Escolar Documentos
Profissional Documentos
Cultura Documentos
MTD Manufacture
Toluene Di- Amine formation:
The desired product of the hydrogenation reaction is 2,4 and 2,6 toluene
diamine isomers. The 80/20 mixture of these two isomers is commonly referred to as
MTD.
2,3 and 3,4 dinitro toluene are also reduced to corresponding toluene diamines, which
are commonly referred as ortho isomers (OTD). If the OTD is not separated from the
MTD it will react to cyclic urea in the phosgenation reaction. Cyclic urea reacts with
TDI, which results in yield loss.
A highly reactive catalyst system results in the further reaction of toluene diamine to
form volatile by-products such as para-toluidine and methyl diamino cyclohexanes.
A catalyst system with low activity results in several incompletely reduced products,
such as nitro amines and azoxy compounds.
Small amounts of dinitro benzene and trinitro toluene present in the DNT are reduced
to the corresponding amines
MTD Storage
The oxidation reaction that can take place at storage produces hydrogen ions.
With hydrogen ions present this by-product can react with other MTD molecules in
different ways. Water and ammonia produced in these reactions later reacts with TDI
and HCl to produce urea and ammonium chloride respectively and thus yield loss.
PROCESS DESCRIPTION:-
CATALYST PREPARATION
The catalyst for the MTD manufacture is produced batch wise in the tank reactor,
where demineralized water and other ingredients are mixed under specific conditions.
The ferric chloride solutions is first prepared with demineralized water and ferric
chloride in the dissolving tank. The solution is heated with the tanks low pressure
steam jacket and agitated with a nitrogen sparger. The solution is then held for
charging to the reactor kettle.
A second solution is then prepared in the reactor kettle with demineralized water. The
water is heated to 30 C with the vesselss low pressure steam jacket. The agitator is
started and the kettle charged with sodium chloride. After 15 minutes the solution is
checked for alkalinity and reagent grade HCl is added if necessary. Than palladium
chloride is slowly added to the reactor kettle. The resulting solution is agitated for 30
minutes.
Next, the ferric chloride solution is charged to the reactor kettle and Shawinigam
Black 100 is added. Sodium bicarbonate is then slowly added. More water is added
and the kettle is agitated for 30 minutes. The solution temperature is then increased to
90C and held for one hour, while continuing agitation.
The slurry is tested for precipitation completeness, then cooled rapidly to 60 C and
finally filtered with the catalyst filter. The filter cake is washed with demineralized
water. Filtrate and wash water are collected in the filtrate hold tank before being
discharged. The filter cake is sluiced to the catalyst slurry hold tank with
demineralized water. The agitator in the catalyst slurry hold tank is started and a
specified amount of demineralized water us used to wash the remaining catalyst from
the filter plates to the catalyst slurry hold tank.
Shawinigan Black 50 is added to the catalyst slurry hold tank, along with a metered
amount of demineralized water. This solution is agitated for two hours. The slurry is
then pumped to the catalyst slurry feed tank. From here, the slurry is then fed to the
hydrogenator as required, via the catalyst feed pump.
DEMINERALIZED WATER:
Demineralized water is pumped into the demineralized water tank from battery limit
for use in the MTD plant. The high pressure seal water pumps provide demineralized
water for the shaft seals of several process pumps. The lower pressure demineralized
water pump is used to supply demineralized water to the catalyst preparation process,
as well as for flushing the hydrogenation system at shutdown.
HYDROGENATION
Dinitro toluene is pumped for DNT plant at 70 C to the hydrogenator. DNT is fed
continuously at the rate needed to maintain the selected MTD production rate.
The hydrogen gas is supplied from battery limits and fed continuously at a rate
sufficient to maintain the hydrogenator pressure. The pressure of the hydrogen gas
supplied from battery limits id approx. reduced before injection in to the
hydrogenator.
Catalyst is fed at periodic intervals to the suction of the slurry recycle pumps which
discharges to the hydrogenator. Catalyst feed is stopped automatically when a pre-set
weight of catalyst slurry has been charged. The amount of catalyst feed is normally
calculated on the basis of DNT reduced. Occasionally, the feed rate is adjusted for
special reasons such as high or low DNT reactivity, or low solids in the
hydrogenator.
DNT is continuously hydrogenated to MTD in the presence of the catalyst. DNT and
hydrogen are fed continuously in to a reaction mass containing toluene
diamine(TDA), water and catalyst. The reaction mass is circulated by the
hydrogenator recycle pump through the hydrogenator recycle cooler to remove the
heat of reaction and then back to the top of the reactor, where it passes through the
jet-plate nozzles. The high velocity streams emerging from the jets impinge on the
liquid surface in the hydrogenator causing the gas to be entrained into the liquid, thus
producing intimate contact between the hydrogen gas and reaction mass.
The reactor temperature is maintained at 115C by controlling the cooling rate in the
external cooler. The hydrogenator is vented automatically through a vapour liquid
separator at a rate required to prevent the build of inerts in the hydrogenator. Vapor
space below the jet plate is maintained at a min. of 85 volume percent hydrogen on
water free basis. The venting rate varies with the inerts level in the hydrogen feed and
hydrogenation rate. The vent gases pas through the hydrogen vent seal pot for TDA
removal and continue to the incinerator or flare.
SLURRY THICKENING
TDA/water catalyst slurry is pumped from the hydrogenator and fed to a continuous
slurry thickener. The thickened slurry containing all of the catalyst, is then pumped
back to the hydrogenator, while the filtered TDA/water solution is sent to the wet
TDA storage tanks at a rate sufficient to maintain a constant level in the hydrogenator
. Periodically, some of the spent catalyst is removed and pumped to the unfiltered
TDA storage tank in order to maintain a constant inventory of active catalyst in the
hydrogenator.