Difference between revisions of "Fractional distillation" - New World Encyclopedia

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'''Fractional distillation''' is the separation of a mixture into its component parts, or fractions, such as in separating [[chemical compound]]s by their [[boiling point]] by heating them to a temperature at which several fractions of the compound will evaporate. It is a special type of [[distillation]]. Generally the component parts boil at less than 25°C from each other under a pressure of one atmosphere ([[atmosphere (unit)|atm]]). If the difference in boiling points is greater than 25°C, a [[Distillation#Simple distillation|simple distillation]] is used.  
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'''Fractional distillation''' is a special type of [[distillation]] designed to separate a mixture of two or more [[liquid]]s that have different [[boiling point]]s. The process involves heating the mixture and partial condensation of the vapors along a column ''(fractionating column)'', which is set up such that components with lower boiling points pass through the column and are collected earlier than components with higher boiling points. Generally, this method is used when the component parts boil at less than 25 °C from each other under a pressure of one atmosphere ([[atmosphere (unit)|atm]]).<ref>If the difference in boiling points is greater than 25 °C, a simple [[distillation]] method is used.</ref>
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The separation [[technology]] of fractional distillation is useful in both research and industrial settings. In industry, it is commonly used in [[oil refinery|petroleum refineries]], [[chemical plant]]s, and [[natural gas]] processing plants. Likewise, if a sample of [[air]] is liquefied, it can be separated into its components to produce liquid [[oxygen]], liquid [[nitrogen]], and [[argon]]. Also, [[chlorosilane]]s can be distilled to produce high-purity [[silicon]] for use as a [[semiconductor]].
  
==Laboratory setup==
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== Fractional distillation in a laboratory ==
Fractional distillation in a laboratory makes use of common laboratory glassware, as well as some single-purpose items like a [[fractionating column]].
 
  
 
===Apparatus===
 
===Apparatus===
[[Image:Fractional distillation lab apparatus.png|thumb|300px|Fractional distillation apparatus using a [[Liebig condenser]]. A [[conical flask]] is used as a receiving flask. Here the distillation head and [[fractionating column]] are combined in one piece.]]
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[[Image:Fractional distillation lab apparatus.png|thumb|300px|An example of a fractional distillation apparatus used in a laboratory. The diagram shows the use of a [[Liebig condenser]] and a [[conical flask]] as a receiving flask. Here, the distillation head and [[fractionating column]] are combined in one piece.]]
  
*heat source, such as a [[hot plate]] with a bath
+
A laboratory setup for fractional distillation often involves use of the following pieces of apparatus, put together as shown in the image on the right:
*distilling flask, typically a [[round-bottom flask]]
 
*receiving flask, often also a round-bottom flask
 
*[[fractionating column]] ([[Vigreux column]])
 
*distillation head
 
*[[thermometer]] and adapter if needed
 
*[[Condenser (heat transfer)|condenser]]
 
**[[Liebig condenser]],
 
**[[Graham condenser]], or
 
**[[Allihn condenser]]
 
*vacuum adapter (not used in upper right image)
 
*[[boiling chip]]s, also known as anti-bumping granules
 
*[[rubber bungs]], unless [[laboratory glassware]] with [[ground glass joint]]s is used, such as a [[quickfit apparatus]].
 
  
===Discussion===
+
* a heat source (such as a [[hot plate]] with a bath)
As an example, consider the distillation of a mixture of [[water]] and [[ethanol]]. Ethanol boils at 78.5&nbsp;°C while water boils at 100 °C. So, by gently heating the mixture, the most volatile component will concentrate to a greater degree in the vapor leaving the liquid.  Some mixtures form [[azeotrope]]s, where the mixture boils at a lower temperature than either component.  In this example, a mixture of 96% ethanol and 4% water boils at 78.2 °C, being more [[Volatility (chemistry)|volatile]] than pure ethanol. For this reason, ethanol cannot be completely purified by direct fractional distillation of ethanol-water mixtures.
+
* a distilling flask (typically a [[round-bottom flask]])
 +
* a receiving flask (often a round-bottom flask or conical flask)
 +
* a [[fractionating column]] ([[Vigreux column]])
 +
* a distillation head
 +
* a [[thermometer]] and adapter if needed
 +
* a [[Condenser (heat transfer)|condenser]] ([[Liebig condenser]], [[Graham condenser]], or [[Allihn condenser]])
 +
* a vacuum adapter (for distillations under reduced pressure)
 +
* [[boiling chip]]s (also known as anti-bumping granules)
 +
* [[rubber bungs]], unless [[laboratory glassware]] with [[ground glass joint]]s is used, such as a [[quickfit apparatus]].
  
The apparatus (the diagram represents a batch apparatus, as opposed to a continuous apparatus) is assembled as in the diagram. The mixture is put into the round bottomed flask along with a few [[Boiling chip|anti-bumping granules]], and the [[fractionating column]] is fitted into the top. As the mixture boils, vapor rises up the column. The vapor [[Condensation|condenses]] on the glass platforms, known as [[theoretical tray|trays]], inside the column, and runs back down into the liquid below, [[reflux]]ing distillate. The column is heated from the bottom. The efficiency in terms of the amount of heating and time required to get fractionation can be improved by insulating the outside of the column in an insulator such as wool, aluminium foil or preferably a vacuum jacket. The hottest tray is at the bottom and the coolest is at the top. At steady state conditions, the vapor and liquid on each tray are at ''[[vapor-liquid equilibrium|equilibrium]]''. Only the most volatile of the vapors stays in [[gas]]eous form all the way to the top. The vapor at the top of the column, then passes into the condenser, which cools it down until it liquefies. The separation is more pure with the addition of more trays (to a practical limitation of heat, flow, etc.) The condensate that was initially very close to the azeotrope composition becomes gradually richer in water. The process continues until all the ethanol boils out of the mixture. This point can be recognized by the sharp rise in temperature shown on the [[thermometer]].
+
=== Procedure ===
  
In laboratory distillation, several types of condensers are commonly found. The [[Liebig condenser]] is simply a straight tube within a [[water jacket]], and is the simplest (and relatively least expensive) form of condenser. The [[Graham condenser]] is a spiral tube within a water jacket, and the [[Allihn condenser]] has a series of large and small constrictions on the inside tube, each increasing the surface area upon which the vapor constituents may condense.
+
The apparatus is assembled as in the diagram (which represents a batch apparatus, as opposed to a continuous apparatus). The mixture is put into a round-bottom flask along with a few [[Boiling chip|anti-bumping granules]], and the [[fractionating column]] is fitted over the mouth of the flask. As the mixture boils, vapor rises up the column. The vapor [[Condensation|condenses]] on the glass platforms, known as [[theoretical tray|trays]], inside the column, and runs back down into the liquid below. This is known as "[[reflux]]ing" the distillate.  
  
Alternate set-ups may utilize a "cow" or "pig" which is connected to three or four receiving flasks. By turning the "cow" or "pig", the distillates can be channelled into the appropriate receiver. A [[Perkin triangle]] is versatile piece of apparatus that can be also be used to collect distillation fractions which does not require a cow" or "pig" adaptor. A [[Perkin triangle]] is most often used where the distillates are [[air-sensitive]] or where the fractions distil and are collected under reduced pressure, but can be used for a simple and fractional distillation.
+
Only the most volatile fraction of the vapors remains in [[gas]]eous form all the way to the top of the column. This fraction passes into the condenser, which cools it down until it liquefies, and this liquid is collected in the receiving flask.
 +
 
 +
The efficiency in terms of the amount of heating and time required to get fractionation can be improved by insulating the outside of the column with an insulator such as wool, aluminum foil, or (preferably) a vacuum jacket. The hottest tray is at the bottom and the coolest is at the top. At steady state conditions, the vapor and liquid on each tray are at ''[[vapor-liquid equilibrium|equilibrium]]''. The fractionation is more thorough with the addition of more trays (up to certain practical limitations).
 +
 
 +
In laboratory distillation, any of several types of condensers may be used. The [[Liebig condenser]] is simply a straight tube within a [[water jacket]], and is the simplest (and relatively least expensive) form of condenser. The [[Graham condenser]] is a spiral tube within a water jacket. The [[Allihn condenser]] has a series of large and small constrictions on the inside tube, each increasing the surface area upon which the vapor constituents may condense.
 +
 
 +
In alternate set-ups, a "cow" or "pig" adapter may be used, connected to three or four receiving flasks. By turning the "cow" or "pig," the distillates can be channeled into the appropriate receiver. A [[Perkin triangle]] may also be used to collect distillation fractions, without requiring a "cow" or "pig" adapter. A Perkin triangle is most often used when the distillates are [[air-sensitive]], or when the fractions distill and are collected under reduced pressure, but it can be used for simple as well as fractional distillations.
  
 
[[Vacuum distillation]] systems operate at reduced pressure, thereby lowering the boiling point of the materials.
 
[[Vacuum distillation]] systems operate at reduced pressure, thereby lowering the boiling point of the materials.
 +
 +
=== Example ===
 +
 +
Consider the distillation of a mixture of [[water]] and [[ethanol]]. Ethanol boils at 78.5 °C, and water boils at 100 °C. On that basis, one should be able to separate the two components by fractional distillation. However, a mixture of 96 percent ethanol and four percent water boils at 78.2 °C, being more [[Volatility (chemistry)|volatile]] than pure ethanol. Such a mixture is called an [[azeotrope]]. When the mixture is gently heated, the azeotrope (being the most volatile component) concentrates to a greater degree in the vapor and separates from the rest of the liquid first. Thus, fractional distillation of a mixture of water and ethanol produces 96 percent ethanol.<ref>Given the formation of an azeotrope, ethanol cannot be completely purified by direct fractional distillation of ethanol-water mixtures.</ref> Once all the ethanol has boiled out of the mixture, the [[thermometer]] shows a sharp rise in temperature.
  
 
==Industrial distillation==
 
==Industrial distillation==
[[Image:Colonne distillazione.jpg|right|thumb|250px|Image 2: Typical industrial fractional distillation columns]]
+
[[Image:Colonne distillazione.jpg|right|thumb|250px|Typical industrial fractional distillation columns.]]
Distillation is the most common form of separation technology used in [[oil refinery|petroleum refineries]], [[petrochemical]] and [[chemical plant]]s and [[natural gas processing]] plants.<ref name=Kister>{{cite book|author=Kister, Henry Z.|title= [[Distillation Design]]|edition=1st Edition|publisher=McGraw-Hill|year=1992|id=ISBN 0-07-034909-6}}</ref><ref name=Perry>{{cite book|author=Perry, Robert H. and Green, Don W.|title=[[Perry's Chemical Engineers' Handbook]]|edition=6th Edition|publisher=McGraw-Hill|year=1984|id=ISBN 0-07-049479-7}}</ref> In most cases, the distillation is operated at a [[Continuous distillation|continuous]] [[steady state]]. New feed is always being added to the distillation column and products are always being removed. Unless the process is disturbed due to changes in feed, heat, ambient temperature, or condensing, the amount of feed being added and the amount of product being removed are normally equal. This is known as continuous, steady-state fractional distillation.
 
  
Industrial distillation is typically performed in large, vertical cylindrical columns known as "distillation or fractionation 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. The distillation towers have liquid outlets at intervals up the column which allow for the withdrawal of different ''fractions'' or products having different [[boiling points]] or boiling ranges. The "lightest" products (those with the lowest boiling point) exit from the top of the columns and the "heaviest" products (those with the highest boiling point) exit from the bottom of the column.
+
Fractional distillation is the most common form of separation technology used in [[oil refinery|petroleum refineries]], [[petrochemical]] and [[chemical plant]]s, and [[natural gas processing]] plants.<ref name=Kister>Henry Z. Kister, ''Distillation Design'', 1st ed. (McGraw-Hill, 1992, ISBN 0-07-034909-6).</ref><ref name=Perry>Robert H. Perry and Don W. Green, ''Perry's Chemical Engineers' Handbook'', 6th ed. (McGraw-Hill, 1984, ISBN 0-07-049479-7).</ref> For example, this technique is used in oil refineries to separate [[crude oil]] into useful substances (or fractions) consisting of different [[hydrocarbons]] with differing boiling points. The crude oil fractions with higher boiling points consist of larger molecules (with more [[carbon atom]]s and higher [[molecular weight]]s), are darker in color, are more [[viscosity|viscous]], and are more difficult to ignite and to [[combustion|burn]].
  
For example, fractional distillation is used in [[oil refinery|oil refineries]] to separate [[crude oil]] into useful substances (or fractions) having different [[hydrocarbons]] of different boiling points. The crude oil fractions with higher boiling points:
+
Most often, new feed is continuously added to the distillation column, and products are continuously removed. Unless the process is disturbed due to changes in feed, heat, ambient temperature, or condensing, the amount of feed being added and the amount of product being removed are normally equal. This is known as continuous, steady-state fractional distillation.
  
* have more [[carbon atom]]s
+
Industrial distillation is typically performed in large, vertical cylindrical columns known as "distillation or fractionation towers" or "distillation columns." Their diameters range from about 65 centimeters to six meters, and their heights range from about six meters to 60 meters or more. The distillation towers have liquid outlets at intervals up the column, allowing for the withdrawal of different ''fractions'' or products with different [[boiling points]] or boiling ranges. The "lightest" products (those with the lowest boiling point) exit from the top of the columns and the "heaviest" products (those with the highest boiling point) exit from the bottom of the column.
* have higher [[molecular weight]]s
 
* are darker in color
 
* are more [[viscosity|viscous]]
 
* are more difficult to ignite and to [[combustion|burn]]
 
  
[[Image:Distillation Column.png|frame|right|Figure 1: Diagram of a typical industrial distillation tower]]
+
Fractional distillation is also used for the separation of (liquefied) air into its components, producing liquid [[oxygen]], liquid [[nitrogen]], and high purity [[argon]]. Distillation of [[chlorosilane]]s enables the production of high-purity [[silicon]] for use as a [[semiconductor]].
Large-scale industrial towers use [[reflux]] to achieve a more complete separation of products. Reflux refers to the portion of the condensed overhead liquid product from a distillation or fractionation tower that is returned to the upper part of the tower as shown in the schematic diagram of a typical, large-scale industrial distillation tower. Inside the tower, the reflux liquid flowing downwards provides the cooling needed to condense the vapors flowing upwards, thereby increasing the effectiveness of the distillation tower. The more reflux is provided for a given number of [[theoretical plate]]s, the better the tower's separation of lower boiling materials from higher boiling materials. Alternatively, the more reflux provided for a given desired separation, the fewer theoretical plates are required.
 
  
Fractional distillation is also used in air separation, producing liquid [[oxygen]], [[liquid nitrogen]], and high purity [[argon]]. Distillation of [[chlorosilane]]s also enable the production of high-purity [[silicon]] for use as a [[semiconductor]].
+
[[Image:Distillation Column.png|frame|right|Diagram of a typical, large-scale industrial distillation tower.]]
  
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 (1-3" wide) such as [[Raschig ring]]s or [[structured packing|structured sheet metal]]. Typical manufacturers are Koch, Sulzer and other companies.  Liquids tend to wet the surface of the packing and the vapors pass across this wetted surface, where [[mass transfer]] takes place. Unlike conventional tray distillation in which every tray represents a separate point of [[vapor liquid equilibrium]] the vapor liquid equilibrium curve in a packed column is continuous. However, when modeling packed columns it is useful to compute a number of [[theoretical plate|"theoretical plates"]] to denote the separation efficiency of the packed column with respect to more traditional trays. Differently shaped packings have different surface areas and void space between packings. Both of these factors affect packing performance.
+
Large-scale industrial towers use [[reflux]] to achieve a more complete separation of products. Reflux refers to the portion of the condensed overhead liquid product from a fractionation tower that is returned to the upper part of the tower as shown in the schematic diagram on the right. Inside the tower, the reflux liquid flowing downward provides the cooling needed to condense the vapors flowing upward, thereby increasing the effectiveness of the distillation tower. The more reflux is provided for a given number of [[theoretical plate]]s, the better the tower's ability to separate lower boiling materials from higher boiling materials. Alternatively, the more reflux provided for a given desired separation, the fewer theoretical plates are required.
 +
 
 +
In industrial uses, sometimes a packing material is used instead of trays within the column, especially when operating under reduced pressures. This packing material can either be random dumped packing (one to three inches wide) such as [[Raschig ring]]s or [[structured packing|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. Unlike conventional tray distillation, in which every tray represents a separate point of [[vapor liquid equilibrium]], the vapor liquid equilibrium curve in a packed column is continuous. However, when modeling packed columns, it is useful to compute a number of [[theoretical plate|"theoretical plates"]] to denote the separation efficiency of the packed column with respect to more traditional trays. Differently shaped packings have different surface areas and void space between packings. Both of these factors affect packing performance.
  
 
===Design of industrial distillation columns===
 
===Design of industrial distillation columns===
Design and operation of a distillation column depends on the feed and desired products. Given a simple, binary component feed, analytical methods such as the [[McCabe-Thiele method]]<ref name=Perry/><ref name=Beychok>{{cite journal | last = Beychok | first = Milton | title = Algebraic Solution of McCabe-Thiele Diagram | journal = Chemical Engineering Progress | date = May 1951 }}</ref><ref name=SeaderHenley>{{cite book|author=Seader, J. D., and Henley, Ernest J.|title=Separation Process Principles|publisher=Wiley| location=New York|year=1998|id=ISBN 0-471-58626-9}}</ref> or the [[Fenske equation]]<ref name=Perry/>  can be used. For a multi-component feed, [[simulation]] models are used both for design and operation.
+
[[Image:Tray Distillation Tower.PNG|frame|right|Chemical engineering schematic of typical bubble-cap trays in a distillation tower.]]
[[Image:Tray Distillation Tower.PNG|frame|right|Figure 2: Chemical engineering schematic of typical bubble-cap trays in a distillation tower]]
 
Moreover, the efficiencies of the vapor-liquid contact devices (referred to as ''plates'' or ''trays'') used in distillation columns, as seen in Figure 2,  are typically lower than that of a theoretical 100% efficient [[equilibrium stage]]. Hence, a distillation column needs more plates than the number of theoretical vapor-liquid equilibrium stages.
 
  
An indication of numbers: the separation of two compounds with [[relative volatility]] of 1.1 requires a minimum of 130 theoretical plates with a minimum reflux ratio of 20.<ref>{{cite book| author=Editors: Jacqueline I. Kroschwitz and Arza Seidel|edition=5th Edition|title=Kirk-Othmer Encyclopedia of Chemical Technology|publisher=Wiley-Interscience|location=Hoboken, NJ|year=2004|id=ISBN 0-471-48810-0}}</ref>. With a relative volatility of 4, the required number of theoretical plates decreased to 9 with a reflux ratio of 0.66. In another source, a [[boiling point]] difference of 30°C requires 12 theoretical plates and, for a difference of 3°C, the number of  plates increased to 1000.<ref>{{cite book|author=Arthur I. Vogel and Brian S. Furnis|edition=5th Edition|title=Vogel's Textbook of Practical Organic Chemistry|publisher=Longman Scientific & Technical|location=London|year=1988|id=ISBN 0-582-46236-3}}</ref>
+
Design and operation of a distillation column depends on the feed and desired products. Given a simple, binary component feed, analytical methods such as the [[McCabe-Thiele method]]<ref name=Perry/><ref name=Beychok>{{cite journal | last = Milton | first = Beychok | title = Algebraic Solution of McCabe-Thiele Diagram | journal = Chemical Engineering Progress | date = May 1951 }}</ref><ref name=SeaderHenley> J. D. Seader and Ernest J. Henley, ''Separation Process Principles'' (New York: Wiley, 1998, ISBN 0-471-58626-9). </ref> or the [[Fenske equation]]<ref name=Perry/> can be used. For a multi-component feed, [[simulation]] models are used both for design and operation.  
  
The '''reflux ratio''' is the ratio of the amount of moles returned as refluxed liquid to the fractionating column and the amount of moles of final product, both per unit time.
+
Moreover, the efficiencies of the vapor-liquid contact devices (referred to as ''plates'' or ''trays'') used in distillation columns, as seen in Figure two, are typically lower than that of a theoretical 100 percent efficient [[equilibrium stage]]. Hence, a distillation column needs more plates than the number of theoretical vapor-liquid equilibrium stages.
  
 
==See also==
 
==See also==
*[[Azeotropic distillation]]
+
 
*[[Batch Distillation]]
+
* [[Azeotrope]]
*[[Distillation]]
+
* [[Boiling point]]
*[[Extractive distillation]]
+
* [[Distillation]]
*[[Fractionating column]]
+
* [[Ethanol]]
*[[Freeze distillation]]
+
* [[Mixture]]
*[[Raschig ring]]s
+
* [[Solution]]
*[[Steam distillation]]
+
* [[Solvent]]
*[[Vacuum distillation]]
+
 
 +
== Notes ==
 +
<references/>
 +
 
 +
==References==
 +
 
 +
* Clark, Shove R. ''Elements of Fractional Distillation''. Blatter Press, 2007. ISBN 978-1406700435
 +
* Kister, Henry Z. ''Distillation Design.'' New York: McGraw-Hill, 1992. ISBN 0070349096
 +
* Parkash, Surinder. ''Refining Processes Handbook.'' Amsterdam: Gulf Professional Pub., 2003. ISBN 978-0750677219
 +
* Seader, J. D., and Ernest J. Henley. ''Separation Process Principles.'' New York: Wiley, 1998. ISBN 978-0471586265
 +
* Stichlmair, Johann, and James R. Fair.  ''Distillation: Principles and Practices.'' New York: Wiley, 1998. ISBN 978-0471252412
 +
* Vogel, Arthur Israel, and Brian S. Furniss. ''Vogel's Textbook of Practical Organic Chemistry.'' Harlow: Pearson, 1996 (original 1989). ISBN 0582462363
  
 
==External links==
 
==External links==
*[http://www.cheresources.com/validatingzz.shtml Validating Your Binary VLE Data]
+
All links retrieved April 1, 2024.
*[http://www.acsseparations.com/separation-technologies/structured-tower-packing/default.html ACS Distillation Tower Packing]
 
*[http://www.chemheritage.org/EducationalServices/pharm/antibiot/activity/distil.htm Chemistry Activity: Fractional Distillation]
 
  
==References==
+
* [http://chemistry.about.com/library/glossary/bldef533p.htm Fractional Distillation Definition]
<references/>
+
* [http://www.chemhelper.com/distillation.html Distillation Guide]
  
 
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[[Category:Chemistry]]
 
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Latest revision as of 06:40, 1 April 2024

Fractional distillation is a special type of distillation designed to separate a mixture of two or more liquids that have different boiling points. The process involves heating the mixture and partial condensation of the vapors along a column (fractionating column), which is set up such that components with lower boiling points pass through the column and are collected earlier than components with higher boiling points. Generally, this method is used when the component parts boil at less than 25 °C from each other under a pressure of one atmosphere (atm).[1]

The separation technology of fractional distillation is useful in both research and industrial settings. In industry, it is commonly used in petroleum refineries, chemical plants, and natural gas processing plants. Likewise, if a sample of air is liquefied, it can be separated into its components to produce liquid oxygen, liquid nitrogen, and argon. Also, chlorosilanes can be distilled to produce high-purity silicon for use as a semiconductor.

Fractional distillation in a laboratory

Apparatus

An example of a fractional distillation apparatus used in a laboratory. The diagram shows the use of a Liebig condenser and a conical flask as a receiving flask. Here, the distillation head and fractionating column are combined in one piece.

A laboratory setup for fractional distillation often involves use of the following pieces of apparatus, put together as shown in the image on the right:

  • a heat source (such as a hot plate with a bath)
  • a distilling flask (typically a round-bottom flask)
  • a receiving flask (often a round-bottom flask or conical flask)
  • a fractionating column (Vigreux column)
  • a distillation head
  • a thermometer and adapter if needed
  • a condenser (Liebig condenser, Graham condenser, or Allihn condenser)
  • a vacuum adapter (for distillations under reduced pressure)
  • boiling chips (also known as anti-bumping granules)
  • rubber bungs, unless laboratory glassware with ground glass joints is used, such as a quickfit apparatus.

Procedure

The apparatus is assembled as in the diagram (which represents a batch apparatus, as opposed to a continuous apparatus). The mixture is put into a round-bottom flask along with a few anti-bumping granules, and the fractionating column is fitted over the mouth of the flask. As the mixture boils, vapor rises up the column. The vapor condenses on the glass platforms, known as trays, inside the column, and runs back down into the liquid below. This is known as "refluxing" the distillate.

Only the most volatile fraction of the vapors remains in gaseous form all the way to the top of the column. This fraction passes into the condenser, which cools it down until it liquefies, and this liquid is collected in the receiving flask.

The efficiency in terms of the amount of heating and time required to get fractionation can be improved by insulating the outside of the column with an insulator such as wool, aluminum foil, or (preferably) a vacuum jacket. The hottest tray is at the bottom and the coolest is at the top. At steady state conditions, the vapor and liquid on each tray are at equilibrium. The fractionation is more thorough with the addition of more trays (up to certain practical limitations).

In laboratory distillation, any of several types of condensers may be used. The Liebig condenser is simply a straight tube within a water jacket, and is the simplest (and relatively least expensive) form of condenser. The Graham condenser is a spiral tube within a water jacket. The Allihn condenser has a series of large and small constrictions on the inside tube, each increasing the surface area upon which the vapor constituents may condense.

In alternate set-ups, a "cow" or "pig" adapter may be used, connected to three or four receiving flasks. By turning the "cow" or "pig," the distillates can be channeled into the appropriate receiver. A Perkin triangle may also be used to collect distillation fractions, without requiring a "cow" or "pig" adapter. A Perkin triangle is most often used when the distillates are air-sensitive, or when the fractions distill and are collected under reduced pressure, but it can be used for simple as well as fractional distillations.

Vacuum distillation systems operate at reduced pressure, thereby lowering the boiling point of the materials.

Example

Consider the distillation of a mixture of water and ethanol. Ethanol boils at 78.5 °C, and water boils at 100 °C. On that basis, one should be able to separate the two components by fractional distillation. However, a mixture of 96 percent ethanol and four percent water boils at 78.2 °C, being more volatile than pure ethanol. Such a mixture is called an azeotrope. When the mixture is gently heated, the azeotrope (being the most volatile component) concentrates to a greater degree in the vapor and separates from the rest of the liquid first. Thus, fractional distillation of a mixture of water and ethanol produces 96 percent ethanol.[2] Once all the ethanol has boiled out of the mixture, the thermometer shows a sharp rise in temperature.

Industrial distillation

Typical industrial fractional distillation columns.

Fractional distillation is the most common form of separation technology used in petroleum refineries, petrochemical and chemical plants, and natural gas processing plants.[3][4] For example, this technique is used in oil refineries to separate crude oil into useful substances (or fractions) consisting of different hydrocarbons with differing boiling points. The crude oil fractions with higher boiling points consist of larger molecules (with more carbon atoms and higher molecular weights), are darker in color, are more viscous, and are more difficult to ignite and to burn.

Most often, new feed is continuously added to the distillation column, and products are continuously removed. Unless the process is disturbed due to changes in feed, heat, ambient temperature, or condensing, the amount of feed being added and the amount of product being removed are normally equal. This is known as continuous, steady-state fractional distillation.

Industrial distillation is typically performed in large, vertical cylindrical columns known as "distillation or fractionation towers" or "distillation columns." Their diameters range from about 65 centimeters to six meters, and their heights range from about six meters to 60 meters or more. The distillation towers have liquid outlets at intervals up the column, allowing for the withdrawal of different fractions or products with different boiling points or boiling ranges. The "lightest" products (those with the lowest boiling point) exit from the top of the columns and the "heaviest" products (those with the highest boiling point) exit from the bottom of the column.

Fractional distillation is also used for the separation of (liquefied) air into its components, producing liquid oxygen, liquid nitrogen, and high purity argon. Distillation of chlorosilanes enables the production of high-purity silicon for use as a semiconductor.

Diagram of a typical, large-scale industrial distillation tower.

Large-scale industrial towers use reflux to achieve a more complete separation of products. Reflux refers to the portion of the condensed overhead liquid product from a fractionation tower that is returned to the upper part of the tower as shown in the schematic diagram on the right. Inside the tower, the reflux liquid flowing downward provides the cooling needed to condense the vapors flowing upward, thereby increasing the effectiveness of the distillation tower. The more reflux is provided for a given number of theoretical plates, the better the tower's ability to separate lower boiling materials from higher boiling materials. Alternatively, the more reflux provided for a given desired separation, the fewer theoretical plates are required.

In industrial uses, sometimes a packing material is used instead of trays within the column, especially when operating under reduced pressures. This packing material can either be random dumped packing (one to three inches 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. Unlike conventional tray distillation, in which every tray represents a separate point of vapor liquid equilibrium, the vapor liquid equilibrium curve in a packed column is continuous. However, when modeling packed columns, it is useful to compute a number of "theoretical plates" to denote the separation efficiency of the packed column with respect to more traditional trays. Differently shaped packings have different surface areas and void space between packings. Both of these factors affect packing performance.

Design of industrial distillation columns

Chemical engineering schematic of typical bubble-cap trays in a distillation tower.

Design and operation of a distillation column depends on the feed and desired products. Given a simple, binary component feed, analytical methods such as the McCabe-Thiele method[4][5][6] or the Fenske equation[4] can be used. For a multi-component feed, simulation models are used both for design and operation.

Moreover, the efficiencies of the vapor-liquid contact devices (referred to as plates or trays) used in distillation columns, as seen in Figure two, are typically lower than that of a theoretical 100 percent efficient equilibrium stage. Hence, a distillation column needs more plates than the number of theoretical vapor-liquid equilibrium stages.

See also

Notes

  1. If the difference in boiling points is greater than 25 °C, a simple distillation method is used.
  2. Given the formation of an azeotrope, ethanol cannot be completely purified by direct fractional distillation of ethanol-water mixtures.
  3. Henry Z. Kister, Distillation Design, 1st ed. (McGraw-Hill, 1992, ISBN 0-07-034909-6).
  4. 4.0 4.1 4.2 Robert H. Perry and Don W. Green, Perry's Chemical Engineers' Handbook, 6th ed. (McGraw-Hill, 1984, ISBN 0-07-049479-7).
  5. Milton, Beychok (May 1951). Algebraic Solution of McCabe-Thiele Diagram. Chemical Engineering Progress.
  6. J. D. Seader and Ernest J. Henley, Separation Process Principles (New York: Wiley, 1998, ISBN 0-471-58626-9).

References
ISBN links support NWE through referral fees

  • Clark, Shove R. Elements of Fractional Distillation. Blatter Press, 2007. ISBN 978-1406700435
  • Kister, Henry Z. Distillation Design. New York: McGraw-Hill, 1992. ISBN 0070349096
  • Parkash, Surinder. Refining Processes Handbook. Amsterdam: Gulf Professional Pub., 2003. ISBN 978-0750677219
  • Seader, J. D., and Ernest J. Henley. Separation Process Principles. New York: Wiley, 1998. ISBN 978-0471586265
  • Stichlmair, Johann, and James R. Fair. Distillation: Principles and Practices. New York: Wiley, 1998. ISBN 978-0471252412
  • Vogel, Arthur Israel, and Brian S. Furniss. Vogel's Textbook of Practical Organic Chemistry. Harlow: Pearson, 1996 (original 1989). ISBN 0582462363

External links

All links retrieved April 1, 2024.

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