Distillation - a process in which a liquid or vapour mixture of two or more substances is separated into its component fractions of desired

purity, by the application and removal of heat.

For any liquid, the individual molecules within the liquid are continuously in motion A small percentage of these molecules attain enough kinetic energy
to leave the liquid phase This exerts an opposing pressure on the atmosphere above the solution known as the vapor pressure, P Atmospheric
pressure, P atm Vapor Pressure, P ==P = P atm P < P atm When enough energy, in the form of heat, is imparted to the solution the vapor pressure
becomes equal to the atmospheric pressure and the liquid begins to boil ==
The vapor obtained from a boiling liquid, once cooled, will re-condense to a liquid known as the distillate The complete process is called a distillation
Separation of one liquid from another C + D Pure C? Pure D? Mixture of C + D? ==
CLASSIFICATION OF CONTINOUS COLUMNS :
Nature of feed Binary column Multi component column Number of product streams Multi product column Feed exits Extractive distillation Azeotropic
distillation Column Internals Packed columns Tray columns
Simple Distillation Vapors produced are immediately channeled into a condenser which cools and condenses the vapors Used only to separate liquids
whose boiling points differ by 25C
Heat Fractional Distillation Utilizes two or more vaporization condensation cyclces, in succession, to effect separation The fractionating column causes
the vaporization-condensation cycle to repeat by providing multiple surfaces for the cycle to take place
Vapors from the Distilling flask As the hot vapors leave the distilling flask, they condense on the first cold surface, completing one vaporization-
condensation cycle. Fractional Distillation
Vapors from the Distilling flask This cycle will continue until the top of the column is reached Each vapor-condensation (or mini-distillation) cycle is
known as one theoretical plate The length of distillation column required to provide one theoretical plate of separation is known as the height equivalent
theoretical plate (HETP)
Fractional Distillation Steam Distillation Methods for distilling compounds which are heat sensitive Involves a process using bubbling steam through
heated mixture of the raw material Applied for aromatic herbs and flowers Vacuum Distillation For compounds that have high boiling points
Air-sensitive vacuum distillation For compounds that have high boiling points as well as air sensitive Perkin Triangle apparatus can be used
Short Path Distillation Use for compounds which are unstable at high temperature Heating temperature can be considerably lower Destructive
Distillation involves the strong heating of solids (often organic material) in the absence of oxygen (to prevent combustion) to evaporate various high-
boiling liquids
evaporation Distillation method for the separation of mixtures of liquids by partial vaporization through a non-porous membrane. Dry Distillation a
chemical reaction known as pyrolysis in which solid substances are heated in a strongly reducing atmosphere and any volatile fractions are collected.
Extractive Distillation distillation in the presence of a miscible, high boiling, relatively non-volatile component, the solvent, that forms no azeotrope with
the other components in the mixture Flash evaporation partial vaporization that occurs when a saturated liquid stream undergoes a reduction in
pressure by passing through a throttling valve or other throttling device
Freeze Distillation analogous method of purification using freezing instead of evaporation It is not truly distillation, and does not produce products
equivalent to distillation Codistillation distillation which is performed on mixtures in which the two compounds are not miscible.
Principles of Distillation
What is distillation? ==Simply, distillation is the process in which a liquid is vaporized (turned to steam), recondensed (turned
back into a liquid) and collected in a container.
Nature uses a form of distillation to turn salt water (seawater) into fresh water (rain).
Why do you use distillation to recycle waste solvents? =Solvent-based waste contains volatile material (solvents) and non-volatile material (contaminants like paint,
ink, grease, fiberglass, etc.). Many of the non-volatile contaminates are dissolved in the solvent (like salt dissolved in salt water) and cannot be filtered-out.
Distillation is an ideal way to separate the two.
Why is distillation an ideal way to separate the two?=During the distillation process, the solvent-based waste is heated until it reaches the boiling point. It then
evaporates (vaporizes) and passes through the condenser where heat is removed from the vapor and it turns back into a cool, clean reusable liquid (same process
that causes dew to form). Fortunately, contaminates
are typically not volatile (easily vaporized) and stay behind in the distillation tank.
You say contaminates are typically not volatile, does this mean some are?= Occasionally there are cases where a potential customer wishes to separate a volatile
solvent from another volatile material. This is not the typical customer. Some cases include customers using an alcohol to remove water from parts to dry them or
where they have solvent mixtures due to poor
house keeping practices (they lump all waste solvents into one drum from different operations like painting and parts cleaning). To separate one volatile from
another effectively requires fractional distillation; our process uses simple distillation.
What are the differences between simple distillation and fractional distillation? =Simply stated, in simple distillation, what you put in is what you get back, but it is
free of non-volatile materials (it is clean!). Fractional distillation is much more complicated (and expensive). It is the base process where crude oil is turned into the
many items that come from oil. Fractional distillation is not
required for virtually all solvent recycling applications. What is vacuum distillation? ==Vacuum distillation is the distillation of a liquid under reduced pressure. The
atmospheric pressure in the distillation tank is reduced making it possible to boil the liquid at a lower temperature. Liquids boil at lower temperatures under reduced
pressure (the inverse is that a liquid boils at a higher temperature under pressure, which is why they use a pressure cap on an automobile radiator to increase the
boiling point of the engine coolant to prevent boil-over).
Why do you use vacuum distillation? =Vacuum distillation is used to safely recover higher boiling point solvents. We limit the maximum temperature of the
distillation unit’s heater. There is a temperature at which a flammable or combustible
material can ignite by temperature only, this is called the autoignition temperature (this is discussed later). Some solvents boil at temperatures that exceed the
temperature that the distillation heater can reach (392º Fahrenheit). Vacuum distillation lowers the boiling point to allow recovery within the heaters maximum
setting.
When do you use vacuum distillation? =It is used to safely recover solvents with boiling points over 300º Fahrenheit. Vacuum distillation should not be used on
solvents with boiling points below 200º Fahrenheit. If the maximum heater setting is 392º Fahrenheit, why do I need to use vacuum distillation for
solvents with boiling points over 300º Fahrenheit, don’t you mean solvents with boiling points over 392º Fahrenheit?
No! When boiling a liquid, two factors come in to play. One is the requirement to have a “driving force” to force the liquid to boil and vaporize. This “driving force”
is in the form of extra temperature to allow the solvent to develop a good rolling boil. The other factor is the role of the non-volatile residue. As you
boil off solvent and the remaining mixture in the distillation tank becomes more concentrated in the nonvolatile material, the vapor pressure drops (Raoult’s Law)
and most important, the boiling point goes up! So bottom line is that you need 50 to 100 degrees of extra temperature to do a good job of boiling the waste
solvent. Also, the concentrated non-volatile material acts as an insulator towards the end of the process as it becomes more and more concentrated. So, as the
percentage of non-volatiles in the contaminated solvent increases, the required heat to completely distill the mixture also increases. Sometimes solvents that have
boiling points of 318ºF (Xylene) may not require a vacuum if they are not highly contaminated but almost definitely would if the solid content was greater than, lets
say 10%. Pulling a vacuum on such a mixture will reduce its boiling point and the overall time to process it.
How is the vacuum created? =The vacuum is generated using our JetVac technology. A stainless steel reservoir is primed once with
clean solvent. A small stainless steel pump is immersed in the liquid and is attached to an explosionproof electric motor. When the motor is started, clean solvent is
drawn into the pump and forced through a metal tube known as an aspirator. The aspirator looks like an open piece of pipe with a small orifice (hole) on one side.
As the high velocity fluid is pumped across the face of the orifice, it creates suction (like a venturi on a carburetor). Air is pulled through the venturi from the
distillation system and passes through a vent.