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Liquid-Liquid Extraction

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Koch Modular Process Systems, LLC. (KMPS) Extraction Technology Group specializes in the design and supply of liquid-liquid extraction equipment engineered to fulfill the chemical, pharmaceutical, petrochemical, biotech and flavor & fragrance industries’ increasingly challenging purification requirements. Our extractor design expertise includes SCHEIBEL® Columns, KARR® Columns, rotating disc contactor (RDC) columns, pulsed, packed (SMVP) and sieve tray.
At KMPS, we don’t just sell extraction equipment; we supply solutions to your difficult separation applications.
KMPS also provides replacements parts, repair services and troubleshooting assistance for all types of extraction columns. A qualified technician or engineer can be provided on-site for both mechanical and process related support.

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Liquid-Liquid Extraction

  1. 1. Telephone: (201) 267-8670 www.modularprocess.com LIQUID-LIQUID EXTRACTION An Introduction 45 Eisenhower Drive, Suite 350, Paramus, NJ 07652 | Tel: (201) 267-8670 | Fax: (201) 368-8989 | www.modularprocess.com
  2. 2. 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.
  3. 3. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Hierarchy of Separation Technologies 3
  4. 4. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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 4
  5. 5. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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 5
  6. 6. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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 6
  7. 7. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 7 Removal of Organics From Water: Distillation vs. Extraction Organic Compound BP [°C] Water Solu. [%] Azeotrope B.P. [°C] Azeotrope Water [%] 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 DistillationExtraction
  8. 8. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Simple Extraction Single Stage 8       4.07.92 99 50M F SE 7.92 99 0.2 50 0.8 RaffinateinSoluteConc. ExtractinSoluteConc. M 0.2 1.0 0.2 FeedinSolute RaffinateinSolute U   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)
  9. 9. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Cross Flow Extraction 9 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 R1 R2 R3 R4 E1 E2 E3 E4 M1 M2 M3 M4 B A C F C C C C A + 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
  10. 10. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Countercurrent Flow Extraction 10 F + S = M E1 + R4 = M F + S = E1 + R4 F – E1 = R4 – S = Δ Equations NOTE: Extract is made up of components B and C A C E1 E2 E3 E4 A + B Feed R1 R2 R3 R4 Solvent C R1 R2 R3 R4 E1 B A F Δ M E2 E3E4
  11. 11. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com B + C A C A + B Feed (F) Solvent (S) Extract (E): Solute Rich Stream Raffinate (R): Solute Lean Stream Primary Interface Continuous Phase Dispersed Phase Countercurrent Extraction 11
  12. 12. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Bench Scale Test Apparatus 12 Variable Speed Drive Thermometer Baffle Tempered Water In Drain 1 – Liter Flask Tempered Water Out
  13. 13. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Simple Extraction 13 Solute Free Basis 𝐹′ = 𝐹 𝑥 𝐴𝑅 𝑆′ = 𝑆 𝑦 𝐴𝑆 𝑦 𝐶𝑆 𝐸′ = 𝐸 𝑦 𝐴𝐸 𝑦 𝐶𝐸 𝑅′ = 𝑅(𝑥 𝐴𝑅 𝑥 𝐶𝑅) 𝑋 𝐵𝐹 = 𝑋 𝐵𝐹 𝑋 𝐴𝐹 𝑌𝐵𝐸 = 𝑦 𝐵𝐸 𝑦 𝐴𝑅 + 𝑦 𝐶𝐸 𝑋 𝐵𝑅 = 𝑥 𝐵𝑅 𝑥 𝐴𝑅 + 𝑥 𝐶𝑅 𝑌𝐵𝑆 = 𝑦 𝐵𝐹 𝑦 𝐴𝑆 + 𝑦 𝐶𝑆 R’ E’ F’ S’ XBF Graphical Solution Y X YBE YBS XBR 𝑚 = 𝑌 𝐵∗ 𝑋 𝐵∗ Distribution Coefficient on Solute Free Basis
  14. 14. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Typical LLE Equilibrium Curve 14 0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.000 0.005 0.010 0.015 0.020 ExtractComp.(Wt.Frac.,SoluteFree) Raffinate Composition (Wt. Frac., Solute Free)
  15. 15. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Graphical Determination of Theoretical Stages 95% Solute Extraction, S/F = 1.0 mass basis 15 0.00 0.02 0.04 0.06 0.08 0.10 0.12 0.000 0.020 0.040 0.060 0.080 0.100 0.120 ExtractComp(WtFrac.,SoluteFree) Raffinate Composition (Wt Frac., Solute Free) 1 2 3 (0.136, 0.114)
  16. 16. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Graphical Determination of Theoretical Stages 98% Solute Extraction, S/F = 1.0 mass basis 16 0.00 0.02 0.04 0.06 0.08 0.10 0.12 0.000 0.020 0.040 0.060 0.080 0.100 0.120 ExtractComp(WtFrac.,SoluteFree) Raffinate Composition (Wt Frac., Solute Free) 2 3 4 5 6 (0.136, 0.118) 1
  17. 17. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Kremser Equation 17 Where: n = Number of theoretical stages required xf = Conc. of solute in feed on solute free basis xn = Conc. of solute in raffinate on solute free basis ys = Conc. of solute in solvent on solute free basis m = Distribution coefficient E = Extraction factor = (m)(S/F) ELOG E 1 E 1 1 m sy nx m sy f x LOG n                              
  18. 18. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Engineering Calculations Kremser Type Plot 18 1.0 0.8 0.6 0.4 0.3 0.2 0.1 0.08 0.06 0.04 0.03 0.02 0.01 0.008 0.006 0.004 0.003 0.002 0.001 0.0008 0.0006 0.0005 1 2 3 4 5 6 7 8 10 15 20 Number of Ideal Stages XBR/XBF=FractionUnextracted E = 0.3 R’ E’ F’ S’ XB YBS XBF YBE E: Extraction Factor E = m (S’/F’)
  19. 19. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Typical Extraction System 19 (A+B) Feed A+B C A+(B+C) B+C+(A) A (B+C) B (C) C (A) C (A+B) Extraction Raffinate Stripping Solvent Recovery Solvent
  20. 20. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Removal of Phenol from Wastewater ppb Phenol Extraction Raffinate Stripping Solvent Recovery Wastewater Feed 0.1 – 8 % Phenol Raffinate Recycled Solvent Extract PhenolBiological Treatment Or Carbon Adsorption < 1 ppm Phenol Steam
  21. 21. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Recovery of Acetic Acid from Water Using a Low Boiling Solvent 21 Aqueous Feed 1 - 30 % Acetic Acid Typical Solvents: Ethyl Acetate MTBE Extraction Raffinate Stripping Solvent Recovery Raffinate Recycled Solvent Extract Acetic Acid Aqueous Raffinate Steam
  22. 22. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Neutralization/Washing of Acid or Base or Polar Compounds from Organic Stream 22 Extraction Water Water + Salts Organic Caustic (Mild)** Feed (Organic + Acid) ** **Organic Feed could contain caustic. Mid-Feed would be mild acid.
  23. 23. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Series Extraction 23 Extractor#1 Extractor#2 Feed A + B Extract B + C Solvent 1 C Solvent 2 D Product B + D Raffinate A Extractor 1 & 2 May Differ In: • Temperature • pH • Solvent
  24. 24. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Recovery of Caprolactam 24 Feed From Reaction Section LactamOilExt. AQ Waste to Discharge Am.SulphateExt. Am. Sulph. Waste to Discharge Re-Extraction Lactam Oil to Recovery Water Lactam Oil Phase 65 – 70% Caprolactam Ammonium Sulphate Phase 2 – 3% Caprolactam Extract Raffinate Solvent
  25. 25. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Phosphoric Acid Extraction 25 Extraction Raffinate to Disposal ScrubExtraction Re-Extraction Phosphoric Acid to Recovery Water Solvent Phosphate Rock Digester HCL Feed Recycle Scrub Solv.
  26. 26. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Organo-Metallic Catalyst Recovery 26 Water Effluent (1 ppm Cobalt) Extraction Feed Makeup Organic Catalyst Preparation Reactor Separator Water Effluent (200 ppm Cobalt) Cobalt Organo-Metallic Catalyst Product Slipstream Organic
  27. 27. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Fractional Extraction Process Scheme 27 NR NS XAS2,XBS 2 XAF,XBF XAS1,XBS1 YAE,YBE XAR,XBR I 2S I 1F I 1S I E I R (B-Rich) (A-Rich)
  28. 28. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Extraction of Flavors and Aromas 28 Oil Essential Extract Extraction Solvent1 Distillation Aqueous Alcohol Solvent2 Distillation Essential Oil Hydrocarbon Typical Products: Orange Oil Lemon Oil Peppermint Oil Cinnamon Oil
  29. 29. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Fractional LLE – Mixed Polymer Feed 29
  30. 30. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Major Types of Extraction Equipment 30 Used primarily in the metals industry due to: - Large flows - Intense mixing - Long Residence time - Corrosive fluids - History Used primarily in the pharmaceutical industry due to: - Low Volume - Short Residence time - Handles Small Gravity Diff. - History Static Agitated Spray Packed Tray Pulsed Rotary Reciprocating Rarely used Used 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
  31. 31. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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 31 Feed Inlet Outlet Sight Glass
  32. 32. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Mixer / Settlers 32 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
  33. 33. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Centrifugal Extractor 33 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
  34. 34. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Packed Column 34 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
  35. 35. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Sieve Tray Column 35 Feed (F) Solvent (S) Extract (E) Primary Interface 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
  36. 36. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com RDC Extractor 36 Vessel Walls Shaft Stators RotorsLight Phase In Heavy Phase In Light Phase Out Heavy Phase Out Drive Motor Gearbox Interface Control 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%)
  37. 37. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com SCHEIBEL® Column 37 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 Light Phase In Heavy Phase In Light Phase Out Heavy Phase Out Variable Speed Drive Interface Control Interface Vessel Walls Rotating Shaft Turbine Impeller Horizontal Inner Baffle Horizontal Outer Baffle KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  38. 38. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com SCHEIBEL® Column Internal Assembly 38 KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  39. 39. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com KARR® Reciprocating Column 39 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 emulsifyLight Phase Inlet Sparger Heavy Phase Inlet Sparger Light Phase Out Interface Baffle Plate Tie Rods & SpacersPerforated Plate Drive Assembly Interface Control Heavy Phase Out KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  40. 40. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com KARR® Column Plate Stack Assembly 40 KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  41. 41. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Comparing Commercial Extractors 41 1 2 4 6 10 20 40 60 100 0.2 0.4 .06 1 2 4 6 10 20 SCHEIBEL KARR RDC Graesser Kuhni RZE PFK PSE FK MS SE Efficiency/StagesperMeter Capacity M3/(M2 HR) Graesser = Raining Bucket MS = Mixer Settler SE = Sieve Plate FK = Random Packed PFK = Pulsed Packed PSE = Pulsed Sieve Plate RDC = Rotating Disc Contactor RZE = Agitated Cell KARR = KARR® Recipr. Plate Kuhni = Kuhni Column SCHEIBEL = SCHEIBEL® Col. Key KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  42. 42. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Column Selection Criteria Static Column 42 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
  43. 43. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Column Selection Criteria Agitated Column 43 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
  44. 44. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Column Selection Criteria SCHEIBEL® 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 44 KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  45. 45. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Column Selection Criteria KARR® Reciprocation Plate Column 45 • 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.
  46. 46. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 3 Cornerstones of Successful Extraction Applications 46 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
  47. 47. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Solvent Selection 47 • 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
  48. 48. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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 48
  49. 49. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Liquid-Liquid Extraction Scale-Up Best method of design: Pilot testing followed by empirical scale-up 49
  50. 50. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Pilot Plant Configuration Determine type of column to be used based on process considerations Use the same kind of equipment for the production unit Determine diameter and height of pilot column based on experience Table 1: Smallest Possible Column for Testing 50 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.
  51. 51. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Continuous Extraction Pilot Plant Arrangement 51 Hot Oil Feed Solvent Raffinate Extract
  52. 52. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com KMPS Pilot Plant Services Group 52 KMPS maintains a pilot plant dedicated to extraction R & D and applications testing
  53. 53. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Which Phase is Continuous? 53 Solvent is Heavy Phase Primary Interface F A + B S C R A Solvent Dispersed E B + C Primary Interface F A + B S C R A Solvent Continuous E B + C Solvent is Light Phase F S E R Primary Interface A + B B + C C A Solvent Dispersed F S E R Primary Interface A + B C A Solvent Continuous B + C
  54. 54. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Determining the Dispersed Phase 54 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
  55. 55. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Determining the Dispersed Phase 55 Surface Wetting • Want the continuous phase to preferentially wet the internals – this minimizes coalescence and therefore maximizes interfacial area. Importance of maintaining droplets Assume – 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
  56. 56. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Determining the Dispersed Phase 56 Marangoni Effect • Coalescence is enhanced by mass transfer from droplets continuous phase A + B A + B C 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
  57. 57. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Interface Behavior 57 Emulsion band builds up at interface due to slow phase separation Rag Layer Rag Layer Solids build up at the interface = Rag Layer
  58. 58. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Rag Layer or Emulsion Band Corrective Action 1. Reverse Phases 2. For Emulsion Band: slow down capacity or reduce agitation speed 3. For Rag Layer: circulate liquid through an external filter 58 Filter Feed
  59. 59. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Entrainment 59 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 column 2.) Coalescer inside the column 3.) Coalescer external to the column E F R S E R F S F S E R E R F S OR OR1 2 3
  60. 60. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Flooding 60 Flooding – the point where the upward or downward flow of the dispersed phase ceases and a second interface is formed in the column Flooding can be caused by: • Increased continuous phase flow rate which increases drag on droplets Primary Interface f F1 S E R Primary Interface f F2 S E R Second Interface F2 > F1
  61. 61. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Flooding 61 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 Interface f1 F1 S E R Primary Interface f2 F2 S E R Second Interface f2 > f1
  62. 62. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Pilot Plant Testing 62 Column Selection Based Upon: 1. Process Criteria 2. Physical/Chemical Properties 3. Laboratory Work 4. Experience Test Method 1. Experimental Design 2. Step-by-Step Optimization
  63. 63. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Agitated Column Testing 63 • 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.)
  64. 64. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Static Column Testing 64 • 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.)
  65. 65. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Extractor Flow Patterns 65 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
  66. 66. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Generalized Scale-up Procedure 66 Pilot Scale f1 Q1 D1 H1 Feed Rate f2 Q2 Feed Rate D2 Basic 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
  67. 67. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Application – SCHEIBEL® Column 67 •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.
  68. 68. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com SCHEIBEL® Column Pilot Plant Setup Nitrated Organics Extraction 68 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
  69. 69. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com SCHEIBEL® Column Nitrated Organics Extraction 69 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
  70. 70. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Application 2 - Recovery of Carboxylic Acids from Fermentation Broth Broth generated from cellulosic materials – approx. 5% acids LLE Goal: To achieve >95% recovery (high purity) and minimize solvent usage Ethyl acetate selected solvent – but emulsified easily Preliminary Data in RDC Columns Difficult operation due to emulsification < 90% acid recovery High S/F ratio – 2.0 KARR® Column Required 70
  71. 71. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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)
  72. 72. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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.
  73. 73. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com KARR® Column Design Carboxylic 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
  74. 74. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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 Columns Many extraction stages High ratio of non-polar to polar solvent Significantly more non-polar solvent stages required 74
  75. 75. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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
  76. 76. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Fraction Extraction Test Variables • 65-99 agitated stages • 12-34 stages above feed • 42-65 stages below feed • Capacity 21 – 25.5 m 3 /m 2 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
  77. 77. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Aromatic Purification Final Results – Design Basis Scale-up design: Diameter 1778 mm (70”) Height 65 Agitated stages Feed Stage 13 from top Polar solvent: Feed 0.7: 1.0 Non-Polar: Feed 1.8: 1.0 Internals = Variable Impeller Diameters 94% recovery with <1.0% impurities 77
  78. 78. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com 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 78
  79. 79. KARR® Column Pilot Plant Setup Alcohol 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 Group www.modularprocess.com Extraction Technology Group www.modularprocess.com KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  80. 80. KARR® Column Pilot Plant Scale-up Methanol 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 Group www.modularprocess.com Extraction Technology Group www.modularprocess.com KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
  81. 81. M O D U L A R P R O C E S S S Y S T E M S | D I S T I L L A T I O N | L I Q U I D E X T R A C T I O N | E N G I N E E R I N G | P I L O T T E S T I N G Telephone: (201) 267-8670 www.modularprocess.com Extraction Experience 81 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?

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