Overview
Overview
Prepared by:
International Process Plants
Hamilton Business Center
17A Marlen Drive
Hamilton, NJ 08691
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The facility had some upgrades over the years. The majority of the site shut down in
2009, but the cyclohexane unit ran until August 2013.
The plant has been well-maintained and is still being kept up with a staff of four
employees. There is a nitrogen pad on the process and they are turning the rotating
equipment monthly.
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This Caprolactam Facility includes all intermediate and byproduct plants. The facility
starts with benzene and finishes with caprolactam and ammonium sulfate byproduct:
• Cyclohexane Plant – 80 kmta • Ammonium Sulfate – 108 kmta
• Cyclohexanone Plant – 55 kmta • Incinerator – 5 m3/hr liquid
• Oximation Plant – 62 kmta waste
• Caprolactam Plant – 60 kmta
The total facility uses the following raw material and utility quantities:
Benzene = 79 kmta Electricity = 52 GWhr/yr Nitrogen = 6.0 MMNm3/yr
Hydrogen = 10 kmta Steam = 720 kmta Fuel Oil = 1.0 kmta
Ammonia = 50 kmta Air = 33 MMNm3/yr
Sulfuric Acid = 78 kmta Water = 1.3 MMNm3/yr
The following chart shows more details about the sub-processes within each of the
individual units.
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Cyclohexane Plant
Hydrogenation of Benzene to Cyclohexane
U-5200 Plant Designation
No sub-series - unit operations listed below:
Benzene Evaporation
Hydrogenation
Separation
Ammonia Refrigeration Unit
Cyclohexanone Plant
Oxidation of Cyclohexane to Cyclohexanone
U-5000 Plant Designation
Series:
5000 Utilities (includes incinerator)
5400 Oxidation
5500 Absorption
5600 Neutralization/Hydrolysis
5700 Distillation
5800 Purification
5900 Conversion of Cyclohexanol to Cyclhexanone
Cyclohexanone-Oxime Plant
Oximation of Cyclohexanone to Oxime
U-6000 Plant Designation
Series
6000 Utilities
6100 Hydrogen Purification
6200 Hydroxylamine Preparation
6300 Oximation/Neutralization/Washing
6400 Touene/Oxime Distillation
6500 Toluene Extraction/Separation
6600 Ammonia Burner
6700 Nitric Adsorption Nitric Acid Plant
6800 NOx Removal
Caprolactam Plant
Rearrangement of Oxime to Caprolactam & Ammonium Sulfate
U-7000 Plant Designation
Series:
7000 Utilities (Includes Effluent Evaporator, Incinerator)
7200 Rearrangement
7300 Extraction
7400 Ion Exchange
7500 Hydrogenation
7600 Evaporation
7700 Distillation
7800 Flocculation
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Cyclohexane Plant
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The drying column has 20 sieve trays, a reboiler, and an overhead condenser
system. The carbon steel column is 0.7 meters diameter by 12.5 meters tall and is
rated for 2.6 bar at 115oC. There is an azeotropic mixture going overhead in the
column at 15,000 ppm water. This stream is used for reflux in the drying column.
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The hydrogenation reactor products then flow to the after-reactor which is filled with
zinc oxide catalyst in the first bed and platinum catalyst on aluminum oxide substrate
in the second bed. The after-reactor is 2.2 meters diameter by 5.2 meters tall. It is
rated for 34 bar at 315oC. All catalysts have been removed from the reactors.
The cyclohexane product is then cooled with a steam-generating boiler and some
other cross-exchangers for energy efficiency. The carbon steel boiler is 2.4 meters
diameter by 5.8 meters long and is rated for 21 bar at 226oC. The condensed
product is sent to the heptane column where n-heptane and other high-boiling
compounds are removed. Pure cyclohexane exits the top of the heptane column.
The pure cyclohexane product is then condensed and pumped to storage. The
heptane column has been removed because it was not necessary.
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The Cyclohexanone Plant uses 80 kmta of cyclohexane along with some air to
produce 55 kmta of pure cyclohexanone. The oxidation reaction takes place in a
series of four agitated reactors followed by multiple distillation and separation steps.
The plant closed in 2009.
The cyclohexane feed first enters the cooling scrubber column. The overheads from
this column go to the cyclohexane absorber while the bottoms stream proceeds to
the direct heat exchanger column. This column prepares the cyclohexane for the
oxidation reaction.
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The reaction products from the oxidation reactors flow to a series of separators. The
overhead vapors from the separators proceed to the series of three distillation
columns. The liquid in the separators flows to the stripper column. The bottoms or
heavies flow from the stripper column are sent to the incinerator. The overheads
from the stripper column proceed to the drying column. The drying column also
receives feed from the salt extraction column and from the dehydrogenation reactor.
The bottoms from the drying column go to the forerun column. The overheads from
the forerun column are sent to the incinerator. The bottoms from the forerun column
are pumped to the large anone distillation column. The overheads from the anone
distillation column are the final cyclohexanone product which is condensed and sent
to storage. The bottoms from the column are pumped to the anol distillation column.
The bottoms or heavies from the anol distillation column are pumped to the
incinerator.
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The overheads from the oxidation reactor separators mentioned earlier flow to the
series of three distillation columns. The overhead from these columns go back to the
oxidation reactor feed lines. The bottoms from the distillation columns are pumped to
a caustic mix vessel for neutralization. The bottoms from the mix vessel are then
pumped to a salt extraction column. The bottoms from this column are pumped to
the waste water line, and the overheads are sent back to the drying column as
previously mentioned.
The specifications for all of the columns in the Cyclohexanone Plant are shown in the
table below. Sulzer reciprocating vacuum pumps are used to supply vacuum on
some of the columns.
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Oximation Plant
The Oximation Plant uses 55 kmta of cyclohexanone along with some hydrogen and
nitric acid (produced in the unit) to manufacture 62 kmta of the oxime intermediate.
The hyam (hydrogen + nitric acid) reaction takes place in a large column reactor and
the oximation reaction takes place in a series of seven agitated reactors followed by
multiple distillation and separation steps. The plant, which is primarily 304 stainless
steel construction, closed in 2009.
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Nitric acid is produced for the hyam reaction in a small nitric acid plant. The plant
can produce about 130 mt/day (dry basis) of 37% nitric acid. With some
modifications, it can probably produce the same amount of acid at the more typical
67% concentration.
The combustion of ammonia takes place at 5.0 bar and 880oC with five layers of 90%
platinum/10% ruthenium gauze catalyst. The total catalyst charge is typically 1,529
grams.
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There is a complete new ammonium burner system which was never used. The
original cost was $2.5MM. This includes the burner, the NO x removal reactor, and
some downstream boiler/exchanger equipment.
The reaction products from the ammonia burner proceed to the large absorber
column. The column is 3.0 meters diameter by 54.1 meters tall. It is constructed of
304 stainless steel and is rated for 7.5 bar at 95oC. The column has 31 sieve trays.
The overheads from the absorber column proceed to the NO x removal reactor which
uses palladium catalyst on an alumina support for destruction of the NO x products.
The stream then proceeds to the tail-gas expander mentioned earlier to assist in
driving the process air compressor. The expanded tail gas then exhausts through a
tall stack.
Absorber Column
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The oximation reaction consists of the hyam reacting with cyclohexanone to produce
the cyclohexanone-oxime with a toluene solvent. Approximately 98% of the
cyclohexanone is converted in the oximation reaction section, while the remaining
2% is converted in the neutralization section of the plant. The seven agitated
oximation reactors are 3.7 meters diameter by 3.0 meters tall. They are constructed
of 304 stainless steel and are rated for 0.1 bar at 85oC.
The oximation reaction products then
proceed through two vacuum
distillation columns for removal of the
toluene and impurities. The bottoms
flow from the second vacuum
distillation column is cyclohexanone-
oxime product ready for rearrangement
in the caprolactam unit described in
the next section of this report. The
overheads from the two vacuum
distillation columns consist mainly of
toluene. This stream goes through an
extraction column and a toluene
stripper column for recovery and
recycle of the toluene back to the
oximation reactors. The bottoms
stream from the toluene stripper is
primarily water and is recycled to the
NO x absorber column in the nitric acid
plant. Oximation Reactor
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Caprolactam Plant
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The overheads from the ammonium sulfate extraction column are fed to the
caprolactam extraction column. This extraction takes place with benzene in a
rotating-disc extraction column. The rotating discs are variable speed from 34 to 61
rpm. The column is 1.7 meters diameter by 18.1 meters tall. It is constructed of 304
stainless steel and is rated for 1.8 bar at 115oC. The bottoms stream from the
column goes to the incinerator. The overheads proceed to the re-extraction column.
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There are six ion exchange beds operating in two groups of three beds. One group
of beds will be in service while the other group is being regenerated. The first bed in
each series is packed with anion resin, the second bed with cation resin, and the
third and final bed again with anion resin.
The product from the ion exchange section is then hydrogenated in a two-stage
hydrogenation reaction system rated for 10.8 bar. The system uses Raney nickel as
catalyst. This process saturates and of the unsaturated compounds in the product.
The aqueous caprolactam solution which was just hydrogenated is now sent through
two vacuum distillation columns to take the caprolactam concentration from 30% to
85%. The first vacuum distillation column is 1.4 meters diameter by 10.5 meters tall
with eight sieve trays. It is constructed of 304 stainless steel and is rated for 4.8 bar
and full vacuum at 165oC. The second vacuum distillation column is 2.7 meters
diameter by 13.9 meters tall with 10 sieve trays. It is constructed of 304 stainless
steel and is rated for 2.8 bar and full vacuum at 135oC. Vacuum is supplied by two
liquid-ring vacuum pumps.
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Evaporator
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The Ammonium Sulfate Plant produces 108 kmta of solid ammonium sulfate
byproduct. The plant consists of evaporation, crystallization, centrifugation, and
drying processes. The plant, which is almost entirely 304 stainless steel
construction, closed in 2009.
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The plant receives its feed as a 52% ammonium sulfate solution from the bottom of
the ammonium sulfate extraction column in the Oximation Plant mentioned earlier in
this report. The solution first enters the evaporator section of the plant. The
evaporators take 30 m3/hr of solution from 52% to 60% ammonium sulfate in the first
evaporator and from 60% to 65% in the second stage evaporator. This equates to
about 8,750 lbs/hr of water removal capabilities.
The solution drops from the second evaporator into a large crystallizer. The
crystallizer is 7.2 meters diameter by 9.3 meters long. It is constructed of 304
stainless steel and is rated for atmospheric pressure at 100oC.
The solution is then pumped from the crystallizer to the two Escher Wyss centrifuges
for thickening. Mother liquor from the centrifuges is recycled back to the crystallizer.
Thickened product is transported by screw conveyor to the dryer.
Centrifuges
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The dryer is 2.3 meters diameter by 8.4 meters long. It is constructed of 304
stainless steel and is rated for 0.1 bar at 180oC. Air for the dryer is steam-heated
with a large 304 stainless steel exchanger. The heater is 1.4 meters diameter by 4.0
meters long and is rated for 1.8 bar at 103oC.
The dry ammonium sulfate discharges from the dryer onto a flat conveyor belt. The
conveyor takes the product to a bucket elevator which transfers the product through
some sieves and onto another conveyor belt going to the warehouse. The product
dumps onto the large concrete warehouse floor and is moved with front-end loaders
to desired warehouse locations.
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Incinerator
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There are two incoming electrical feeders with automatic switching gear which is
included in the plant sale.
There are 13 transformers in the 1,000 to 2,000 kva range. The frequency for all
electrical equipment in this facility is 60 Hz.
There are three cooling tower cells with three Worthington cooling tower water
pumps. The cooling tower is in poor condition, but the pumps are in good condition.
There are four Trane chillers which appear to be about 300 tons of refrigeration
capacity each.
There are two Centac instrument air compressors. The compressor is missing from
one of the units.
There are two diesel-driven fire water pumps capable of 18 bar discharge pressure.
There are about 17 major tanks in the tank farms. They are a mix of carbon steel
and 304 stainless steel construction.
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Equipment List
Ma jor Equipme nt De scription Dia me te r He ight Pre ssure Te mp Ma te ria l of
Qua ntity (m) (m) (ba r) (o C) Ye a r Comme nts Construction
Cyclohe x a none Pla nt (5000)
C5401 Cooling Scrubber 1 2.0 22.6 12.8 215 3-packed 304SS
C5402 Direct Heat Exchange Col 1 2.8 13.0 12.8 215 2-packed CS
C5501 Cyclohexane Absorber 1 0.9 14.3 12.8 90 2-packed 304SS
C5601 Stripper 1 1.2 13.6 2.3 175 1-packed 304SS
C5602 Salt Extraction Col 1 1.8 11.4 5.2 115 1-packed CS
C5701 1st Distillation Col 1 2.3 20.4 7.3 175 18-Sieve CS
C5702 2nd Distillation Col 1 2.2 21.5 7.3 175 18-Sieve CS
C5703 3rd Distillation Col 1 3.2 25.9 7.3 190 21-Sieve CS
C5801 Drying Col 1 1.2 16.3 2.3 190 14-Sieve CS
C5802 Fore Run Col 1 1.6 38.3 1.8/FV 190 60-Sieve CS
C5803 Anone Distillation Col 1 3.0 49.7 1.8/FV 190 80-Valve CS
C5804 Anol Distillation Col 1 3.0 28.6 1.8/FV 190 30-Sieve CS
E5502 Ammonia Evaporator 1 1.3 6.2 26.4 75 CS
E5701A/B - C5701 Reboilers 2 1.1 5.5 16.8 280 CS
E5702 - C5702 Reboiler 1 1.7 6.7 7.3 175 1988 CS
E5703A/B - C5703 Reboiler 2 1.6 7.2 7.3 175 CS
E5705 Distillation Condenser 1 2.3 7.2 2.3 115 CS
E5801 - C5801 Reboiler 1 1.0 5.2 16.8 280 CS
E5802 - C5802 Reboiler 1 1.1 4.0 16.8 280 1987 CS
E5806 - C5803 Reboiler 1 1.0 5.2 16.8 280 CS
E5807 - C5803 Condenser 1 1.8 7.7 1.8 115 CS
E5812 - C5804 Reboiler 1 1.4 5.4 16.8 280 1999 CS
E5813 - C5804 Condenser 1 1.5 6.4 1.8 130 CS
F5901 Hot Oil Furnace 1 3.1 23.2 ATM 565 CS
R5411-14 Oxidation Reactors 1-4 4 3.4 6.0 12.8 190 Agitated CS
R5419 Post Oxidation Reactor 1 3.4 6.5 12.8 190 CS
R5901 Anol Reactor 1 2.6 7.2 1,483 tubes CS/CS
S5401 Water Separator 1 2.5 7.6 14.3 175 CS
S5601-3 Separator/Neutralizer 1-3 3 2.6 7.8 20.4 190 CS
S5702 Reflux Vessel 1 3.1 7.7 2.3 115 CS
V5004 Ammonia Storage Tank 1 1.5 8.2 27.5 62 CS
V5401A Cyclohexane Recirc Tank 1 3.8 8.4 2.3 115 304SS
Ta nk Fa rms
T0201 Caustic Tank 1 5.8 6.9 ATM 132 304SS
T0202 Oleum Tank 1 1.5 2.7 ATM 172 304SS
T0203 Sulfate Tank 1 4.0 5.4 ATM 73 304SS
T0301 Sulfuric Acid (98%) Tank 1 8.2 10.6 ATM 45 CS
T0302 Oleum Tank 1 8.1 9.1 ATM 45 CS
T0303 Ammonium Sulfate Tank 1 10.4 12.1 ATM 60 304SS
T0304A Caustic Tank 1 4.8 6.1 ATM 55 304SS
T0304B Caustic Tank 1 2.9 20.0 17.6 343 CS
T5201A/B Benzene Tanks 2 8.5 10.6 ATM 65 CS
T5202A Cyclohexane Tank 1 8.2 10.6 ATM 65 CS
T5202B Cyclohexane Tank 1 13.4 15.6 ATM 65 CS
T5802A Intermediate Tank 1 5.7 7.6 0.1 190 1987 CS
T5803 Cyclohexanone Tank 1 11.6 14.4 ATM 90 CS
T7801A/B/C Caprolactam Tanks 3 9.0 12.1 ATM 140 304SS
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