Process Description

Introduction
The process described is for a Nickel Oxide Reduction Plant to be built for the client. The
plant will be located at Panki situated in Kanpur Nagar, Uttar Pradesh, India. Aker
Solutions E&C Ltd, Stockton on Tees, UK, has provided a technology package which
has been used to carry out a FEED by Aker Solutions, Mumbai, leading on to the
detailed design phase.
The main chemistry of the process is the reduction of nickel oxide to nickel using
recirculating hydrogen gas through a reactor which contains the catalyst. In order to
ensure that the nickel catalyst is not oxidised back to nickel oxide once it is removed
from the reactor, CO2 and air are also fed to the catalyst within the reactor in order to
form a coating around the catalyst. Any moisture which is produced from the reduction
step is removed in a knockout pot and sent to an effluent pond, which is outside the
scope of Project 123. Any gases that require to be vented during the reduction, CO2 or
air stabilisation steps, or during the nitrogen purge steps will be vented to a safe
location.
Overall Description
The process gas will be compressed up to the desired pressure by the circulator. The
gas will be heated up due to this compression and therefore heat will be partially
removed from the stream by an aftercooler and afterchiller unit located downstream of
the circulator during process steps when this is necessary. Otherwise the aftercooler and
afterchiller will be bypassed so as to utilise the heat of compression in order to raise the
temperature of the process gas.

This will therefore reduce the amount of heating

required by the electric heater. Pressure letdown valve, located downstream of the
Circulator, is adjusted to kill the pressure of the gas stream being fed to the aftercooler
and afterchiller depending on the process step. The gas stream will then be fed to a
series of 3 heat exchangers (collectively called the interchanger) where it will be heated
countercurrently by the exit gas stream of the reactor. A bypass facility will be allowed for
the gas stream to partially bypass the interchanger to allow temperature control of the
cooled gas leaving the interchanger. The heated gas stream will then be further heated
up to the desired temperature, as required depending on the process step, by an electric

heater. The gas stream will then be fed to the reactor where it will react with the catalyst
and depending on the process step will either reduce the NiO to Ni (section 2) or
stabilise the Ni by forming a layer on the catalyst so as to prevent the re-oxidation of Ni
(sections 4 & 5). The gas stream exiting the reactor will pass back through the
interchanger. The gas stream will then be filtered and fed to a second cooler and chiller
unit. Prior to feeding the cooler a vent line will allow venting of the main gas loop, if
required, depending on the process step. The gas stream will be cooled in the cooler
and further in the chiller to cause the water (produced in the reaction see section 2) in
the stream to condense and be separated from the gas stream in the downstream
knock-out pot. Condensed water will be sent to the effluent pit. During other process
steps there will be no water being produced so the chiller can be bypassed to save
energy. CO2, H2 and process air will all be supplied to the knock-out pot, depending on
the process step being carried out, where the gas will join the main process loop. The
additional gas is to replace losses from the reaction or vent. The gas stream leaving the
top of the knock-out pot will then feed into the suction side of the circulator where it will
be compressed and once again sent to the aftercooler / afterchiller unit. Nitrogen gas
used for the pressurisation / depressurisation stage and purging stage will be fed into
the main gas stream, upstream of the interchanger prior to heating and feeding the
reactor.

Details of the process will be split into the following sections:

Section
2.0

Reduction of NiO Catalyst

3.0

Hot N2 Purge

4.0

CO2 Stabilization

5.0

Air Stabilization

6.0

Summary

This document should be read in conjunction with the following documents:

1) Aker Solutions Document 1707-10-7007-001, Process Design Basis.
2) Aker Solutions Piping and Instrumentation Diagrams (P&IDs), 1707-7001-10-L001 to
L007.

2.0 Reduction of NiO catalyst

This plant is designed to reduce and stabilise a range of nickel catalysts in a batch
process of between 3 to 6 days duration, depending on the catalyst type. Up to 12m 3
of catalyst is charged into the reactor vessel and reduced in circulating hydrogen at a
maximum temperature of 700C. The actual temperature varies from catalyst to
catalyst. The gas stream will be heated at a defined rate using an electric heater,
located upstream of the reactor.
NiO (s) + H2 (g) ----> Ni (s) + H2O (g)
The reduction of nickel oxide to nickel is thermally neutral - it does not generate heat
or absorb it. Water is produced in this reaction and is condensed by cooling the gas
stream to approximately 4C by using 20% ethylene glycol. The condensate is
removed from the system using a knockout pot. The dried gas has a residual water
level of 0.25 vol% and is recirculated over the catalyst.
3.0 Hot N2 Purge
After reduction, the catalyst is purged with nitrogen at 10C above the reduction
temperature (710C for the highest case) for 4 hours to remove any absorbed
hydrogen. Failure to do this will lead to a methanation reaction when CO 2 is
introduced at the next step. The catalyst bed is then cooled down to 90C in
recirculating nitrogen.
4.0 CO2 Stabilization
Nickel is much more stable as nickel oxide than it is as nickel, so it would therefore
rather undergo the oxidation back to nickel oxide.
Ni + O2 ----> NiO
The catalyst has to be stabilized to allow it to be removed from the reactor and packed
in drums for customers.

CO2 is bled into the system to give the appropriate CO 2/N2 atmosphere for a given
period of time to stabilise it, with the reactor bed maintained at a maximum temperature
of up to 155C, dependent on the recipe.
5.0 Air Stabilization
Once CO2 stabilisation is complete the bed is cooled. The monolayer formed by CO 2 is
not complete and some unreacted sites remain exposed which react with O2. In the
atmosphere of CO2/N2, process air is then slowly bled into the catalyst to stabilise any
remaining reactive sites on the catalyst. This is highly exothermic process and if not
carefully controlled will break up the CO 2 monolayer and lead to bulk oxidation and
associated temperature runaway.
During the air stabilisation the temperature is maintained around 30C. The length of
time the temperature is held is around 120 minutes but will be longer if there is a
temperature rise.
After the air stabilization process, O2 uptake tests are carried out for a number of times
depending upon catalyst grade. For this, the plant is kept in a boxed-up state and the
percentage decrease in oxygen level over a period of half an hour is measured. The
oxygen concentration in the subsequent steps is raised gradually from 0.1 mole % to a
maximum of 4 % depending on the catalyst grade. Finally air is introduced to bring the
oxygen level up to 20%. After acceptable levels are achieved, the catalyst is unloaded
from the reactor into drums.
6.0 Summary
The following are the typical steps carried out for the reduction of Nickel based catalyst:

1. Charge the catalyst into the reactor and box-up (manual operation).
2. Pressurise / depressurise the plant from 1.5 bara to 5 bara at ambient
temperature 4 times with nitrogen to drive out air in the plant.
3. Repeat the pressurisation / depressurisation steps with hydrogen.
4. Circulate the hydrogen while heating the reactor at up to 50C/hr to a maximum
temperature specified by the selected recipe (ramp rate TBC).

5. Pass hydrogen through the reactor at constant temperature for 6-8hrs depending
on recipe.
6. Repeat the pressurisation / depressurisation with nitrogen to drive out hydrogen
from the plant.
7. Pass the nitrogen through reactor for a 4 hour duration at a temperature 10 to
20C higher than reduction temperature. This N2 is vented to atmosphere.
8. Circulate the N2 to cool the reactor to maximum temperature of 90C.
9. Pass the CO2 into the reactor until a 50/50 mixture with N 2 is reached. Circulate
and reheat the reactor to 155C and hold at this temperature for a specified
number of hours.
10. Cool the reactor by circulating the gas.
11. Pass air into the system maintaining 0.1% O2 in the reactor inlet gas. Continue
this air stabilization until the reaction front passes down the reactor, then cool the
reactor to 30C.
12. Carry out the O2 uptakes according to the recipe.
13. Carry out an air purge to increase the O 2 level up to the air purge value
(approximately 20%).
14. Discharge the catalyst from the reactor (manual operation).