Introduction to Separation Processes Engr. Ralph John Erwin R. Ornales Department of Chemical Engineering Learning Objectives ◉ ◉ ◉ To categorize different types of separation processes and separation techniques. To learn the role of separation operations in an industrial chemical process. To explain what constitutes the separation of a chemical mixture and enumerate the five general separation techniques. 2 Learning Objectives 3 What is Separation? Separate (definition from dictionary) ◉ To isolate from a mixture; extract ◉ To divide into constituent parts 4 What are Separation Processes? Defined as those operations which transform a mixture of substances into two or more products which differ from each other in composition. ◉ A technique to achieve any mass transfer occurrence that converts a mixture of substances into two or more individual product mixtures. ◉ The specific separation design may vary depending on what chemicals are being separated, but the basic design principles for a given separation method are always the same. ◉ 5 Separation Processes The main goal of separation process is to purify solution. To do this, we must cause different transport of species or convection of species so that the purer mixture can be collected. Most separation processes involve differential transport. 6 Separations The separation of chemical mixtures into their constituents has been practiced, as an art, for millennia. 7 Separations including enrichment, purification, isolation, concentration, and refining, are important to chemists and chemical engineers. ◉ Chemists use analytical separation methods while chemical engineers are more concerned with the manufacture of chemicals using economical, large-scale separation methods. ◉ Separations 8 Why Separation Processes are Important? ◉ Almost every element or compound is found naturally in an impure state such as a mixture of two or more substances. Many times the need to separate it into its individual components arises. ◉ A typical chemical plant is a chemical reactor surrounded by separators. 9 Applications of Separation Processes Raw Materials Physical Transformation Water to distilled water Crude oil to gasoline Air to nitrogen gas ; oxygen gas Coconut oil to cooking oil Limestone to gravel Chemical Transformation Product 1 Product 2 10 Water to hydrogen Crude oil to polyester Air to ethylene glycol (antifreeze) Coconut oil to medicinal oil Limestone to cement Separation Processes The separation technology involved in crude oil reforming includes: ◉ Distillation – separates various chemical component according to volatility. ◉ Alkylation – to react small hydrocarbon molecules to create larger ones ◉ Catalytic reforming – to modify the structure of medium-sized hydrocarbons. ◉ Fluid catalytic cracking – to break apart very large hydrocarbon molecules. ◉ Hydrocracking – to break apart very large hydrocarbon molecules 11 Why Separation? There are many reasons for wanting pure substances. Some of these include: ◉ Need for pure material in engineering applications ◉ Preparation of raw materials into their component ◉ Need for pure material for materials processing ◉ Need to remove toxins or inactive components from solutions (drugs) ◉ Need for ultra-pure samples for testing ◉ Need for analysis of the components of mixture (DNA testing) 12 Examples of Separation Processes ◉ ◉ ◉ ◉ ◉ ◉ ◉ ◉ Separation of blood Purification of drugs Purification of Au, Ag, Ti Refining of crude oil DNA testing Purification of organic material Purification of water Separation of water and waste product of metabolism from kidney 13 1. Industrial Chemical Processes 14 Industrial Chemical Processes A chemical process is conducted in various manners. Feed ◉ Naturally occurring raw materials ◉ Plant or animal matter Operating Mode ◉ Batch wise ◉ Continuous ◉ Semi continuous Operations ◉ Key Operations (chemical reactions, separations) ◉ Auxiliary operations (phase separations, heat addition, heat removal, shaft work addition, shaft work removal, mixing, dividing, etc.) ◉ Chemical intermediates ◉ Chemicals of commerce ◉ Waste products 15 Block-flow Diagrams ◉ Used to represent chemical processes; indicate chemical reaction and separation steps and, by connecting lines, the major process streams that flow from one processing step to another. 16 Base Units 17 18 2. Mechanism of Separation 19 Why Separation is Difficult to Occur? Second Law of Thermodynamics ◉ Substances are tend to mix together naturally and spontaneously. ◉ All natural processes take place to increase the entropy, or randomness of the universe. 20 Mechanism of Separation A schematic diagram of a general separation process is shown. 21 General Separation Techniques 22 How Separations are Achieved? ◉ Enhancing the mass transfer rate by diffusion of certain species relative to mass transfer of all species by bulk movement within a particular phase, with the following considerations which are crucial in separation operations. Rate of Separation – governed by mass transfer Extent of Separation – limited by thermodynamic equilibrium 23 How Separations are Achieved? The extent of separation achieved depends on the following properties of species in the different phases present. 24 3. Separation by Phase Creation or Addition 25 Separation by Phase Creation or Addition If the feed mixture is a homogeneous, single-phase solution, a second immiscible phase must often be developed or added before separation of chemical species can be achieved. ◉ The second phase is created by an energy-separating agent (ESA) and/or added as a mass-separating agent (MSA). ◉ Although separations that use an ESA are generally preferred, an MSA can make possible a separation that is not feasible with ESA. ◉ 26 Disadvantages of MSA ◉ ◉ ◉ ◉ Need for additional separator to recover the MSA for recycle Need for MSA makeup Possible contamination of the product with the MSA More difficult design procedures 27 Partial Condensation or Vaporization ◉ When the feed mixture includes species that differ widely in their tendency to condense or vaporize ◉ Separating agent: heat transfer (ESA) ◉ Example: Recovery of 𝐻2 and 𝑁2 from ammonia by partial condensation and high-pressure phase separation 28 Flash Vaporization ◉ Caused by reducing the pressure of the feed with a valve. ◉ The resulting vapor phase is enriched with respect to the species that are most volatile while the liquid phase is enriched with respect to the least volatile species. ◉ Separating agent: pressure reduction ◉ Example: Recovery of water from sea water 29 Distillation ◉ The ◉ ◉ ◉ ◉ most widely utilized industrial separation technique. When the volatility differences among species are not sufficiently large. Involves multiple contacts between countercurrently flowing liquid and vapor phases. Separating agent: ESA and sometimes work transfer Example: Purification of styrene 30 Extractive Distillation ◉ When volatility differences between species to be separated are so small ◉ Separating agent: Liquid solvent (MSA) and heat transfer (ESA) ◉ Example: Separation of acetone and methanol 31 MSA Absorption ◉ If the feed is all vapor and the stripping section of the column is not needed to achieve the desired operation. ◉ Separating agent: Liquid absorbent (MSA) ◉ Example: Separation of carbon dioxide from combustion products by absorption with aqueous solutions of an ethanolamine 32 Stripping ◉ A liquid mixture is separated, generally at elevated temperature and ambient pressure, by contacting liquid feed with a stripping agent. ◉ Separating agent: Stripping vapor (MSA) ◉ Example: Stream stripping of naphtha, kerosene, and gas oil side cuts from crude distillation unit to remove light ends 33 Azeotropic Distillation ◉ Formation of minimum-boiling azeotropic mixtures ◉ Separating agent: Liquid entrainer (MSA) and heat transfer (ESA) ◉ Example: Separation of acetic acid from water using n-butyl acetate as entrainer to form azeotrope with water 34 Liquid-Liquid Extraction ◉ Widely used when distillation is impractical, especially when the mixture to be separated is temperature-sensitive. ◉ The solvent selectively dissolves only one or a fraction of the components in the feed mixture. ◉ Separating agent: Liquid solvent (MSA) ◉ Example: Recovery of Aromatics 35 Liquid-Liquid Extraction (Two Solvents) ◉ Each solvent has its own specific selectivity for dissolving the components of the feed mixture. ◉ Separating agent: Two liquid solvents (𝑀𝑆𝐴1 and 𝑀𝑆𝐴2 ) ◉ Example: Use of propane and cresylic acid as solvents to separate paraffins from aromatics and naphthenes 36 Leaching ◉ Referred to as solid-liquid extraction ◉ Widely used in the metallurgical, natural product, and food industries. ◉ To promote diffusion of the solute out of the solid and into the liquid solvent. ◉ Separating agent: Liquid solvent ◉ Example: Extraction of sucrose from sugar beets with hot water 37 4. Separation by Barrier 38 Separation by Barrier The use of microporous and nonporous membranes as semipermeable barriers for difficult and highly selective operations is rapidly gaining adherents. ◉ For microporous membranes, separation is effected by differing rates of diffusion through the pores. ◉ For nonporous membranes, separation occurs because of differences in both solubility in the membrane and the rate of diffusion through the membrane. 39 Osmosis ◉ Involves transfer, by a concentration gradient, of a solvent through a membrane into a mixture of solute and solvent. ◉ The membrane is almost nonpermeable to the solute. ◉ Separating agent: Nonporous membrane 40 Reverse Osmosis ◉ Transport of solvent in the opposite direction and is effected by imposing a pressure, higher than osmotic pressure on the feed side. ◉ Separating agent: Nonporous membrane with pressure gradient ◉ Example: Desalination of sea water 41 Dialysis ◉ Transport, by concentration gradient, of small solute molecules, sometimes called crystalloids, through a porous membrane. ◉ Separating agent: Porous membrane with pressure gradient ◉ Example: Recovery of caustic from hemicellulose 42 Microfiltration ◉ Retention of molecules typically in the size range from 0.02 𝑡𝑜 10 𝜇𝑚 ◉ Separating agent: Microporous membrane with pressure gradient ◉ Example: Removal of bacteria from drinking water 43 Ultrafiltration ◉ Retention of molecules typically in the size range from 1 𝑡𝑜 20 𝑛𝑚 ◉ Separating agent: Microporous membrane with pressure gradient ◉ Example: Separation of whey from cheese 44 Pervaporation ◉ The species being absorbed by and transported through the nonporous membrane are evaporated. ◉ Uses lower pressures than RO ◉ Separating agent: Nonporous membrane with pressure gradient ◉ Example: Separation of azeotropic mixtures 45 Gas Permeation ◉ Separation of gas mixtures through membranes, using pressure as the driving force ◉ Separating agent: Nonporous membrane with pressure gradient ◉ Example: Hydrogen enrichment 46 5. Separation by Solid Agent 47 Solid Mass Separating Agent ◉ ◉ ◉ Usually in the form of granular material or packing Acts as an inert support for a thin layer of absorbent or enters directly into the separation operation by selective adsorption of, or chemical reaction with, certain species in the mixture. The active separating agent eventually becomes saturated with solute and must be regenerated or replaced periodically. 48 Adsorption ◉ Used to remove components present in low concentrations in non-adsorbing solvents or gases and to separate the components in gas or liquid mixtures ◉ Separating agent: Solid adsorbent ◉ Example: Purification of p-xylene 49 Adsorption 50 Chromatography ◉ A method for separating the components of a feed gas or liquid mixture by passing the feed through a bed of packing. ◉ Separating agent: Solid adsorbent or liquid adsorbent on a solid support ◉ Example: Separation of xylene isomers and ethylbenzene 51 Ion Exchange ◉ Resembles adsorption in that solid particles are used and regeneration is necessary, however involves chemical reaction. ◉ Separating agent: Resin with ion-active sites ◉ Example: Demineralization of water 52 6. Separation by External Field or Gradient 53 Centrifugation ◉ Establishes a pressure field that separates fluid mixtures according to molecular weight. ◉ Force field or gradient: Centrifugal force field ◉ Example: Separation of uranium isotopes 54 Electrolysis ◉ When water is decomposed into hydrogen at the cathode and oxygen at the anode. ◉ Force field or gradient: Electrical force field ◉ Example: Concentration of heavy water 55 Electrodialysis ◉ Cation and anion-permeable membranes carry a fixed charge, preventing the migration of species of like charge. ◉ Force field or gradient: Electrical force field and membrane ◉ Example: Desalinization of sea water 56 7. Selection of Feasible Separation Processes 57 Important Factors 58 Thanks! ANY QUESTIONS? 59