavior varies significantly through length of the column
• Sometimes requiring non-metallic internals, such as Teflon due to wetting characteristics or corrosive materials
• Fouling applications that may have tars formations and/or solids precipitation
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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3 Cornerstones of Successful Extraction Applications
Selection Based on:
• Sound thermodynamic principles• Sound economic principles
• Availability• Recoverability
• Sound environmental principles• Toxicity• Safety
Testing Based on:
• Actual feed stocks• Full process including
solvent recovery• Wide range of operating
conditions
Scale-Up Based on:
• Proven techniques• Proper safety factors
Successful Application
Proper Solvent Selection Meaningful
Pilot Tests
Accurate Scale-Up
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Solvent Selection
• Literature – DECHEMA, Perry’s Chemical Engineers Handbook
• Internet search
• Understanding the chemistry of the process
• Experience – consulting with experts
• Laboratory Experiments:
1. Quickly screen solvents
2. Generate equilibrium data
3. Observe phase behavior
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Liquid-Liquid Extraction Scale-Up
Theoretical scale-up is difficult due to
Complex processes occurring in an extractor• Coalescing / Wetting Characteristics• Interfacial and Drop Turbulence Effects• Axial and Radial Mixing• Tendency to Emulsify• Phase Ratio Variability and Density Gradients• Effects of Impurities or Solids• Mass Transfer Rate
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Liquid-Liquid Extraction Scale-Up
Best method of design: Pilot testing followed by empirical scale-up
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Pilot Plant Configuration
Determine type of column to be used based on process considerationsUse the same kind of equipment for the production unitDetermine diameter and height of pilot column based on experience
Table 1: Smallest Possible Column for Testing
Type of Column Diameter Height
Packed 3” to 4” 3’ to 6’ per Theoretical Stage (TS)
Tray ≥ 6” 4 to 5 Trays per TS
KARR® 1” 1’ to 3’ per TS
SCHEIBEL® 3” 3 to 6 Actual Stages per TS (Approx. 3” to 6”)
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Continuous Extraction Pilot PlantArrangement
Hot Oil
Feed Solvent
Raffinate
Extract
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KMPS Pilot Plant Services Group
KMPS maintains a pilot plant dedicated to extraction R & D and applications testing
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Which Phase is Continuous?
Solvent is Heavy Phase
Primary Interface
FA + B
SC
RA
SolventDispersed
EB + C
Primary Interface
FA + B
SC
RA
SolventContinuous
EB + C
Solvent is Light Phase
F
S
E
R
Primary Interface
A + B
B + C
C
A
SolventDispersed
F
S
E
R
Primary Interface
A + B
C
A
SolventContinuous
B + C
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Determining the Dispersed Phase
Flow Rate (Phase Ratio)• For Sieve Tray and Packed Columns – disperse the higher flowing phase
• For Agitated Columns – disperse lower flowing phase
Viscosity• For efficiency – disperse less viscous phase
• For capacity – disperse more viscous phase
Viscous drop
Diffusion rate inside the drop is inhibited by viscosity
Viscous continuous phase
Drop rise or fall will be inhibited
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Determining the Dispersed Phase
Surface Wetting• Want the continuous phase to preferentially wet the internals – this
minimizes coalescence and therefore maximizes interfacial area.
Importance of maintaining dropletsAssume – 30% holdup of dispersed phase in 1 M3 of solution
Droplets coalesce. Interfacial area lost.
Droplets retain shape. Maximizes interfacial area.
Droplet Diameter [m]
Droplet Volume [M3]
Number Droplets
Droplet SA [M2]
Interfacial Area [M2/M3]
100 0.3 7.16x1010 1.26x10-7 9022
300 0.3 2.65x109 1.13x10-6 2995
500 0.3 5.73x108 3.14x10-6 1796
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Determining the Dispersed Phase
Marangoni Effect• Coalescence is enhanced by mass transfer from
droplets continuous phase
A + B A + BC
A
A + B
C
C + B C + B
C
Mass Transfer Direction
Dispersed Continuous (d c)
• Droplets tend to coalesce
• Must be counteracted by additional energy
Continuous Dispersed (c d)
• Droplets tend to repel each other
• Less energy required to maintain dispersion
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Interface Behavior
Emulsion band builds up at interface due to slow phase separation
Rag Layer
Rag Layer
Solids build up at the interface = Rag Layer
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Rag Layer or Emulsion Band
Corrective Action1. Reverse Phases2. For Emulsion Band: slow down capacity or reduce agitation speed3. For Rag Layer: circulate liquid through an external filter
Filter
Feed
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Entrainment
Entrainment refers to removing a small portion of one phase out of the wrong end of the column i.e. where the other phase exits. Entrainment is controlled by:
1.) Increased settling time inside the column2.) Coalescer inside the column3.) Coalescer external to the column
E
F
R
S
E
R
F
S
F
S
E
R
E
R
F
SOR OR1 2 3
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Flooding
Flooding – the point where the upward or downward flow of the dispersed phase ceases and a second interface is formed in the columnFlooding can be caused by:
• Increased continuous phase flow rate which increases drag on droplets
Primary Interfacef
F1
S
E
R
Primary Interfacef
F2
S
E
R
SecondInterface
F2 > F1
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Flooding
Flooding can be caused by:• Increased agitation speed which forms smaller droplets which cannot overcome
flow of the continuous phase• Decreased interfacial tension – forms smaller drops – same effect as increased
agitation
Primary Interfacef1
F1
S
E
R
Primary Interfacef2
F2
S
E
R
SecondInterface
f2 > f1
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Pilot Plant Testing
Column Selection Based Upon:1. Process Criteria
2. Physical/Chemical Properties
3. Laboratory Work
4. Experience
Test Method5. Experimental Design
6. Step-by-Step Optimization
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Agitated Column Testing
• Set-up column (multiple inlets)
• Select continuous and dispersed phases
• Select initial operating conditions(capacity – S/F – No. Stages)
• Operate at increasing agitation speed (flooding)
• Based on results, vary:
1. Continuous phase
2. S/F vs No. Stages
3. Capacity
4. Other Variables(temp, pH, etc.)
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Static Column Testing
• Set-up column (multiple inlets)
• Select continuous and dispersed phases
• Select initial operating conditions(capacity – S/F – height)
• Operate 3 different capacities
• Based on results, vary:
1. Continuous phase
2. S/F vs Column Height
3. Other Variables(temp, pH, etc.)
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Extractor Flow Patterns
Ideal Plug Flow Actual Flow
This “axial” or “back” mixing causes concentration gradients that decrease driving force and therefore increase HETS
Y
X
Y
X
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Generalized Scale-up Procedure
Pilot Scalef1
Q1
D1
H1
Feed Rate
f2
Q2
Feed Rate
D2Basic Scale-up Relationships:
D2/D1 = K1(Q2/Q1 )^M1
H2/H1 = K2(D2/D1 )^M2
f2/f1 = K3(D2/D1)^M3
Where: K1, M1 = Capacity Scale-up Factors K2, M2 = Efficiency Scale-up Factors K3, M3 = Power Scale-up Factors
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Application – SCHEIBEL® Column
• Extraction of nitrated organics from spent acid stream using an organic solvent
• Reduce nitrated organic compounds from 3.9% to less than 50 ppm
• S/F ratio fixed by process at 3.9
• Equilibrium data indicated that 4.5 theoretical stages required
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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SCHEIBEL® Column Pilot Plant SetupNitrated Organics Extraction
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
Hot Oil
Spent Acid Feed
MCB Solvent
Aqueous Raffinate
Organic Extract
Interface
Variable Speed Drive
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SCHEIBEL® Column Nitrated Organics Extraction
Column designed based upon results from the pilot plant tests:
•Diameter = 14” (D1)
• Expanded Head Diameter = 20” (D2)
• Bed Height = 9’-6” (A)
• Overall Height = 16’-4” (B)A
D1
D2
B
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Application 2 - Recovery of Carboxylic Acids from Fermentation Broth
Broth generated from cellulosic materials – approx. 5% acidsLLE Goal: To achieve >95% recovery (high purity) and minimize solvent usageEthyl acetate selected solvent – but emulsified easily
Preliminary Data in RDC ColumnsDifficult operation due to emulsification< 90% acid recovery High S/F ratio – 2.0
KARR® Column Required
70
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Pilot KARR® Column for Carboxylic Acids 1” diameter x 12’ Plate Stack
71
Hot Oil
Whole Broth Feed Ethyl Acetate
Variable Speed Drive
Aqueous Out
(Raffinate)
Organic Out (Extract Phase)
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Results from Extraction Testing
• Process successfully tested in KARR® Column and data generated for scale-up
• KARR® Column is the correct design for this process which failed in RDC column
• S/F ratio improved to 1.5 (client expected 2)• 96-97% recovery at room temperature and 98-99% recovery at 40-45 C• Complete system (LLE + distillations) designed, fabricated, and installed• LLE testing identified “unknown” component
72KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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KARR® Column DesignCarboxylic Acid Extraction from Broth
• Diameter = 22” (D1)
• Expanded Ends Diameter = 44” (D2)
• Plate Stack = 38’-0” (A)
• Overall Height = 50’-6” (B)
A D1
D2
B
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Application - Aromatic Purification by Fractional Liquid-Liquid Extraction
•Light tar feed with polar aromatics (product) and non-aromatic impurities
•>90% recovery; 1% impurities
•Polar solvent for aromatics
•Alkane for non-polar impurities
•Preliminary Data in RDC ColumnsMany extraction stagesHigh ratio of non-polar to polar solventSignificantly more non-polar solvent stages required
74
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PFD - Pilot Plant Setup: Aromatic Purification by Fractional Extraction
75
Mixed Polar Solvent
Organic Feed
Non-Polar Solvent (Alkane)
Stage 77
Stage 65
Stage 53
Stage 42
Stage 99
Stage 0
Extract Raffinate
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Fraction Extraction Test Variables
• 65-99 agitated stages• 12-34 stages above feed• 42-65 stages below feed• Capacity 21 – 25.5 m3/m2 hr
• Polar solvent to feed ranged between 0.5: 1 and 1.4 : 1• Non-polar solvent to feed ranged between 1.1:1 and 3:1• Agitation speed 400-850 RPM
76
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Aromatic PurificationFinal Results – Design Basis
Scale-up design:Diameter 1778 mm (70”)Height 65 Agitated stagesFeed Stage 13 from topPolar solvent: Feed 0.7: 1.0Non-Polar: Feed 1.8: 1.0Internals = Variable Impeller Diameters94% recovery with <1.0% impurities
77
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Alcohol Extraction from Acrylates
Extraction of methanol from an acrylate stream using water as the solvent
Reduce methanol from 2.5% to less than 0.1%
S/F ratio specified by client as 0.32 wt. basis
Equilibrium data: distribution coefficient generated by KMPS, with average value of 5.3
KARR® Column Pilot Plant SetupAlcohol Extraction from Acrylates
Hot Oil
Water Feed
Acrylate Feed (methyl or ethyl)
Extract(H2O + Alcohol)
Raffinate(Acrylate Phase)
Interface
Variable Speed Drive
KARR® Column
1” Dia. x 8’ Plate Stack
Variable Plate Spacing
Extraction Technology Groupwww.modularprocess.com
Extraction Technology Groupwww.modularprocess.com
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
KARR® Column Pilot Plant Scale-upMethanol Extraction from Acrylate
• Diameter = 45” (D1)
• Expanded Head Diameter = 68” (D2)
• Plate Stack = 26’-0” (A)
• Overall Height = 36’-8” (B)
A D1
D2
B
Extraction Technology Groupwww.modularprocess.com
Extraction Technology Groupwww.modularprocess.com
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Extraction Experience
KMPS has supplied over 300 commercial extraction columns
KMPS has also supplied hundreds of pilot scale extraction columns
We have tested more than 200 different processes in the pilot plant
QUESTIONS?