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1.1 GENERAL
Most aniline is produced by reduction of nitrobenzene in various liquid and
vapour phase reactions using a variety of catalyst.
1.2 INTRODUCTORY
Du Pont has produced aniline from nitrobenzene by a proprietary catalysed
liquid phase Hydrogenation process since 1960. The first production unit was
situated in New Jersey, But is has now been dismantled. A plant at Beaumont,
Texas, was started up in 1972 and is the sole Du Pont aniline production unit.
Crude aniline, containing non-reactor NB, water, and excess hydrogen, which
leave the top of The reactor as vapours or gases, are cooled and condensed through
a cooling train. This Cooling train consists of two waste heat boilers, which
generates medium pressure steam, a set of boiler feed water pre-heaters and
finally water-cooled heat exchangers. The final cooling is critical to reduce the
temperature of the stream to <40C to promote gravimetric separation. After
cooling, this stream enters a gas-liquid separator and pressure letdown tank where
the un-reacted hydrogen is separated from the liquid water/aniline mixture. The
un-reacted gases are discharged through a pressure control valve, which controls
the pressure at the top of the aniline reactor, and are returned and used as fuel.
The crude aniline and water are separated in a gravimetric decanter. The
water wet crude aniline is transferred to storage for refining. The water phase,
containing dissolved aniline is drawn off and stored in a coarse water tank for
recycle as a direct coolant to the aniline reactor or for aniline recovery by
extraction.
EXTRACTORS
This system consist of two stages of counter-counter, liquid-liquid extraction
Which utilize static mixers to promote contact between phases. Nitrobenzene
Extracts and recovers the dissolved aniline from the water generated in the Aniline
synthesis reactor. The nitrobenzene, containing recovered aniline,
Discharges from the first stage extractor (S0905) to a reactor NB feed tank (T1001)
and is pumped by high speed centrifugal pumps (P1002 A/B) to the aniline reactor
(R1004) for conversion to aniline. The extracted process water, containing < 100 ppm
(wt) of aniline, is transferred to waste treatment facilities. The extractors are
comprised of two horizontal, cylindrical tanks, each equipped with an internal static
mixer. After the intensive mixing the two forming phases are allowed to separate.
The water phase overflows a baffle near the end of the vessel into a small
component from which it is transferred by a centrifugal pump P0906 (first stage
extractor)/P0904 A/B (second stage extractor). Nitrobenzene, the heavy phase,
discharges through a nozzle in the bottom of the extractor vessel.
Raw process water, containing about 4% (wt) aniline, is mixed with
Nitrobenzene from the second stage extractor (S0901), and fed to the static Mixer in
the first stage extractor (S0905).
The light and heavy phases separate in the extractor vessel. The
Nitrobenzene Phase discharges from the first stage extractor by gravity to the
reactor NB feed tank (T1001). The water phase from the first stage extractor is
transferred and mixed with fresh nitrobenzene as the feed to the second stage
extractor. The light and heavy phases separate in the extractor vessel. The
nitrobenzene phase from the second stage Extractor is pumped (P0902 A/B) to the
static mixture of the first stage extractor. The water phase from the second phase
extractor is pumped to a storage tank (T9410) for Waste treatment. A portion of the
heavy liquid from the each extractor can be recycled back to the static mixture feed
point of that stage to maintain a high liquid velocity through the mixers.
PROCESS PARAMETETRS
PROCESS PARAMETERS
NB PREHEATER
Nitrobenzene is preheated with steam in shell and heat exchanger (E1003),
to Promote reaction, and is fed to the bottom of the aniline reactor (R1004).
PROCESS PARAMETERS
ANILINE REACTOR
The aniline reactor is a multi-stage, trayed, vertical column. Nitrobenzene,
recycled process water, catalyst slurry, and aniline, are introduced into the bottom
of the column, below the first tray. Hydrogen is fed to the bottom of the reactor
through a ring pipe distributor. At operating pressure, hydrogen dissolves in the liquid
mixture and reacts with nitrobenzene, in the presence of the catalyst, to form
aniline and water. The reaction is highly exothermic and aniline and water are
vaporized and removed overhead as vapour. The temperature of the reactor is
controlled at a mid-column high temperature of 215-230 C by feeding recycled
process water and aniline. The reactor vapour line is provided with a rupture disc
and relief valve in series to protect from vessel over-pressure.
PROCESS PARAMETERS
DEGASIFIER
Since catalyst particles tend to migrate to the top of the reactor, a liquid
side stream containing aniline, tar, water and catalyst is drawn-off from the top tray
of the reactor through a gas-liquid separator or Degasifier (S1005). The gas is
returned to the vapour space above the top tray and the liquid side stream is
processed through the catalyst recycle system.
PROCESS PARAMETERS
SAFETY TANK
The over-pressure protection devices on the reactor vapour line discharge to
a safety tank (T1006), which contains and separates the gas and liquid discharged
from the reactor, should an over-pressure occur. The vent on this tank is equipped
with a Steam sparger to prevent light-off of gases by a lightning storm. This tank is
also used to receive draining from the reactor when it is emptied for inspections and
maintenance. Aniline and catalyst are recovered from the safety tank by filtration.
PROCESS PARAMETERS
REACTOR COOLING
Aniline, water vapour and un-reacted hydrogen in the overheads of the
aniline reactor pass through a cooling train, which cools and condenses these
vapours. This cooling train consists of two kettle type steam boilers product
condensers (E4301/E4302), one shell- and-tube product cooler (E4303), which boiler
feed water, and two water cooled shell- and-tube trim coolers (E4304/E4305).
The product condensers are a kettle type reboiler with process on the tube
side of a U-tube bundle. The shell contains boiler feed water and produces steam at
two different Pressures. The boilers are equipped with two mesh type demisters
(S4301.01/S4302.01)
The trim coolers are water-cooled, shell and tube type exchangers with process on
the tube side and cooling tower water on the shell. They are designed to cool the
water/aniline/non-condensable stream to a temperature that minimizes entrainment
of liquid in the gas phase during subsequent separation and enhance separation of
the aniline and water phases.
PROCESS PARAMETERS
PROCESS PARAMETERS
PROCESS PARAMETERS
CRUDE DECANTERS
The cooled water and aniline products from the aniline reactor coolers are
directed to one of two vertical, cylindrical decanters here the aniline and water
phases are allowed to separate by gravity. One of these tanks is called the product
decanter (S1101) and the other, the off-spec decanter (S1108). The water phase from
these decanters overflow to the coarse water tank (T1114). The aniline phase from
the product decanter is pumped (P1102A/B) to one of two crude analysis tanks
(T1103/T1104). The aniline phase from the off-spec decanter is pumped (P1109 A/B)
to rework aniline storage tank (T1110)
PROCESS PARAMETERS
PROCESS PARAMETERS
PROCESS PARAMETERS
PROCESS PARAMETERS
THICKENER
A portion of the cooled, liquid side stream is processed through a thickener (F4508
A/B). The thickener serves to purge soluble tars from the aniline reactor system by removing a
small stream of filtrate, which contains soluble tars generated in the aniline reactor. The bulk of
the side stream slurry circulated through the thickener is returned to the thickener feed tank
(T4502). The small stream of thickener filtrate is transferred to the purge recovery column feed
tank (T1709) for further processing for aniline recovery and tar disposal.
PROCESS PARAMETERS
Operating pressure 6 bar a
Operating temperature 95 C
CATALYST FILTER
A catalyst filter (F4509) is provided to recover catalyst solids for return to a Catalyst
manufacturer for precious metals recovery whenever the aniline Reactor is emptied, or when
material accumulates in the Safety Tank (T1006).
PROCESS PARAMETERS
PROCESS PARAMETERS
PROCESS PARAMETERS
PROCESS PARAMETERS
PROCESS PARAMETERS
DEHYDRATION COLUMN
Crude aniline, which contains about 5.5% (wt) of dissolved water, is pumped (P1107
A/B) From the crude storage tank to the dehydration column (C1201) for water removal. This
Column is equipped with structured packing. Vacuum pumps (B1801/B1802) provide the
necessary sub-atmospheric pressure for the column operation. A steam heated, forced draft
reboiler (calandria) (E1203), and pumps (P1202 A/B) provide the circulated draft, provides
boil-up for the column. An overhead condenser (E1204) condenses and cools the water and
aniline mixture stripped from the crude material. The overheads stream is returned to the
product decanter (S1101) where it is recycled to the process. The dry bottoms stream,
containing < 0.05% (wt) of water, is pumped to the Schiffs base Reactor (R1302) through the
base reactor preheater (E1301).
PROCESS PARAMETERS
PROCESS PARAMETERS
RECTIFIER COLUMN
Dry aniline is pumped from the Schiffs base reactor column (C1501).This column is
A trade column. The column operates at sub-atmospheric pressure by the use of vacuum
pumps(B1801/B1802). It has also a forced draft, steam heated reboiler (calandria) (E1503).
Refined aniline is taken overhead and condensed in a water cooled condenser (E1504) from
which it is pumped (P1507 A/B) to finished product analysis tanks (T1671/T1672).A small
bottom stream is drawn from the rectifier column to remove tars and Schiffs base as high-
boiling impurities. This stream is pumped either to the purge recovery Column (C1701) for
recovery of aniline or directly to the tar heels tank (T9420) for disposal by burning in the
incinerator (H9424).
PROCESS PARAMETERS
PROCESS PARAMETERS
PROCESS PARAMETERS