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Chapter-
Separation processes

Impurities in crude
Impurities can be classified as
(i) Oleophobic (insoluble in crude oil)
(ii) Oleophilic (soluble in crude oil)

Oleophobic:
Includes, salts - mainly chlorides and sulphates of Na, Ca, Mg
Sediments as silt, sand, drilling mud, iron oxide, iron sulphate, etc.
Water as soluble, emulsifies and finely dispersed water
Caused corrosion in atmospheric distillation over head system caused by HCl
Increased consumption of ammonia to neutralize liberated HCl
Erosion of crude oil pumps, pipe line and valves by suspended matter
Plugging of equipments and fouling of heat transfer surfaces
Product degradation (e.g. High ash content in fuel oil)
Trace metal in distillates works as catalyst poison

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Oleophilic
Must be removed to remove problems in subsequent operations
Includes, sulphur compounds,
Organometallic compounds containing Ni, V, Fe, As, etc.,
Natphthenic acids,
and nitrogen compounds

Need for desalting of crude oil

Every crude oil has salt water together with sediments. Even crude oil can be
contaminated during shipping in tankers.

Salt content is normally measured as pounds of salt, measured as sodium

chloride, per thousand barrel of oil (PTB).

Normal salt range in oil = 10-200 TPB

Early method of separating impurities is primarily settling. Improvements can be

made by heating the oil before settling. Sometimes, chemical addition further
improves settling process also.

Electrical desalting is used by most refinery to reduce salt content.

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Electrical desalting of crude oil

Two step process (i) emulsification of crude and water (ii) demulsification by
means of electrical fields

Process variables affecting desalting

Pressure drop through mixing valve
Chemical addition
Water injection rate
Conductivity
Voltage
Desalter temperature
Desalter pressure
pH value
Solids at water-oil interface

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Typical operating conditions in different desalters

Crude oil distillation

Block diagram of two stage distillation process

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Desalted crude flows to atmospheric and vacuum

distillation through crude pre flashing section.

Heavier fraction of crude oil obtained from atmospheric

column requires high temperature. In order to avoid
cracking at higher temperature, the heavier fractions
are fractionated under vaccum.

Atmospheric distillation of crude oil

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Atmospheric distillation is carried out slightly above atmospheric

temperature to raise boiling point of light ends, to pressure
uncondensed gases and to allow for column pressure drop.

Desalted crude oil is first preheated (350-360C) in heat

exchangers and furnaces for required percentage of
vaporization in flash zone.

Furnace effluent is flashed into flash zone of atmospheric

column where vapour liquid separate.

The liquid leaving the flash zone is steam stripped to recover the
side-stream components.

The flashed hydrocarbon vapors from flash section are

fractionated into different sections above flash zone.

Intermediate refluxes are withdrawn to recover maximum heat

and to have uniform vapour and liquid loads in the column. They
exchange heat with cold streams and are returned to the
column.

Four fractions are separated in atmospheric column.

Overhead vapours are condensed. Overhead product is

separated as hydrocarbon and water, in reflux drum from which
water is withdrawn and sent to sour water section.

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The unstabilized neptha containing fuel gas, LPG and neptha is

partially refluxed and sent to neptha stabilizer section.

Three other products kerosene, light gas oil and heavy gas oil are
also withdrawn from different sections of the column.

Gas oil is withdrawn as other side stream from atmospheric

column which is used as diesel blending stock.

Prefractionation: It is known that crude contains high percentage

of light ends, a flash drum or a prefractionator with an overhead
condensing system may be used to recover most of the light
ends and a part of light neptha.

Typical yields of various products from atmospheric distillation unit

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Various streams from atmospheric and vaccum distillation column

Typical operating parameters for atmospheric crude distillation column

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Vacuum distillation
The atmospheric residue, commonly called reduced crude oil, contains a large
volume of distillable oils and further distilled.

This is carried out at sub-atmospheric pressure, i.e. vacuum.

Reduced crude oil is first preheated by heat exchange with products from
vacuum column and in furnace to get required of vaporization in flash zone (at
temperature of 380-400C).

Steam (about 30% of total steam) is introduced in furnace oil to decrease the
residence time and minimum cocking.

Depending on the weather vacuum column is used for middle distillate

production or lubricating oil production, there may be one or more side
streams.

Residue from vacuum may be used for bitumen production or it can be

blended with lighter streams to meet specifications like fertilizer feedstock.

Vacuum distillation process

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Steam is introduced at bottom section of column to reduce the partial pressure

of hydrocarbons in flash zone. This steam also helps to strip off light ends in the
bottom product.

The vapours and steam rise in the column and products are withdrawn at
different sections. Circulating refluxes are also introduced at different sections
of the column to balance the liquid and vapour loads in the column.

Overhead vapours are condensed by pre- and after condensers of ejector

system. Products are cooled and sent to storage tanks.

The vacuum column bottom product is quenched by adding a part of cold

vacuum residue in column, to avoid cracking of vacuum residue at high
temperature at bottom of the column.

Since raising the flash zone pressure increases the requirements of stripping
steam and column sectional area and lowering the system pressure increases
the steam requirement for vacuum producing jets. This requires optimum
pressure in flash zone.

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Operation of fractionating columns

Temperature
Top temperature of column is usually dew point temperature of over head
vapours at operating pressure.

Top temperature of column must be just high enough to allow complete

vaporization of overhead product. Vaporization at lower temperature can
incorporate desired overhead product in first side-stream product. A higher
temperature causes the inclusion of high boiling point components in
overhead products.

Bottom temperature of column is bubble point temperature of bottom liquid

and controls quality of the bottom products.

Side draw-off temperature is the temperature ate which desired product is in

liquid phase at operating conditions in the column.

The maximum limit of furnace outlet temperature is fixed at which the crude
starts cracking.

Column pressure
Normally pressure is not an operating variable. Higher pressure means higher
temperature requirement for vaporization.

For residue stock distillation, even atmospheric pressure may be high

considering the temperature requirement for distillation and thermal stability of
stock. So, vacuum distillation is done.

Since high pressure operation reduces relative volatility of components, more

reflux and more reboiled heat are required for achieving the same
fractionation at higher pressure.

The column diameter can lower at higher pressure due to higher vapour
density.

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Flow rates
Feed to distillation column is determined by production demand placed on the
plant and by capacity of distillation equipments.

Flow rates of overhead and bottom products from a column are determined by
feed composition and degree of separation which is a function of reflux rates.

Reflux
Firstly, it provides liquid in the rectifying section to cause vapour-liquid contact
resulting in fractionation.

Secondly, it is provided to maintain temperature gradient in the column.

Higher reflux ratio results in better separation between light and heavy fraction
but requires higher condenser and reboiler loads (loss of energy).

Reboiler/ Stripping steam

To provide vapour in stripping section of column for vapour-0liquid contact,
either re-boiler is used or steam is admitted directly into bottom of the column.

Supplying steam has additional advantage of lowering partial pressure of liquid

being distilled throughout column.

Stability of column operation

Effectiveness of the column depends on intimate contact of vapour and liquid
streams on each tray to provide vaporization of light fraction and
condensation of heavy ones.

When the liquid or vapour rate inside the column becomes too low or too high,
the contact is insufficient and poor separation results.

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Pulsation: When amount of vapour passing through a tray is so small that

bubble cap pass vapour intermittently.

Dumping: This results at relatively high liquid loads when some of the
upstream bubble caps do not pass vapour.

Coning: This takes place when the combination of weir height and liquid crest
over weir does not adequately seal the cap slots. If the slots are not sealed
properly, vapours can pass to the tray without contacting liquid on the tray.

Blowing: This results when amount of vapours passing through bubble caps is
so large that it literally tears holes in liquid on the tray.

Entrainment

Important points for improvements in fractionating column

Degree of separation achieved is a function of number of trays and reflux ratio for a
specific pressure. The addition of trays results in higher initial investment but it can allow
lower reflux ratios and thus energy requirement can be reduced.

For efficient operation, the feed to a column should be admitted at correct point
according to composition. The feed should be added in form of vapour-liquid mixture
in which the proportion of vapour is about the same as proportion of overhead
product.

The consumption of stripping steam is dependent on three parameters, viz. degree of

fractionation obtained in main column, stripper design and desired quality of product
(flash point). Excessive use of steam is a wastage of energy apart from increase in
column and condenser loads.

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