Vacuum distillation

Vacuum distillation is a method of distillation performed under reduced pressure.

As with distillation, this technique separates compounds based on differences in
boiling points. This technique is used when the boiling point of the desired
compound is difficult to achieve or will cause the compound to decompose. A
reduced pressure decreases the boiling point of compounds. The reduction in boiling
point can be calculated using a temperature-pressure nomograph using the Clausius–
Clapeyron_relation [1].

Contents
Laboratory-scale applications
Distillation of high-boiling and/or air sensitive materials
Perkin triangle distillation set-up
Vacuum distillation set-up using a short-pathhead
Rotary evaporation Figure 1: At atmospheric pressure,
Safety considerations dimethyl sulfoxide boils at 189 °C. In
Industrial-scale applications the vacuum apparatus here, it distills
Vacuum distillation in petroleum refining off into the connected receiver flask
on the left at only 70 °C.
Molecular distillation
Gallery
See also
References
External links

Laboratory-scale applications
In the laboratory vacuum distillation is used to purify compounds or remove solvent.

Distillation of high-boiling and/or air sensitive materials

Distillation is used to separate compounds based on differences in boiling point. Vacuum distillation allows for this purification
technique to be used on compounds with high boiling points, or those which are air-sensitive. Compounds with a boiling point lower
than 150oC can typically be distilled without reduced pressure. Using a fractionating column in the set-up improves the separation of
mixtures, and can allow separation of compounds with similar boiling points. With the apparatus under reduced pressure, exposure to
[2] .
the atmosphere is minimized and the apparatus can be filled with the inert atmosphere when the distillation is complete

For better results or for very air sensitive compounds, either a Perkin triangle distillation set-up or a short-path distillation set-up can
be used.

Perkin triangle distillation set-up

The Perkin triangle set-up (Image 5) uses a series of Teflon valves to allow the distilled fractions to be isolated from the distillation
flask without the main body of the distillation set-up being removed from either the vacuum or the heat source, and thus can remain
in a state of reflux.
To do this, the distillate receiver vessel is first isolated from the vacuum by means of theeflon
T valves.

The vacuum over the sample is then replaced with an inert gas (such as nitrogen or argon) and the distillate receiver can then be
stoppered and removed from the system.

Vacuum distillation set-up using a short-path head

Vacuum distillation of moderately air/water-sensitive liquid can be done using standard Schlenk-line techniques (Image 6). When
assembling the set-up apparatus, all of the connecting lines are clamped so that they cannot pop f.of

Once the apparatus is assembled, and the liquid to be distilled is in the still pot, the desired vacuum is established in the system by
using the vacuum connection on the short-path distillation head. Care is taken to prevent potential "bumping" as the liquid in the still
pot degases.

While establishing the vacuum, the flow of coolant is started through the short-path distillation head. Once the desired vacuum is
established, heat is applied to the still pot.

If needed, the first portion of distillate can be discarded by pur

ging with inert gas and changing out the distillate receiver
.

When the distillation is complete: the heat is removed, the vacuum connection is closed, and inert gas is purged through the
distillation head and the distillate receiver. While under the inert gas purge, remove the distillate receiver and cap it with an air-tight
cap. The distillate receiver can be stored under vacuum or under inert gas by using the side-arm on the distillation flask.

Rotary evaporation
Rotary evaporation[3] is a common technique used in laboratories to concentrate or isolate a compound from solution. Many solvents
are volatile and can easily be evaporated using rotary evaporation. Even less volatile solvents can be removed by rotary evaporation
under high vacuum and with heating. It is also used by environmental regulatory agencies for determining the number of solvents in
paints, coatings and inks.[4]

Safety considerations
Safety is an important consideration when using glassware as part of the set-up. All of the glass components should be carefully
examined for scratches and cracks which could result in implosions when the vacuum is applied. Wrapping as much of the glassware
with tape as is practical helps to prevent dangerous scattering of glass shards in the event of an implosion.

Industrial-scale applications
Industrial-scale vacuum distillation[6] has several advantages. Close boiling mixtures may require many equilibrium stages to
separate the key components. One tool to reduce the number of stages needed is to utilize vacuum distillation.[7] Vacuum distillation
columns (as depicted in Figures 2 and 3) typically used in oil refineries have diameters ranging up to about 14 meters (46 feet),
heights ranging up to about 50 meters (164 feet), and feed rates ranging up to about 25,400 cubic meters per day (160,000 barrels per
day).

Vacuum distillation increases therelative volatility of the key components in many applications. The higher the relative volatility, the
more separable are the two components; this connotes fewer stages in a distillation column in order to effect the same separation
between the overhead and bottoms products. Lower pressures increase relative volatilities in most systems.

The second advantage of vacuum distillation is the reduced temperature requirement at lower pressures. For many systems, the
products degrade or polymerize at elevated temperatures.

Vacuum distillation can improve a separation by:

 Prevention of product degradation or
polymer formation because of reduced
pressure leading to lower tower bottoms
temperatures,
Reduction of product degradation or
polymer formation because of reduced
mean residence time especially in
columns using packing rather than trays.
Increasing capacity, yield, and purity.
Another advantage of vacuum distillation is the
reduced capital cost, at the expense of slightly
more operating cost. Utilizing vacuum distillation
can reduce the height and diameter, and thus the
capital cost of a distillation column.

Vacuum distillation in petroleum

refining Figure 2: Simplified animation of a typical dry vacuum distillation
column as used in oil refineries
Petroleum crude oil is a complex mixture of
hundreds of different hydrocarbon compounds
generally having from 3 to 60 carbon atoms per molecule, although there may be small
amounts of hydrocarbons outside that range.[8][9][10] The refining of crude oil begins with
distilling the incoming crude oil in a so-called atmospheric distillation column operating at
pressures slightly above atmospheric pressure.[6][8][9]

Vacuum distillation can also be referred to as "low-temperature distillation"

In distilling the crude oil, it is important not to subject the crude oil to temperatures above
370 to 380 °C because of the high molecular weight components in the crude oil will
undergo thermal cracking and form petroleum coke at temperatures above that. Formation
of coke would result in plugging the tubes in the furnace that heats the feed stream to the
crude oil distillation column. Plugging would also occur in the piping from the furnace to
the distillation column as well as in the column itself.

The constraint imposed by limiting the column inlet crude oil to a temperature of less than
370 to 380 °C yields a residual oil from the bottom of the atmospheric distillation column
consisting entirely of hydrocarbons that boil above 370 to 380 °C.
Figure 3: Large-scale vacuum
To further distill the residual oil from the atmospheric distillation column, the distillation
distillation tower at theFawley
must be performed at absolute pressures as low as 10 to 40 mmHg (also referred to as Torr) oil refinery[5]
so as to limit the operating temperature to less than 370 to 380 °C.

Figure 2 is a simplified process diagram of a petroleum refinery vacuum distillation column that depicts the internals of the column
and Figure 3 is a photograph of a large vacuum distillation column in a petroleum refinery.

The 10 to 40 mmHg absolute pressure in a vacuum distillation column increases the volume of vapor formed per volume of liquid
ge diameters.[11]
distilled. The result is that such columns have very lar

Distillation columns such those in Images 1 and 2, may have diameters of 15 meters or more, heights ranging up to about 50 meters,
and feed rates ranging up to about 25,400 cubic meters per day (160,000 barrels per day).

The vacuum distillation column internals must provide good vapor-liquid contacting while, at the same time, maintaining a very low-
pressure increase from the top of the column top to the bottom. Therefore, the vacuum column uses distillation trays only where
withdrawing products from the side of the column (referred to as side draws). Most of the column uses packing material for the
vapor-liquid contacting because such packing has a lower pressure drop than distillation trays. This packing material can be either
structured sheet metal or randomly dumped packing such asRaschig rings.

The absolute pressure of 10 to 40 mmHg in the vacuum column is most often achieved by using multiple stages of steam jet
ejectors.[12]

Many industries, other than the petroleum refining industry, use vacuum distillation on a much a smaller scale. Copenhagen-based
Empirical Spirits,[13] a distillery founded by former Noma chefs,[14] uses the process to create uniquely flavoured spirits. Their
Y [15] .
flagship spirit, Helena, is created using Koji, alongside Pilsner Malt and Belgian Saisoneast

Molecular distillation
Molecular distillation is vacuum distillation below the pressure of 0.01 torr[16] (1.3 Pa). 0.01 torr is one order of magnitude above
high vacuum, where fluids are in the free molecular flow regime, i.e. the mean free path of molecules is comparable to the size of the
equipment. The gaseous phase no longer exerts significant pressure on the substance to be evaporated, and consequently, the rate of
evaporation no longer depends on pressure. That is, because the continuum assumptions of fluid dynamics no longer apply, mass
transport is governed by molecular dynamics rather than fluid dynamics. Thus, a short path between the hot surface and the cold
surface is necessary, typically by suspending a hot plate covered with a film of feed next to a cold plate with a line of sight in
between. Molecular distillation is used industrially for purification of oils.

Gallery

A simple short path Kugelrohr – a short path Perkin triangle – for air- Vacuum distillation
vacuum distillation vacuum distillation sensitive vacuum apparatus
apparatus apparatus distillation

See also
Continuous distillation
Fractionating column
Fractional distillation
Kugelrohr

References
This article incorporates material from the Citizendium article "Vacuum distillation", which is
licensed under the Creative Commons Attribution-ShareAlike 3.0 Unported License but not
under the GFDL.

1. "Pressure-Temperature Nomograph Interactive Tool" (https://www.sigmaaldrich.com/chemistry/solvents/learning-cent

er/nomograph.html). Sigma-Aldrich. Retrieved 2018-03-23.
 2. Leonard, J.; Lygo, B.; Procter, Garry. Advanced practical organic chemistry(3rd ed.). Boca Raton.
ISBN 9781439860977. OCLC 883131986 (https://www.worldcat.org/oclc/883131986).
3. Operation of a Rotary Evaporator (Rotovap)(http://www.chem.ubc.ca/courseware/235/danalabsess/rotovap.html)
(from the website of theUniversity of British Columbia)
4. [1] (http://aqmd.gov/tao/methods/lab/303-91.pdf)
SCAQMD Test method 302-91
5. Energy Institute website page(http://resources.schoolscience.co.uk/SPE/knowl/4/2index.htm?vacuum.html)
6. Kister, Henry Z. (1992). Distillation Design (1st ed.). McGraw-Hill.ISBN 0-07-034909-6.
7. Karl Kolmetz, Andrew W. Sloley et al. (2004), Designing Distillation Columns for Vacuum Service, 11th India Oil and
Gas Symposium and International Exhibition, September 2004,Mumbai, India (also published inHydrocarbon
Processing, May 2005)
8. Gary, J.H. & Handwerk, G.E. (1984).Petroleum Refining Technology and Economics (2nd ed.). Marcel Dekker, Inc.
ISBN 0-8247-7150-8.
9. Leffler, W.L. (1985). Petroleum refining for the nontechnical person(2nd ed.). PennWell Books. ISBN 0-87814-280-0.
10. James G, Speight (2006).The Chemistry and Technology of Petroleum(4th ed.). CRC Press. 0-8493-9067-2.
11. Karl Kolmetz, Andrew W. Sloley et al (2004), Designing Distillation Columns for Vacuum Service, 11th India Oil and
Gas Symposium and International Exhibition, September 2004,Mumbai, India (also published inHydrocarbon
Processing, May 2005)
12. Photo gallery (http://www.graham-mfg.com/ejphotos.html)Archived (https://web.archive.org/web/20090207173354/ht
tp://graham-mfg.com/ejphotos.html)2009-02-07 at the Wayback Machine. (from website of Graham Manufacturing
Company)
13. "Empirical Spirits" (https://empiricalspirits.co/). empiricalspirits.co. Retrieved 2018-10-15.
14. Kahn, Howie (2018-04-25)."A Fresh Take on Liquor From Two Noma Alums" (https://www.wsj.com/articles/a-fresh-t
ake-on-liquor-from-two-noma-alums-1524666332) . Wall Street Journal. ISSN 0099-9660 (https://www.worldcat.org/is
sn/0099-9660). Retrieved 2018-10-15.
15. "Empirical Spirits" (https://shop.empiricalspirits.co/). Empirical Spirits. Retrieved 2018-10-15.
16. Vogel's 5th ed.

External links
D1160 Vacuum Distillation
How vacuum distillation works
Pressure-temperature nomograph
Short path distillation, includes a table comparing methods

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