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ESE652 PROCESS CONTROL ii CHAPTER 5.

2 DISTILLATION COLUMN
Introduction 1. A fractionating column is an essential item used in the distillation of liquid mixtures so as to separate the mixture into its component parts, or fractions, based on the differences in their volatilities. 2. Fractionating columns are used in small-scale laboratory distillations as well as for largescale industrial distillations. Laboratory fractionating columns Image 1: Fractional distillation apparatus using a Liebig condenser. The Liebig condenser is the most
basic water-cooled design. The inner-tube is straight, making it cheaper to manufacture.

3. A laboratory fractionating column is a piece of glassware used to separate vaporized mixtures of liquid compounds with close volatilities. It can also be called a fractional column. 4. Most commonly used is either a Vigreux column or a straight column packed with glass beads or metal pieces such as Raschig rings.
a. A Vigreux condenser is a modification of the air condenser. It is usually used as a fractionating column for fractional distillations. Unlike straight-walled columns, a Vigreux column has a series of downward-pointing indentations on the inside wall which serve to dramatically increase the surface area without increasing the length of the condenser. b. Raschig rings are pieces of tube (approximately equal in length and diameter) used in large numbers as a packed bed within columns for distillations and other chemical engineering processes. They are usually ceramic or metal and provide a large surface area within the volume of the column for interaction between liquid and gas or vapour. They form what is now known as random packing, and enabled Raschig to perform distillations of much greater efficiency than his competitors using fractional distillation columns with trays.

5. Fractionating columns help to separate the mixture by allowing the mixed vapors to cool, condense, and vaporize again in accordance with Raoult's law. 6. With each condensation-vaporization cycle, the vapors are enriched in a certain component. A larger surface area allows more cycles, improving separation. This is the rationale for a Vigreux fractionating column or a packed fractionating column. 7. As shown in Image 1, as a liquid mixture in the round bottomed flask is boiled, vapor rises up the fractionating column. The vapor condenses on the glass platforms (known as trays or plates) inside the column, and runs back down into the liquid below and refluxes the upflowing distillate vapor. The hottest tray is at the bottom of the column and the coolest tray is at the top. At steady state conditions, the vapor and liquid on each tray is at equilibrium. Only the most volatile of the vapors stays in gas form all the way to the top. The vapor at the top of the column then flows through the water-cooled condenser, which cools the vapor down until it condenses into a liquid distillate. The separation may be enhanced by the addition of more trays (to a practical limitation of heat, flow, etc.)
a. Reflux is a technique involving the condensation of vapors and the return of this condensate to the system from which it originated. It is used in industrial and laboratory distillations.

Industrial fractionating columns Image 2: Typical industrial fractionating columns 8. Fractional distillation is one of the unit operations of chemical engineering. Fractionating columns are widely used in the chemical process industries where large quantities of liquids have to be distilled. 9. Such industries are the petroleum processing, petrochemical production, natural gas processing, coal tar processing, brewing, liquified air separation, and hydrocarbon solvents production and similar industries but it finds its widest application in petroleum refineries.

10. In such refineries, the crude oil feedstock is a very complex multi-component mixture that must be separated and yields of pure chemical compounds are not expected, only groups of compounds within a relatively small range of boiling points, also called fractions and that is the origin of the name fractional distillation or fractionation. It is often not worthwhile separating the components in these fractions any further based on product requirements and economics.
a. The boiling point of an element or a substance is the temperature at which the vapor pressure of the liquid equals the environmental pressure surrounding the liquid. A liquid in a vacuum environment has a lower boiling point than when the liquid is at atmospheric pressure. A liquid in a high pressure environment has a higher boiling point than when the liquid is at atmospheric pressure. In other words, the boiling point of liquids varies with and depends upon the surrounding environmental pressure. Usually, boiling points are published with respect to atmospheric pressure (1 atm). The boiling point of water is 100 C (212 F) at standard pressure. On top of Mount Everest the pressure is about 260 mbar (26.39 kPa) so the boiling point of water is 69 C. (156.2 F). b. Example: Petroleum is refined to produce petrol and diesel. Fractional Distillation process is used on petroleum and at various temperatures, different by products are formed from it. Petrol and diesel both are derived at varying temperatures during refining process. Petrol is produced at temperature between 35 degrees to 200 degrees while diesel is produced at a boiling point of 250-350 degrees. After distillation, in order to use these byproducts as commercially acceptable petrol and diesel, some blending with other elements has to be done. Petrol is produced first in this process as it is produced at a lower temperature than diesel.

11. Industrial distillation is typically performed in large, vertical cylindrical columns (as shown in image 2) known as "distillation towers" or "distillation columns" with diameters ranging from about 65 centimeters to 6 meters and heights ranging from about 6 meters to 60 meters or more. 12. Industrial distillation towers are usually operated at a continuous steady state. Unless disturbed by changes in feed, heat, ambient temperature, or condensing, the amount of feed being added normally equals the amount of product being removed. 13. It should also be noted that the amount of heat entering the column from the reboiler and with the feed must equal the amount heat removed by the overhead condenser and with the products.
a. Reboilers are heat exchangers typically used to provide heat to the bottom of industrial distillation columns. They boil the liquid from the bottom of a distillation column to generate vapors which are returned to the column to drive the distillation separation.

Image 3: Chemical engineering schematic of a continuous fractionating column

14. Image 3 depicts an industrial fractionating column separating a feed stream into one distillate fraction and one bottoms fraction. However, many industrial fractionating columns have outlets at intervals up the column so that multiple products having different boiling ranges may be withdrawn from a column distilling a multi-component feed stream. The "lightest" products with the lowest boiling points exit from the top of the columns and the "heaviest" products with the highest boiling points exit from the bottom. 15. Industrial fractionating columns use external reflux to achieve better separation of products. Reflux refers to the portion of the condensed overhead liquid product that returns to the upper part of the fractionating column as shown in Image 3. Inside the column, the downflowing reflux liquid provides cooling and condensation of upflowing vapors thereby increasing the efficacy of the distillation tower. The more reflux and/or more trays provided, the better is the tower's separation of lower boiling materials from higher boiling materials. Image 4: Chemical engineering schematic of typical bubble-cap trays in a fractionating column Image 5: Section of fractionating tower of Image 4 showing detail of a pair of trays with bubble caps 16. The design and operation of a fractionating column depends on the composition of the feed and as well as the composition of the desired products. Given a simple, binary

component feed, analytical methods such as the McCabe-Thiele method or the Fenske equation can be used. For a multi-component feed, simulation models are used both for design and operation. 17. Bubble-cap "trays" or "plates" are one of the types of physical devices which are used to provide good contact between the upflowing vapor and the downflowing liquid inside an industrial fractionating column. Such trays are shown in Images 4 and 5. 18. The efficiency of a tray or plate is typically lower than that of a theoretical 100% efficient equilibrium stage. Hence, a fractionating column almost always needs more actual, physical plates than the required number of theoretical vapor-liquid equilibrium stages. 19. In industrial uses, sometimes a packing material is used in the column instead of trays, especially when low pressure drops across the column are required, as when operating under vacuum. This packing material can either be random dumped packing (13" wide) such as Raschig rings or structured sheet metal. Liquids tend to wet the surface of the packing and the vapors pass across this wetted surface, where mass transfer takes place. Differently shaped packings have different surface areas and void space between packings. Both of these factors affect packing performance