Reflux

1
Reflux
This article is about using reflux in chemical engineering and chemistry. For other usage, see Reflux
(disambiguation).
The reflux system in a typical industrial distillation column
Reflux is a distillation 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. It is also used in chemistry to supply energy to
reactions 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 and fractionators such as
petroleum refineries, petrochemical and chemical plants, and
natural gas 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 of the upflowing vapors thereby
increasing the efficiency of the distillation column.
The more reflux provided for a given number of theoretical
plates, 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.
Reflux
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Reflux to regulate energy in chemical reactions
Laboratory reflux apparatus for adding energy to a
chemical reaction
A liquid reaction mixture is placed in a vessel open only at the top.
This vessel is connected to a Liebig or Vigreux 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's boiling point).
[1]
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 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 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 or mantle) is preferred.
Furthermore, a high boiling, thermally stable silicone oil 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. If
even higher temperatures are required, the oil bath can be replaced with a sand bath.
Reflux
3
Reflux in laboratory distillation
Laboratory apparatus using reflux to supply energy to
chemical reactions. An Erlenmeyer flask is used as a receiving
flask. Here the distillation head and fractionating column are
combined in one piece.
The apparatus shown in the diagram represents a batch
distillation as opposed to a continuous distillation. The liquid
feed mixture to be distilled is placed into the round-bottomed
flask along with a few anti-bumping granules, and the
fractionating column is fitted into the top. As the mixture is
heated and boils, vapor rises up the column. The vapor
condenses 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. Only the most volatile of the
vapors stays in gaseous form all the way to the top. The
vapor at the top of the column then passes into the
condenser, 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, the feed mixture enters in the middle
of the column.
Reflux in beverage distillation
By controlling the temperature of the condenser, often called a dephlegmator, a reflux still may be used to ensure that
higher boiling point components are returned to the flask while lighter elements are passed out to a secondary
condenser. This is useful in producing high quality alcoholic beverages, while ensuring that less desirable
components (such as fusel alcohols) are returned to the primary flask. For high quality neutral spirits (such as
vodka), or post distillation flavored spirits (gin, absinthe) , 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. The
geometry of the still also plays a role in determining how much reflux occurs. In a pot still, if the tube leading from
the boiler to the condenser, the lyne arm, is angled upward, more liquid will have a chance to condense and flow
back into the boiler leading to increased reflux. Typical results can increase production as high as 50% over the basic
worm type condenser. The addition of a copper "boiling ball" in the path creates an area where expansion of gasses
into the ball causes cooling and subsequent condensation and reflux. In a column still, the addition of inert materials
in the column (e.g., packing) creates surfaces for early condensation and leads to increased reflux.
Reflux
4
References
[1] Chemistry Online Reflux: What is reflux? (http:/ / webapps. utsc. utoronto. ca/ chemistryonline/ reflux. php) From the website of the
University of Toronto Scarborough.
External links
Distillation column components (http:/ / lorien. ncl. ac. uk/ ming/ distil/ distileqp. htm), Dr. Ming Tham,
Newcastle University, United Kingdom.
Gallery
Toluene is refluxed with
sodiumbenzophenone desiccant before it is
distilled to give pure oxygen- and water-free
toluene.
Industrial fractionating columns all of which
use reflux
Organic
synthesis
apparatus
using reflux
Article Sources and Contributors
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