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DEWAXING PROCESSES

Dewaxing Process
Paraffinic crude oils often contain microcrystalline or paraffin
waxes.
The crude oil may be treated with a solvent such as methylethyl-ketone (MEK) to remove this wax before it is processed.
This is not a common practice
Solvent dewaxing processes are designed to remove wax from
lubricating oils to give the product good fluidity characteristics
at low temperatures (e.g., low pour points) rather than from the
whole crude oil.
The mechanism of solvent dewaxing involves either
Separation of wax as a solid that crystallizes from the oil solution at low
temperature or
the separation of wax as a liquid that is extracted at temperatures above the
melting point of the wax through preferential selectivity of the solvent.

However, the former mechanism is the usual basis for


commercial dewaxing processes.

Paraffinic Oil Dewaxing


The lowest viscosity paraffinic oils were dewaxed by the
cold press method to produce oils with a pour point of 28 C
(35 8F) .
The light paraffin distillate oils contained a paraffin wax that
crystallized into large crystals when chilled, and could thus
readily be separated from the oil by the cold press filtration
method.
The more viscous paraffinic oils (intermediate and heavy
paraffin distillates) contained amorphous or microcrystalline
waxes , which formed small crystals that plugged the filter
cloths in the cold press and prevented filtration.
Because the wax could not be remove d from intermediate
and heavy paraffin distillates , the high-quality, highviscosity lubricating oils in them could not be used except
as cracking stock.

Methods were therefore developed to dewax


these high-viscosity paraffinic oils.
The methods were essentially alike in that the
waxy oil was dissolved in a solvent that would
keep the oil in solution; the wax separated as
crystals when the temperature was lowered.
The processes differed chiefly in the use of the
solvent .
Commercially used solvents were naphtha,
propane, sulfur dioxide , acetone benzene,
trichloroethylene, ethylenedichloridebenzene
(Barisol), methylethyl ketonebenzene ( benzol
), methyl-n-butylketone, and methyl-n-propyl
ketone.

Keton
e 1-4V

The process, as now practised , involves


mixing the feedstock with 1 to 4 times its
volume of the ketone
The mixture is then heated until the oil is in
solution
Solution is chilled at a slow , controlled rate
in double-pipe, scraped- surface
exchangers.
Cold solvent , such as filtrate from the
filters, passes through the 2 inch annular
space between the inner and the outer
pipes and chills the waxy oil solution
flowing through the inner 6 inch pipe.

To prevent wax from depositing on the walls of the inner pipe,


blades or scrapers extending the length of the pipe are
fastened to a central rotating shaft to scrape off the wax.
Slow chilling reduces the temperature of the waxy oil solution
to 28 C (35 8F), and then faster chilling reduce s the
temperature to the approximate pour point required in the
dewaxed oil.
The waxy mixture is pumped to a filter case into which the
bottom half of the drum of a rotary vacuum filter dips.
The drum (8 feet in diameter, 14 feet long), covered with filter
cloth, rotates continuously in the filter case.
Vacuum within the drum sucks the solvent and the oil dissolved
in the solvent through the filter cloth and into the drum.
Wax crystals collect on the outside of the drum to form a wax
cake, and a s the drum rotates, the cake is brought above the
surface of the liquid in the filter case and under sprays of
ketone that wash oil out of the cake and into the drum.
A knife- edge scrapes off the wax, and the cake falls into the
conveyor and is moved from the filter by the rotating scroll.

The recovered wax is actually a mixture of wax crystals


with a little ketone and oil
Filtrate consists of the dewaxed oil dissolved in a large
amount of ketone, which is removed from both by
distillation.
But before the wax is distilled, it is de-oiled, mixed with
more cold ketone, and pumped to a pair of rotary filters
in series, where further washing with cold ketone
produces a wax cake that contains very little oil.
The de-oiled wax is melted in heat exchangers and
pumped to a distillation tower operated under vacuum,
where a large part of the ketone is evaporated or flashed
from the wax.
The rest of the ketone is remove d by heating the wax
and passing it into a fraction al distillation tower
operated at atmospheric pressure and then into a
stripper where steam remove s the last traces of ketone.

Solvent dewaxing can be applied to light, intermediate, and


heavy lubricating oil distillates
Each distillate produces a different kind of wax.
Eac h of these waxes is actually a mixture of a number of
waxes.
Wax obtained from light paraffin distillate consists of a series
of paraffin waxes that have melting points in the range of 30
8 C to 708 C (90 8F to 160 8 F), which are characterize d by a
tendency to harden into large crystals .
How ever, heavy paraffin distillate yields a wax composed of
a series of waxes with melting points in the range of 60 C to
90C (140 8F to 200 8F), which harden into small crystals
from which they derive the name of microcrystalline wax or
microwax.
On the other hand, intermediate paraffin distillates contain
paraffin waxes and waxes intermediate in properties between
paraffin and microwax.

Solvent dewaxing process produces


three different slack waxes (also known
as crude waxes or raw waxes),
depending on whether light, inter
mediate, or heavy paraffindistillate is
process ed.
The slack wax from heavy paraffin
distillate may be sold as dark raw wax
Wax from inter mediate paraffin
distillate as pale raw wax.
The latter is treated with lye and clay to
remove odor and improve color.

Dewaxing Processes
Several processes in use for solvent dewaxing,
but all have the same general steps, which are:
Contacting the feedstock with the solvent ,
Precipitating the wax from the mixture by chilling,
Recovering the solvent from the wax and dewaxed oil for
recycling.

The processes use benzeneacetone (solvent


dewaxing), propane (propane dewaxing),
trichloroethylene (separator-Nobel dewaxing),
ethylene dichloridebenzene (Barisol
dewaxing), and urea (urea dewaxing), as well
as liquid sulfur dioxidebenzene mixtures.

Urea Dewaxing
Urea dewaxing is worthy of further mention in so far
as the process is highly selective and, in contrast to
the other dewaxing techniques, can be achieved
without the use of refrigeration.
Process cannot compete economically with the
solvent dewaxing processes for treatment of the
heavier lubricating oils.
When it is applied to the lighter materials that
already may have been subjected to a solvent
dewaxing operation, products are obtained that may
be particularly useful as refrigerator oils, transformer
oils, and the like.

The process description is essentially


the same as that used for solvent
dewaxing with the omission of the
chilling stage
Insertion of a contactor, where the
feedstock and the urea (with a solvent)
are thoroughly mixed before filtration.
The solvents are recovered from the
dewaxed oil by evaporation, and the
urea complex is decomposed in a urea
recovery system.

Residual lubricating oils, such as cylinder oils and


bright stocks, are made from paraffinic or mixedbase reduced crude oils and contain waxes of the
microcrystalline type.
Removal of these waxes from reduced crude
produces petrolatum, a grease-like material that is
known in a refined form as petroleum jelly.
This material can be separated from reduced crude
in several ways.
The original method was cold settling, whereby
reduced crude was dissolved in a suitable amount
of naphtha and allowed to stand over winter until
the microwax settled out.
This method is still used, but the reduced crude
naphtha solution is held in refrigerated tanks until
the petrolatum settles out.

The supernatant naphthaoil layer is


pumped to a still where the naphtha
is removed, leaving cylinder stock
that can be further treated to
produce bright stock.
The petrolatum layer is also distilled
to remove naphtha and may be clay
treated, or acid and clay treated to
improve the color.
Centrifuge dewaxing

Catalytic dewaxing
Catalytic dewaxing yields various grades of lube oils
and fuel components suitable for extreme winter
conditions.
Paraffinic (waxy) components that precipitate out at
low temperatures are removed.
In the UOP catalytic dewaxing process, the first stage
saturates olefins and desulfurizes and denitrifies the
feed via hydrotreating
In the second stage, a dual function, non noble metal
zeolite catalyst selectively adsorbs and then
selectively hydrocracks the normal and near-normal
long-chain paraffins to form shorter-chain (nonwaxy)
molecules.

Chevron Isodewaxing
Process
Dewaxing results from isomerizing the linear paraffins
to branched paraffins by using a molecular sieve
catalyst containing platinum
During isodewaxing process, which is followed by a
hydrofinishing step , waxy feedstock from a
hydrocracker or hydrotreater, together with the
hydrogen-containing gas, is heated and fed to the
isodewaxing reactor.
The conditions in the reactor cause isomerization of nparaffins to iso-paraffins, and other paraffins are
cracked to highly saturated low boiling products such
as jet fuel and diesel fuel.
The effluent from the isodewaxing reactor is then sent
to the hydrofinisher where hydrofinishing, including
aromatics saturation, provides the product.

The catalysts used in the isodewaxing


and hydrofinishing units are selective for
dewaxing and hydrogenation.
The catalysts are at their maximum
efficiency with low sulfur and low
nitrogen feedstocks.
The process generally uses a highpressure recycle loop. Because of the
conversion of wax constituents to other
usable products, the process has obvious
benefits over solvent dewaxing, insofar
as quality of the product is increased.

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