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Reflux



 
 
Reflux is a technique involving the condensation
Condensation

Condensation is the change of the physical state of aggregation of matter from gaseous phase into liquid phase. When the transition happens from the gaseous phase into the solid phase directly, bypassing the liquid phase the change is called Deposition , which is the opposite of sublimation....
 of vapors and the return of this condensate to the system from which it originated. It is used in industrial and laboratory distillation
Distillation

Distillation is a method of separation process mixtures based on differences in their Volatility in a boiling liquid mixture. Distillation is a unit operation, or a physical separation process, and not a chemical reaction....
s. It is also used in chemistry
Chemistry

Chemistry is the science concerned with the composition, structure, and properties of matter, as well as the changes it undergoes during chemical reactions....
 to supply energy
Energy

In physics, energy is a scalar physical quantity that describes the amount of Work_ that can be performed by a force. Energy is an attribute of objects and systems that is subject to a conservation law....
 to reaction
Reaction

Reaction may refer to:*Response to another event*Adverse drug reaction*Chemical reaction*Light reaction*Nuclear reaction*Reaction , as defined by Newton's third law...
s over a long period of time.

Reflux in industrial distillation
The term reflux is very widely used in industries that utilize large-scale distillation columns
Fractionating column

A fractionating column or fractionation 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 Volatility ....
 and fractionators
Fractional distillation

Fractional distillation is the separation of a mixture into its component parts, or fractions, such as in separating chemical compound by their boiling point by heating them to a temperature at which several fractions of the compound will evaporate....
 such as petroleum refineries
Oil refinery

An oil refinery is an industrial process plant where crude oil is processed and refined into more useful petroleum products, such as gasoline, diesel fuel, asphalt, heating oil, kerosene, and liquefied petroleum gas....
, petrochemical
Petrochemical

Petrochemicals are chemical products made from raw materials of petroleum or other hydrocarbon origin. Although some of the chemical compounds that originate from petroleum may also be derived from coal and natural gas, petroleum is the major source....
 and chemical plant
Chemical plant

A chemical plant is an industry Industrial process factory that manufactures chemicals, usually on a large scale. The general objective of a chemical plant is to create new material wealth via the chemical or biological transformation and or separation of materials....
s, and natural gas
Natural gas

Natural gas is a gas consisting primarily of methane. It is found associated with fossil fuels, in coal beds, as methane clathrates, and is created by methanogenic organisms in marshes, bogs, and landfills....
 processing plants.

In that context, reflux refers to the portion of the overhead liquid product from a distillation column or fractionator that is returned to the upper part of the column as shown in the schematic diagram of a typical industrial distillation column.






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Encyclopedia


Reflux is a technique involving the condensation
Condensation

Condensation is the change of the physical state of aggregation of matter from gaseous phase into liquid phase. When the transition happens from the gaseous phase into the solid phase directly, bypassing the liquid phase the change is called Deposition , which is the opposite of sublimation....
 of vapors and the return of this condensate to the system from which it originated. It is used in industrial and laboratory distillation
Distillation

Distillation is a method of separation process mixtures based on differences in their Volatility in a boiling liquid mixture. Distillation is a unit operation, or a physical separation process, and not a chemical reaction....
s. It is also used in chemistry
Chemistry

Chemistry is the science concerned with the composition, structure, and properties of matter, as well as the changes it undergoes during chemical reactions....
 to supply energy
Energy

In physics, energy is a scalar physical quantity that describes the amount of Work_ that can be performed by a force. Energy is an attribute of objects and systems that is subject to a conservation law....
 to reaction
Reaction

Reaction may refer to:*Response to another event*Adverse drug reaction*Chemical reaction*Light reaction*Nuclear reaction*Reaction , as defined by Newton's third law...
s over a long period of time.

Reflux in industrial distillation


The term reflux is very widely used in industries that utilize large-scale distillation columns
Fractionating column

A fractionating column or fractionation 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 Volatility ....
 and fractionators
Fractional distillation

Fractional distillation is the separation of a mixture into its component parts, or fractions, such as in separating chemical compound by their boiling point by heating them to a temperature at which several fractions of the compound will evaporate....
 such as petroleum refineries
Oil refinery

An oil refinery is an industrial process plant where crude oil is processed and refined into more useful petroleum products, such as gasoline, diesel fuel, asphalt, heating oil, kerosene, and liquefied petroleum gas....
, petrochemical
Petrochemical

Petrochemicals are chemical products made from raw materials of petroleum or other hydrocarbon origin. Although some of the chemical compounds that originate from petroleum may also be derived from coal and natural gas, petroleum is the major source....
 and chemical plant
Chemical plant

A chemical plant is an industry Industrial process factory that manufactures chemicals, usually on a large scale. The general objective of a chemical plant is to create new material wealth via the chemical or biological transformation and or separation of materials....
s, and natural gas
Natural gas

Natural gas is a gas consisting primarily of methane. It is found associated with fossil fuels, in coal beds, as methane clathrates, and is created by methanogenic organisms in marshes, bogs, and landfills....
 processing plants.

In that context, reflux refers to the portion of the overhead liquid product from a distillation column or fractionator that is returned to the upper part of the column as shown in the schematic diagram of a typical industrial distillation column. Inside the column, the downflowing reflux liquid provides cooling and condensation
Condensation

Condensation is the change of the physical state of aggregation of matter from gaseous phase into liquid phase. When the transition happens from the gaseous phase into the solid phase directly, bypassing the liquid phase the change is called Deposition , which is the opposite of sublimation....
 of the upflowing vapors thereby increasing the efficacy of the distillation column.

The more reflux provided for a given number of theoretical plate
Theoretical plate

A theoretical plate in many separation processes is a hypothetical zone or stage in which two phases, such as the liquid and vapor phases of a substance, establish an Vapor-liquid equilibrium with each other....
s, the better is the column's separation of lower boiling materials from higher boiling materials. Conversely, for a given desired separation, the more reflux is provided, the fewer theoretical plates are required.

eflux in laboratory distillation



The apparatus shown in the diagram represents a batch distillation as opposed to a continuous distillation
Continuous distillation

Continuous distillation, a form of distillation, is an ongoing separation in which a mixture is continuously fed into the process and separated fractions are removed continuously as output streams as time passes during the operation....
. The liquid feed mixture to be distilled is placed into the round-bottomed flask along with a few anti-bumping granules
Boiling chip

Boiling chips, also known as boiling stones, boileezers or anti-bumping granules, are small, irregularly shaped stones added to liquids to make them boiling more smoothly mainly in distillation....
, and the fractionating column
Fractionating column

A fractionating column or fractionation 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 Volatility ....
 is fitted into the top. As the mixture is heated and boils, vapor rises up the column. The vapor condenses
Condensation

Condensation is the change of the physical state of aggregation of matter from gaseous phase into liquid phase. When the transition happens from the gaseous phase into the solid phase directly, bypassing the liquid phase the change is called Deposition , which is the opposite of sublimation....
 on the glass platforms (known as plates or trays) inside the column and runs back down into the liquid below, thereby refluxing 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
Vapor-liquid equilibrium

Vapor-liquid equilibrium, abbreviated as VLE by some, is a condition where a liquid and its vapor are in Chemical equilibrium with each other, a condition or state where the rate of evaporation equals the rate of condensation on a molecular level such that there is no net vapor-liquid interconversion....
. Only the most volatile of the vapors stays in gas
Gas

In physics, a gas is a state of matter, consisting of a collection of particles without a definite shape or volume that are in more or less random motion....
eous form all the way to the top. The vapor at the top of the column then passes into the condenser
Condenser (heat transfer)

In systems involving heat transfer, a condenser is a device or unit used to Condensation a substance from its gaseous to its liquid state, typically by cooling it....
, where it cools until it condenses into a liquid. The separation can be enhanced with the addition of more trays (to a practical limitation of heat, flow, etc.). The process continues until all the most volatile components in the liquid feed boil out of the mixture. This point can be recognized by the rise in temperature shown on the thermometer. For continuous distillation
Continuous distillation

Continuous distillation, a form of distillation, is an ongoing separation in which a mixture is continuously fed into the process and separated fractions are removed continuously as output streams as time passes during the operation....
, the feed mixture enters in the middle of the column.

eflux to apply energy to chemical reactions


A liquid reaction mixture is placed in a vessel open only at the top. This vessel is connected to a Liebig condenser, such that any vapours given off are cooled back to liquid, and fall back into the reaction vessel. The vessel is then heated vigorously for the course of the reaction. The purpose is to thermally accelerate the reaction by conducting it at an elevated temperature (i.e. the solvent
Solvent

A solvent is a liquid or gas that dissolves a solid, liquid, or gaseous solute, resulting in a solution.The most common solvent in everyday life is water....
's boiling point
Boiling point

The boiling point of a liquid is the temperature at which the vapor pressure of the liquid equals the environmental pressure surrounding the liquid....
.)

The advantage of this technique is that it can be left for a long period of time without the need to add more solvent or fear of the reaction vessel boiling dry as any vapour is immediately condensed in the condenser. In addition, as a given solvent
Solution

In chemistry, a solution is a homogeneous mixture composed of two or more substances. In such a mixture, a solute is dissolved in another substance, known as a solvent....
 will always boil at a certain temperature, one can be sure that the reaction will proceed at a constant temperature. By careful choice of solvent, one can control the temperature within a very narrow range. The constant boiling action also serves to continuously mix the solution, although a magnetic stirring rod mechanism is often used to achieve a uniform solution. This technique is useful for performing chemical reactions under controlled conditions that require substantial time for completion.

The diagram shows a typical reflux apparatus for applying energy to chemical reactions. It includes an optional beaker of water between the reactants and the heat. This is often used as a safety precaution when using flammable reactants and a Bunsen burner
Bunsen burner

A Bunsen burner is a common piece of laboratory equipment that produces a single open gas flame, which is used for heating, sterilization, and combustion....
 in order to keep the flame away from the reactants. In modern laboratories, open flames are avoided due to the many flammable solvents often in use, and electrical heating, (i.e., with a hot plate
Hot plate

A hot plate is a small electric stove often used in food preparation, generally for small dishes in places where a full kitchen stove would not be convenient....
 or mantle) is preferred. Furthermore, a high boiling, thermally stable silicone oil
Silicone oil

Silicone oils are silicon analogues of carbon based organic compounds, and can form long and complex molecules based on silicon rather than carbon....
 is generally used to immerse the reaction vessel, rather than water which evaporates too readily to be useful for lengthy reactions. Using an oil bath, temperatures of up to several hundred degrees can easily be achieved, which is higher than the boiling point of most commonly used solvents
Solvent

A solvent is a liquid or gas that dissolves a solid, liquid, or gaseous solute, resulting in a solution.The most common solvent in everyday life is water....
. If even higher temperatures are required, the oil bath can be replaced with a sand bath
Sand bath

A sand bath is a common piece of laboratory equipment made from a container filled with heated sand. It is used to provide even heating for another container, most often during a chemical reaction....
.

Reflux in beverage distillation


By controlling the temperature of the condenser, a reflux still may be used to ensure that higher boiling point components (which are also of higher molecular weight) are returned to the flask while lighter elements are passed out to a secondary condenser. This is useful in producing high quality alcoholic
Alcohol

In chemistry, an alcohol is any organic compound in which a hydroxyl Functional group is bound to a carbon atom of an alkyl or substituted alkyl group....
 beverages, while ensuring that less desirable components (such as fusel alcohol
Fusel alcohol

Fusel alcohols, also sometimes called fusel oils, or potato oil in Europe, are higher order alcohols formed by Fermentation and present in cider, mead, beer, wine, and Distilled beverage to varying degrees....
s) are returned to the primary flask. This is particularly effective in the production of alcoholic beverages in which it is appropriate to retain the flavors and aromas of the source fruit - such as applejack
Applejack (beverage)

Applejack is a strong alcoholic beverage produced from apples, originating from the American colonies period. It is made by concentrating hard cider, either by the traditional method of fractional freezing or by true evaporative distillation....
. For high quality neutral spirits (such as vodka
Vodka

Vodka is a distilled beverage. It is a clear liquid which consists of mostly water and ethanol purified by distillation ? often multiple distillation ? from a Fermentation substance, such as cereal , potatoes or sugar beet molasses, and an insignificant amount of other substances such as flavorings or unintended impurities....
), or post distillation flavored spirits, a process of multiple distillations or charcoal filtering may be applied to obtain a product lacking in any suggestion of its original source material for fermentation
Fermentation (food)

Fermentation in food processing typically refers to the conversion of sugar to alcohol using yeast under anaerobic conditions. A more general definition of fermentation is the chemical conversion of carbohydrates into alcohols or acids....
.

See also

  • Batch distillation
    Batch distillation

    Batch distillation refers to the use of distillation in batches, meaning that a mixture is distilled to separate it into its component fractions before the distillation still is again charged with more mixture and the process is repeated....
  • Fractional distillation
    Fractional distillation

    Fractional distillation is the separation of a mixture into its component parts, or fractions, such as in separating chemical compound by their boiling point by heating them to a temperature at which several fractions of the compound will evaporate....
  • Fractionating column
    Fractionating column

    A fractionating column or fractionation 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 Volatility ....


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