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PARAFFIN WAX petroleum by de-waxing light lubricating oil
stocks
Wax Sweating and Solvent De-oiling are the most commonly employed
processes for separating oil from slack wax. The current trend is more
towards solvent de-oiling though both methods are widely in practice.
In INDIA, production of petroleum wax started with the commissioning of
the wax sweating plant of the Assam Oil Company at Digboi Refinery. The
wax sweating process can’t be employed for de-oiling of all varieties of
feedstocks particularly those with high content of Iso-Paraffins which must
be handled by solvent de-oiling process only . The reason for this is the
amorphous nature and high viscosity.
Wax Sweating
Wax sweating has been defined as the process of drainage, fractional fusion, and
solution. In the solid state wax crystals have large number of interstices and voids
containing oil. On gradual heating, these cells expand and open up for the oil to
drain away.
Wax Sweating
A typical sweating oven comprises a vertical, shell and tube heat
exchanger. Wax from the lube oil de-waxing units is charged as a liquid to
the shell side of the oven, then solidified by running cold water through the
tube side. After the wax sets up, it is heated at a specified rate over a period
of many days. As the oven warms, the wax begins to melt.
The first liquid fractions to drain from the bed through the rundown line
have the lowest melting point and contain the most oil. Conversely, the last
liquid to come from the bed has the highest melting point and the least
amount of oil.
The liquid drippings collect in the bottom of the oven and drain into pans.
As each pan becomes full, the wax in the pan is typically tested for its oil
content. The results of this analysis determine whether the wax in the pan is
pumped to Foots oil for catalytic cracker feed, intermediate storage to be
re-sweat in another sweating oven, or to hi-fi feed storage to be processed
as finished wax.
Wax Sweating
In Conventional Practice, sweating continues until all of the wax has been melted
from the bed. Unfortunately, it is very difficult to control the quality and
composition of the actual wax product. It is determined in part by the size of the
pans and the oil content of the charge wax.
Conventional sweating requires that the oven temperature be raised slowly until all
of the wax has melted. In the Early Meltdown Method of wax sweating, however,
the slow heating (sweating) cycle is interrupted and stopped when monitoring of the
liquid drippings indicates that the solid bed of wax remaining in the sweating oven
has the desired properties of the final wax product. Then the sweating oven is shut-
in, the drain valve closed, and the sweating oven is heated at a rate substantially
faster than the sweating rate to melt the wax remaining in the sweating oven as
quickly as possible. This early interruption in the normal sweating cycle can save as
much as 50% of the actual sweating time and 30% of the overall time, which
includes charging, cooling, etc. Advantageously, the time savings achieved by the
early meltdown method of wax sweating substantially increases production volumes
and throughput for each sweating oven.
Solvent De-oiling
Waxy stocks for refined wax manufacture generally contain upto 30% oils
and can be considered to be made up of three components: oil, soft wax,
hard wax.
The solvent de-oiling process aims at separating the oil and soft wax from
hard wax using a volatile solvent such as MEK/MIBK
Solvent De-oiling
The main process steps involved are:
The waxy feed cooled by the passage through a double pipe chiller to
crystallize the hard wax portion. The chiller portion is equipped with
scraper blades to keep walls free of wax crystals.
A volatile solvent is added to dissolve the oil and soft wax components,
thereby maintaining a pumpable slurry of hard wax crystals.
A rotary vacuum filter separates hard wax crystals from the slurry and
bulk of liquid retained in the filter cake is displaced by application of
solvent wash.
Because the oil separation is incomplete more solvent is added, the
renewed slurry sent to a second rotary filter.
Solvent is expelled separately from wax cake and filtrate by heating
and steam stripping.
The solvent is dried before reuse on fresh feed.
Solvent De-oiling
Processes Variables:
Higher De-oiling Temperature result in a product of
lower oil content but wax yield is adversely effected.
Higher Solvent-to-feed Ratio, the possible gains in
degree of refinement will be weighed against increased
solvent losses.
Quality Control Of Petroleum Waxes
Tests associated with waxy nature of petroleum products:
1. Cloud and Pour point:-
Below the cloud point the petroleum products release their wax
components, thus forming a cloudy layer above the liquid fuel.
Similarly, pour point is a measure of waxy nature of oils
2. Melting & Setting point of wax:-
1. The point at which the temperature remains within a range of 0.1 OC
for one minute is taken as the setting point.
2. The congealing point of petrolatum is determined by applying a drop
of molten wax to a thermometer bulb, and noting the temperature at
which it congeals when thermometer rotates under a standard
cooling condition.
3. The drop melting point of wax is that temperature of the wax when a
drop of sample falls from the bulb of thermometer when heated
under standard heating conditions.
References
https://www.britannica.com/science/petrol
eum-wax
https://www.britannica.com/science/paraf
n-wax
https://www.britannica.com/science/microcr
ystalline-wax
https://www.britannica.com/science/petroleu
m-jelly
https://www.irmwax.com/FAQ/Classificati
on%20of%20petroleum%20waxes.aspx
https://patents.google.com/patent/US4824
553A/en
Dr Ram Prasad,Petroleum Refining
THANK YOU!!