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Oper - Man - Unit 105 - Rev01

This 3-sentence summary provides the key details about the document: The document is an operating manual for carbon dioxide removal system 105 of the Sorfert ammonia plant 1, which contains sections that describe the fundamentals, utilities, start-up and operation, shut-down, checks, troubleshooting, and safety instructions for the system. The table of contents lists the sections and subsections that make up the operating manual. The document was revised on November 30, 2008 and approved for information purposes.

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0% found this document useful (0 votes)

302 views88 pages

Oper - Man - Unit 105 - Rev01

Uploaded by

Hadj Meknassi

We take content rights seriously. If you suspect this is your content, claim it here.

Available Formats

Download as DOC, PDF, TXT or read online on Scribd

You are on page 1/ 88

Code:

Sorfert
Operating Manual
UAN (for QMHA) pages total

11-3100 88

Part: II/1 Operating Manual Ammonia Plant 1

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5. System 105: Carbon dioxide removal

Table of Contents

Section 1
Fundamentals
Section 2
Utilities, auxiliary materials,
consumption figures
Section 3
Preparation of the system for start-up
Section 4
Start-up and operation of the system
Section 5
Shut-down of the system
Section 6
Operational checks
Section 7
Troubleshooting, Trip- and Interlock system
Section 8
Safety instructions

01 General Revision 30.11.08 Te 30.11.08 Sk 30.11.08 Te

00 First Issue 15.08.08 Te 15.08.08 RJ 15.08.08 Te 3
Rev Status Description Date Prepared Date Checked Date Approved AC
Status Code: Category Code (CC)
A-E According to Uhde’s 1 For Approval
Standard 2 For Information
Engineering 3 Not transmitted (internal)
Procedure
F For inquiry Acceptance Code (AC)
G For order placement 1 Approved / reviewed
H For Prefabrication 2 Appr./rev. as noted
J For Construction / 3 Not accepted, to be re-
Fabrication vised and resubmitted
K General issue
L Cancelled document

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Section 1
1 Fundamentals
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1.1 Process fundamentals

1.1.1 CO2 removal
1.1.2 Process condensate stripping
1.2 Process description
1.2.1 Gas route
1.2.2 MDEA solvent cycle
1.2.3 Carbon dioxide vapors
1.2.4 Process condensate
1.2.5 CO2 vapor condensate
1.2.6 Polished water
1.2.7 Boiler feed water
1.2.8 Auxiliary facilities

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1 Fundamentals
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1.1. Process fundamentals

1.1.1 CO2 removal

The CO2 is removed from the convert gas by BASF's activated MDEA-PROCESS.

The solvent used is an aqueous amine solution with an activator, MDEA being the active
component. The chemical formula is

CH2 - CH2OH
CH3 N (N-Methyldiethanolamine)
CH2 - CH2OH

The composition of the used activator is a proprietary of the licensor BASF.

The scrubbing solution contains about:

40 wt-% activated methyldiethanolamine (aMDEA)
60 wt-% water

The process is mainly characterized in that it combines the advantages of both a chemical and
a physical scrubbing solution. This results in low energy requirements for the regeneration of the
solvent and in extensive flexibility of the process.

Methyldiethanolamine (MDEA) is a non-corrosive tertiary amine. Consequently, the activated

MDEA solvent is not corrosive. Neither long time passivation of the system nor the addition of a
corrosion inhibitor is required.

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The CO2 is absorbed mainly according to the following reaction equations:

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CO2 + H2O  H2CO3

H2CO3 + R2 R'N  HCO3- R2R'NH+
where: R = CH2CH2OH and R' = CH3

The CO2 absorption is exothermic and reversible. Ease of solvent regeneration is based
especially on the reversibility of the bicarbonate formation. The bulk of the dissolved CO2 is
expelled by simple flashing of the solvent.

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1.2 Process description

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Flow-sheet No. 105-1/2/3

1.2.1 Gas route

The convert gas from the LT-conversion outlet 104E002 arrives the CO2-removal system at a
temperature of approx. 164 °C and a pressure of approx. 37.2 bar abs. Its heat is utilized in the
following three heat exchangers connected in series, LP-steam generator 105E001 for producing
LP-steam, reboiler 105E002 for generating the stripping steam required for regeneration of the
lean MDEA solvent and Demin Water Preheater 105E004 for preheating the deaerator feed
water. During this period the gas temperature is lowered to approx. 70 °C.

Prior to entrance of convert gas into absorber 105C001, condensate obtained is being separated
from the gas in separator 105F001.

The gas flows through the two-stage absorber 105C001 from bottom to top in countercurrent to
the scrubbing solvent. Most of the carbon dioxide is absorbed by the MDEA solvent in the lower
part of the absorber , while further removal of the carbon dioxide to the specified residual value
of 500 ppm v/v CO2 is performed in the upper part of the absorber 105C001. The gas leaves the
absorber at the inlet temperature of the lean solvent, i.e. at approx. 50 °C. Any droplets of the
solvent entrained in the gas are retained by two transfer trays to which BFW is admitted, and a
demister installed in the upper part of the absorber 105C001. Droplets carried out of absorber
during operational disturbances are separated from process gas in the separator 105F002.

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1.2.2 MDEA solvent cycle

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Regeneration of the rich MDEA solvent is effected in two steps. The CO2-enriched solvent, which
has a temperature of approx. 85 °C, is fed from the bottom of absorber 105C001 via hydraulic
turbine 105MT01 to HP-Flash Vessel 105C002, where it is expanded to approx. 6.6 bar abs.
During this process, mainly the dissolved inert gases (H2, N2, CH4 and CO) are liberated. These
inert gases are then fed into the fuel gas system of primary reformer 103B001. Condensate
scrubbing trays arranged in the head of the HP-Flash vessel minimizes the solvent losses. Via
separator 105F004 the inert gases are fed to the primary reformer. If required, this flash gas can
also be burnt in flare 106V801.

During the second step, the flashed MDEA solvent is expanded to approx1.6 bar abs into the
LP-Flash Vessel 105C003. In the LP-Flash Vessel, the MDEA solvent is heated in
countercurrent with overhead gas/steam from the stripper 105C004. About half of the CO2 is
expelled during this process.

After leaving the bottom of the LP-Flash Vessel, the semi lean solvent, which has thus been
regenerated, is split into two streams. Without any further cooling, the major part-stream, i.e.
approx. 82 %, is fed to the middle of absorber 105C001 at a temperature of approx. 75 °C by
means of semi-lean solvent pump 105P001A/B. Pump 105P001A is coupled with hydraulic
turbine 105MT01 and an electric motor. Pump 105P001B is only driven by an electric motor.

The remaining part-stream, i.e. approx. 18 %, is fed by means of stripper feed pumps
105P002A/B via lean/semilean solvent heat exchanger 105E005, and preheating to approx. 94
°C, to the head of the stripper 105C004.

In the stripper, the semi lean solvent is stripped in countercurrent with steam, which is generated
in reboiler 105E002. In this manner, most of the CO2 is removed from the solvent.
The regenerated lean MDEA solvent leaves the stripper bottom at approx. 119 °C via a Filter
105F008 A or B and is cooled to approx. 85 °C in lean/rich solvent heat exchanger 105E005.
Thereafter, the lean MDEA solvent is cooled to 50°C in solvent cooler 105E003 and fed by
means of lean solvent pump 105P003A/B to the head of absorber 105C001.
The lean MDEA and the semi lean MDEA streams to the absorber are distributed evenly, by
means of distribution trays, over the cross sectional area.

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In hydraulic turbine 105MT01 part of the pump energy is recovered. The hydraulic turbine
105MT01 is connected to the semi lean solvent pump 105P001A. The missing energy is effected
by an electric motor. All other pumps are driven by electric motors only.
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1.2.3 Carbon dioxide vapors

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The CO2 vapors from the head of stripper 105C004 are fed into the bottom of the LP-Flash
Vessel 105C003 where they are used for heating up the MDEA solvent, resulting in a better
performance of the low pressure flash.

The carbon dioxide/water vapor mixture, having passed through two transfer trays to which
condensate is admitted and through a demister for removing of entrained solvent droplets,
leaves the LP-Flash Vessel 105C003 at a temperature of approx. 74 °C and a pressure of
approx. 1.6 bar abs.

The stream is routed via the CO2 cooler 105E006A/B/C/D/E where the temperature is reduced to
approx. 40 °C using cooling water.

Condensate obtained in 105E006A/B/C/D/E is separated from the carbon dioxide gas in

separator 105F003. Most of the CO2 gas from 105F003 will be sent to the CO2-compressor
020K002 via separator 020F001, the surplus CO2 will be discharged into the atmosphere via a
pressure control valve.

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1.2.4 Process condensate

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The condensate obtained when cooling the process gas in LP-steam generator 105E001,
reboiler 105E002 and Demin Water Preheater 105E004 is separated from the gas in separator
105F001.

The condensate obtained in separator 105F001 containing impurities (Methanol, Ammonia and
dissolved CO2) is discharged by stripper feed pump 180P001A/B to the condensate stripper
180C001 via condensate preheater 180E001.

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1.2.5 CO2 vapor condensate

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The condensate obtained is separated from the CO2-gas in separator 105F003.

From the separator the condensate is discharged with a temperature of 40 °C by the reflux pump
105P006A/B to several users. The major part of the condensate approx. 9 m3/h is fed to the
transfer trays (2 bubble cap) at the top of the LP-Flash Vessel 105C003.

A small stream of the condensate about 1 m3/h is used as wash water on the transfer trays
(bubble cap trays) at top of the HP-flash vessel 105C002.

CO2 condensate from separator 105F003 will be used intermittent as flushing liquid for the
MDEA-filters 105F006A/B and 105F007A/B.

In order to maintain the water balance of the MDEA system it is possible to withdraw condensate
from 105F003.

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1.2.6 Polished water

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Excess heat of the CO2 removal system is used to preheat Polished feed water to deaerator
from 40 °C to 90 °C in the Demin Water Preheater 105E004. This preheater 105E004 is the gas
route between reboiler 105E002 and separator 105F001.

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1.2.7 Boiler feed water

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A small stream approx. 1.0 m3/h of MP-boiler feed water is used on the two wash trays in the top
of absorber 105C001 to minimize the solvent entrainment in the process gas and maintain the
water balance of the CO2 removal system.

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1.2.8 Auxiliary facilities

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Make-up and slop drum 105D001

Any solvent leakage is being collected in the slop drum 105D001 arranged in the ground below
plant level.

MDEA filter 105F005

A part-stream of approx. 50 m3/h MDEA solvent is continuously recirculated via MDEA filter
105F005 to prevent an enrichment of impurities in the solvent. The part-stream is withdrawn on
the discharge side of stripper feed pump 105P002A/B, fed via the filter and returned to the
suction side of the pump.

Solvent storage tank 105T001

Solvent storage tank 105T001 with a capacity of 833 m³ is dimensioned to receive the entire
volume of solvent which is present in the system. Consequently, the system can be drained for
maintenance work. The system is filled with solvent by means of slop pump 105P004 via slop
drum 105D001. The storage tank is nitrogen-blanketed.

Filter 105F006A/B and 105F007A/B

Lean MDEA solvent of approx. 2.3 m3/h is continuously circulated via filter 105F006A/B and
105F007A/B and used for flushing of mechanical seals, etc. on pumps 105P001A/B,
105P002A/B, 105P003A/B and hydraulic turbine 105MT01.

Antifoam dosing station 105U300

In the event of foaming of MDEA solvent antifoam agent should be fed to the suction side of
semi lean solvent pump 105P001A or 105P001B, to the suction side of lean solvent pump
105P003A or 105P003B and to the discharge side of hydraulic turbine 105MT01 via a small
MDEA loop from the discharge side of lean solvent pump 105P003A/B to the above mentioned
locations for good antifoam agent distribution with the MDEA solvent.

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Section 2
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2 Utilities, auxiliary materials, consumption figures

2.1 Utilities (continuous operation)
2.1.1 Electric power
2.1.2 Cooling water
2.1.3 Instrument air
2.1.4 Boiler feedwater
2.2 Utilities (intermittent operation)
2.2.1 Steam
2.2.2 Nitrogen
2.2.3 Water
2.3 Auxiliary materials
2.3.1 Methyldiethanolamine
2.3.2 Piperazine
2.3.3 Anti foam agent
2.4 Consumption figures

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2 Utilities, auxiliary materials, consumption figures

2.1 Utilities (continuous operation)
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2.1.1 Electric power

For heating, lighting and instruments.
See part I, section 1.

2.1.2 Cooling water

See part I, section 1.

2.1.3 Instrument air

For measuring and control instruments according to the current requirements, pressurized air will
be used.
See part I

2.1.4 Boiler feed water

Boiler feed water is required for keeping the water balance constant during the operation of the
system.

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2.2 Utilities (intermittent operation)

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2.2.1 Steam

Low-pressure steam is required for heating the stripper 105C004 during start up.
Pressure : 5.5 bara abs.
Temperature : 170 °C

2.2.2 Nitrogen

Nitrogen for purging the system and blanketing of the solvent storage tank and the slop and
make-up drum will be available from the inert gas system. See part I, section 1.

2.2.3 Polished Water

Polished water will be used for solvent make-up and for filling of separator 105F003, if necessary
for start up of the reflux pumps.
temperature: 130 °C
pressure: approx. 2.3 bar abs.

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2.3 Auxiliary materials

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Leakage fluids from pumps and fluids drained from machinery, equipment and piping are sent to
the slop piping system, collected in slop and make-up drum 105D001 and returned to the plant.
The quantity of MDEA entrainment leaving the absorber 105C001 and the LP-flash vessel
105C003 with the gas is minimized by the equipment design.

Therefore, the loss of chemicals will be very small and will essentially depend on the mechanical
state of the plant. However, keeping a certain stock of chemicals is required in any case.

The owner of the plant should check the quantities specified below and then determine the
holdings.

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2.3.1 activated Methyldiethanolamine

Analysis:
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aMDEA min. 96.0 wt-%

Water max. 4.0 wt-%

In water insoluble substances max. 0.03 wt-%.

No other impurities detectable.

Characteristics:
Color colorless - yellow
Boiling point >100°C
Melting point < -10°C
Density at 20 °C 1040 to 1050 kg/m3
Viscosity at 25 °C 88.6 mPas
Flash point (DIN 51758) >100 °C
Ignition temperature >200 °C
Quantity:
For the initial charge of the system approx. 300 t
consumption per year 10 - 20 t
Delivery:
Initial charge in tank container 19.5 t

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2.3.2 Antifoam agent

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
As antifoam agent AMEREL 1500 foam control agent is used.
Specification Limits
Appearance opaque, off-white liquid
Viscosity approx 1500 mPas at 25°C
Freezing point < 0 °C
Boiling point > 250 °C
Flash point > 250 °C
Density 1030 kg/m3
Vapor pressure 6.66 mbar at 20 °C

Quantity:
For initial charge of the system 20 kg
For consumption of the system 280 kg
Delivery: PE drums

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2.3.3 Caustic Soda

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Analysis: Total alkalinity 30% as NaOH

Quantity: approx. 67 t

NaOH will be used in the initial washing procedure

Delivery

By truck

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2.4 Consumption figures

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The expected consumption figures are as follows:

Case A Case B

Electric power 2614 4498 kWh/h

Cooling water 2451 2451 t/h
Boiler feed 0.67 0.67 t/h

Chemicals:
activated MDEA (aMDEA) appr. 10-20 t/year
Amerel 1500 appr. 0.3 t/year

Case A: Hydraulic turbine 105MT01 in operation

Case B: Operation without hydraulic turbine

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Section 3
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3. Preparation of the system for start-up

3.1 General notes
3.1.1 Checking the system after erection
3.1.1.1 Process checks
3.1.1.2 Mechanical checks
3.1.2 Cleaning of the system by purging, flushing etc.
3.1.3 Pressure tests of the equipment
3.1.4 Tightness tests of the equipment
3.1.5 Start-up of the cooling water system
3.1.6 Start-up of centrifugal pumps
3.1.7 Start-up of piston pumps
3.2 Special preparatory work
3.2.1 Mechanical cleaning of equipment and piping
3.2.2 Filling HP-flash vessel, LP-flash vessel and absorber with packing material
3.2.3 Water test for transfer tray
3.2.4 Chemical cleaning of equipment and piping
3.2.5 Start-up and operation of the liquid cycle

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3. Preparation of the system for start-up

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3.1 General notes

The information contained in paragraphs 3.1 to 3.1.4 generally applies to all plant sections. For
this reason, the information is given only once in the Operating Manual in Part I, section 2.

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3.2 Special preparatory work

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3.2.1 Mechanical cleaning of equipment and piping

The carbon dioxide scrubbing system operates according to BASF's activated MDEA process.
Careful cleaning of the system prior to start-up is extremely important.

Independent of the general instructions under 3.1.2, all equipment and piping coming into
contact with solvent must therefore be carefully cleaned on the inside. Mechanical cleaning of
the piping is effected by knocking prior to insulation and the equipment is cleaned by rubbing
with wire brushes in order to remove any coarse impurities or rust which is peeling off or with
other more effective cleaning procedures.

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3.2.2 Filling HP-flash vessel, LP-flash vessel and absorber with packing material
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The required dimensions of the packing material and the max. permissible tolerances are
specified in the specifications of the
105C001 Absorber,
105C002 HP-flash vessel
105C003 LP-flash vessel
105C004 Stripper.

A sample of the packing material is to be kept for checking or comparison purposes.

Adequate facilities for transporting the packing material are to be made available. The packing
material is to be handled with care during unloading and storage. It must not be dropped or set
down forcefully.

Packing materials may never be placed into the column in their transport containers, in which
they arrive at the job site. The packing material transport sacks may also be used if there is no
other possibility. But in this case, it must be completely ensured by means of a suitable control
system that none sack remains in the columns.

Personnel working inside the equipment must wear dust masks for their protection. Damage to
material already filled in is to be avoided by using running boards of more than 0.6 m2 and soft
foot-wear.

The following instructions are to be observed for filling the packing material:
a) The columns must be clean.

b) It has to be checked whether the supporting grids are installed and fixed as specified.

c) It has to be marked on the columns circumference the filling height by measuring from the
support grid.

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d) Attention: The packing in the bottom sump of absorber 105C001 and HP-flash vessel
105C002 must be chemical cleaned outside of the column and shall be filled in when the
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chemical cleaning of the whole system is finished before MDEA solvent is filled in.

e) The filling operation is to be carried out symmetrically over the entire equipment cross
section. The free fall of the packing material should by no means exceed 1 m as long as
the packing height is below a half meter. When the packing height of a half meter is
reached the free fall of the packing material should by no means exceed 5 m. The
manholes are more than 5 m above the support grids, so that a chute and a heavy plastic
sock are necessary to avoid the deformation of packing elements by free fall. Care has to
be taken to prevent the formation of cavities in the packing material layer since they would
cause irregular gas velocities or adversely influence the liquid distribution. This shall be
avoided by moving the plastic sock to several points periodically and a cone of max. 30°
on the packing area.

The depth of each layer is to be measured and the measurements are to be entered into
the equipment drawings; the same applies to the position of the measuring nozzles, e.g.
analyzer sampling points, pressure measurements, thermowells.
In the columns, the structure of the layer, the dimensions of the packing material and the
working procedure employed by the personnel are to be checked from time to time.

f) After filling the packing material it must be ensured that the surface is equalized across
the column area. It is not absolute necessary to fill the packing material to or above the
marking.

Furthermore the remaining components, distribution and redistribution trays, transfer

trays, demister and the column sumps are to be checked with regard to the
manufacturer's drawings.

g) The work performed is recorded in a report.

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3.2.3 Water test for transfer tray

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In order to ensure trouble-free operation of the carbon dioxide scrubbing system, it is mandatory
that all transfer and distribution trays in absorbers, flash vessels and stripper have been installed
in horizontal position and that the gaskets as far as necessary, between transfer tray plates and
supports are put in.

The work has been completed according to 3.2.2. A water test can be carried out on the bubble
cap trays in the absorber and LP-flash vessel only.

The transfer trays of the absorber and the LP-flash vessel are to be checked by means of boiler
feed water or Polished water whether the trays are horizontal and the gaskets are tight.

Each transfer tray has a manway to be opened from above and below. In order to maintain the
proper horizontal position of the transfer trays, the distributor tray below should be checked and
adjusted first. The next tray to be checked and adjusted is the lower transfer tray. Finally the
upper transfer tray will be checked and adjusted. Each tray should show an uniform water
distribution, indicated by the measurement of the water level on the tray.

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3.2.4 Chemical cleaning of equipment and piping

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Mechanical cleaning of the plant is followed by chemical cleaning which is combined with the
start-up of liquid cycles, to be carried out according to 3.2.5. The work according to 3.2.1, 3.2.2
and partly 3.2.3 has been completed. For operation of the liquid cycles the CO2-removal system
must be pressurized by means of a suitable gas, e.g. nitrogen, natural gas containing less than
0.5 ppm sulfur or compressed air (for flushing with water only).
Usually, nitrogen under sufficient pressure is available from the network.
Basically, chemical cleaning is performed in four steps.

1st Step: Cleaning and water flush

The cleaning and water flush is used to remove grease from packing, trays and supports as well
as coarse grime which may have been introduced during construction.
 open manholes and bottom drains of the column and tanks
 remove orifice meters in the liquid lines and close the taps in the impulse pressure line
connections beforehand
 flush the equipment with water using firehoses, if possible
 it may be expedient to clean out pipelines section wise in the same manner

Preparation for flushing by circulation

 Close manholes drains and vents. Isolate the CO2-removal system properly from other
systems.
 Install strainers on the suction side of the pumps.
 Check operation of all remote-controlled actuators and control valves.
 Check operation of all equipment activated by the safety shutdown system (simulate
shutdown conditions).
 Purge the system free of oxygen and perform a leak test by pressurizing the system to
approx. 4.0 bar abs with nitrogen. Check the flanges and cover seals on the columns and
vessels which were opened for the water flush for gas-tightness using a suitable indicator
(e.g. NEKAL solution).
 Water, free of deposits and chlorine, is pumped into the system and a pH value of approx. 7.5
is set by adding NaOH. Approx. 100 to 150 mg/l of water are required for this purpose.
Simultaneously the level indicators are to be checked.
 Increase the absorber pressure to approx. 15.0 bar g, if possible.
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Copyright 2008 Uhde GmbH
SO-UD-M801.00006 01
Code:
Sorfert
Operating Manual
UAN (for QMHA) Page:

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Flushing by circulation
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The pumps have to be put in operation according to the vendor's instructions. Additionally refer
to 3.2.5, start up and operation of the liquid cycle. During cleaning of the system carefully,
monitoring of the circulation rate by notifying the ampere capacity on the ampere-meter and
the pressure at pump suction is imperative as solids flushed from the system may block the
suction strainers.

In order to remove dirt and solids from the system, it is recommended to replace as much of the
liquid volume as possible by fresh water in a short time. The drained water has to be replaced by
nitrogen in order to prevent vacuum in the columns and piping (LP-flash vessel and stripper).
Care has to be taken, that liquid levels required for the circulation pump operation is sufficient. If
the liquid level becomes to low for the pumps, the pumps have to be shut-down and restarted if
the level is back (after refilling with fresh water). Removing the dirt and solids in this way, is more
effective than having a continuous withdrawn of water and replacing by new water.

When the water remains clear and solids can hardly be detected, the flushing operation is
completed. Towards the end of the flushing operation, the temperature should be increased to
approx. 70 °C by adding steam via line SL21-105333-4" (PID105-1) to stripper 105C004.

2nd Step: Flushing with 3 % (w/w) NaOH solution

The next step comprises flushing with a solution containing approx. 30 g/l NaOH. Prepare the
solution from Polished water and NaOH in the slop drum 105D001. Introduce the solution into
the system at the bottom of LP-flash vessel 105C004 by means of slop pump 105P004.

The pressure of the absorber is kept constant at approx. 15.0 bar g; the pressure of the HP-flash
vessel 105C002 is about 5.0 bar g maintained by PIC 105006B venting gas to the flare stack
106V801. The pressure within the LP-flash vessel should be in the range of 1.0 to 3.0 bar g and
is maintained by pressure controller PIC 105016 in the CO2-offgas line to atmosphere.

Circulate the solution through the system for more than 8 hours at a temperature of 70 to 80 °C
using pumps 105P002A/B, 105P003A/B and 105P001A/B. For this purpose the pumps have to

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put in operation according to the vendor's instructions. The pH value must be at least 10. The
following analyses are to be made during the circulation:
1. Foaming test
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2. Permanganate consumption (organic comp.)

3. Iron content

If the pH value decreases and strong foaming occurs, part of the solution is to be removed and
replaced by fresh solution. After at min. 5 hours the flushing operation is completed when all
values remain constant. The solution is then gradually diluted with water and the excess solution
thus formed is bled off from the system and simultaneously used for flushing of slop drum
105D001. Empty the entire system. Take liquid samples. Check strainers in the pump suction
lines.

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3rd Step: Neutralization by Polished water flush

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The plant is refilled with Polished water which is circulated until foam no longer forms and no
permanganate consumption occurs. The water should be heated up initially to about 70 °C. All
flushing operations should be carried out at the highest possible circulation rate, the system
pressure shall be as mentioned above. After flushing the system for at least 5 hours the water is
drained. Water and suction strainers are to be checked for dirt.

4th Step: Flushing by Polished water

Install the carefully cleaned additional packing for the bottom section (vortex breaking packing)
into the bottom of the absorber 105C001 and HP flash vessel 105C002.
The fourth step of cleaning the entire system is carried out by polished water cycle. To
accomplish this step, the plant should be filled with Polished water via line WL21-105154-3" to
separator 105F003 and pumped by reflux pump 105P006A/B to the top of LP- and HP-flash
vessel.
Reinstall orifice meters and carry out the circulation of Polished water as described for the
caustic solution below 2nd step.
This Polished water will be circulated through the entire system for min. 6 hours, and the
temperature of the Polished water is simultaneously to be raised to the operating temperature of
approx. 115 °C at the bottom of stripper 105C004 (TI 105012).
The Polished water flush should be carried out at the highest possible circulation rates. After
min. 6 hours the Polished water is to be cooled down.
In order to finalize this step, the complete system is to be emptied.

Take a liquid sample from the water and add about the same volume of MDEA to the sample.
Check this diluted amine solution for foaming activity ( see Part VII Analytical Manual). If foaming
activity exceeds guidelines repeat flushing with fresh 3 % (by weight) NaOH solution followed by
the two flushing steps with Polished water.
The suction strainers of the solvent pumps to be checked again.

Each flushing step is to be recorded in a report.

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These four flushing operations will take about 1 week. The quantities of auxiliary materials
required are:
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approx. 67000 kg 30% NaOH

approx. 900 m3 Polished water
approx. 1200 m3 water, free of deposits, chlorine-free (Polished water)
approx. 5000 kg/h 5.5 bar steam for heating purposes

After completion of the flushing operations, the pumps are to be shut down, the plant is to be
drained completely and the strainers of the pumps are to be cleaned. Subsequently, column
sumps and distribution trays must be checked and, if necessary, cleaned. Then, all drains are to
be closed. The entire plant must remain filled with nitrogen and the operating solvent should be
pumped by means of 105P004 via slop drum105D001 from solvent storage tank 105T001 into
LP-flash vessel 105C003.

Solvent level within stripper 105C004 is to be built up by means of 105P002A or B stripper feed
pump. The absorber 105C001is filled with 105P003A or B lean solvent pump.
Attention: After chemical cleaning remove the strainer in the inlet line to hydraulic turbine
105MT01.

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3.2.5 Start-up and operation of the liquid cycle

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The purpose of test period of the liquid cycle is to ensure trouble-free operation when the system
is later put into operation. The conditions of the test period should as far as possible be
analogous to the future operating conditions.
The test period is also used for personnel training.

Furthermore, the respective piping is additionally cleaned during the start-up period. Therefore,
the pumps must be equipped with strainers on the suction side, that will retain the dirt particles.
The intake pressure of the pumps shall be measured between suction nozzle and strainer.
Frequent checks are necessary.

All pertaining measuring instruments are to be operated during this test period.

As long as there is still any danger of contamination, all orifice plates are to be either by-passed
or removed and replaced by dummies; the connections for instruments are to be cleaned by
flushing.

The quantity of liquid required is to be made available. The quantity has to be such that the rated
discharge of the pumps can be delivered in continuous operation at normal liquid level in the
equipment. The absorber 105C001 from which the liquid is transferred to the HP-flash vessel
105C002 by the pressure in the plant, must be put under sufficient pressure 15.0 to 25.0 bar by
means of a suitable gas (refer to 3.2.4). The HP-flash vessel 105C002 must be put under 5.0
bar nitrogen pressure via line NI20-105302-1" (PID 105-5) in order to transfer the liquid to LP-
flash vessel 105C003.

However, the pressure shall be lower than the working pressure because after start-up of the
solvent pumps the pressure increases due to the liquid volume fed into the absorber.
The supply of utilities - electric power, water, steam instrument air, etc. - is to be checked.
Operating and stand-by pumps are to be prepared for start-up. During the test period, pumps are
operated alternately.

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Mechanical seals of semi lean solvent pump 105P001A/B, stripper feed pump 105P002A/B and
lean solvent pump 105P003A/B must be flushed during operation. Under steady operating
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conditions this is performed by MDEA solvent withdrawn from the discharge side of lean solvent
pump 105P003A/B. In this case the solvent is cleaned by filters 105F006A/105F0007A resp.
105F006B/105F007B and distributed to the mechanical seals of pumps 105P001A/B,
105P002A/B, 105P003A/B and 105MT01.
Stripper feed pump 105P002A/B and lean solvent pump 105P003A/B are equipped with
cyclones enabling start up of these pumps without external supply of liquid for flushing the
mechanical seals. Therefore a small sidestream is withdrawn from the pump discharge, released
from solid particles within the cyclone and fed to the mechanical seal of the respective pump. As
soon as lean solvent pump 105P003A/B is started up, the liquid for flushing of the mechanical
seals shall be taken from filters 105F006/105F007 as mentioned above.

The pumps are started according to 3.1.6 and 3.1.7. In addition, points 4.2.1, 4.2.5, 4.2.6 and
4.2.7 must be observed for start-up of the solvent pumps.

First a liquid stream is fed to the LP-flash vessel 105C003 by means of slop pump 105P004 until
the highest level (LI 105010A/B) has been reached. LP-flash vessel 105C003 serves as the
pump suction for semi lean solvent pump 105P001A/B and stripper feed pump 105P002A/B. By
means of 105P002A or B a small quantity of liquid is now pumped into the stripper 105C004,
until the highest level (LIC 105014) is been observed. Reboiler 105E002 (shellside) is filled
simultaneously. High points in the solvent system to lean solvent pumps shall be vented.
A small liquid stream is now fed to absorber 105C001 by means of lean solvent pump 105P003A
or B, until the highest level (LIC 105004) has been reached.

Absorber 105C001 is pressurized to 15.0 to 25.0 bar. HP-flash vessel 105C002 is now filled by
opening bypass around quick-acting valve XV 105001 and expansion valve LV 105004B. The
pressure within 105C002 will be controlled by venting through PV 105006B to flare 106V801.
Stop lean solvent pump 105P003A/B if the level in the stripper is lost.
The lean solvent liquid cycle is now closed by opening LV 105009A/B, thus feeding liquid from
HP-flash vessel 105C002 to LP-flash vessel 105C003. Now open the quick acting valve XV
105001 and close the bypass.

As soon as the levels in the columns have been stabilized, the semi lean solvent cycle may be
started by means of start-up semi lean solvent pump 105P001B.

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The measuring instruments and controllers of the cycle are successively put into operation and
local and remote readings are compared.
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As soon as the instruments operate satisfactorily, the liquid flow rate may be increased
gradually. After each step wait until the entire cycle has adjusted itself to the higher flow rate.
During this period the response of the controllers and indicators as well as the position of the
control valves must be observed.

Tall packed columns require a relatively long period until the higher flow rate can be detected by
opening the outlet valve.

After each increase of the liquid flow-rate, the electric power consumption of the pump motors is
to be measured. The motor load must not exceed the rated capacity stated on the rating plate.

If the suction pressure of the semi lean solvent pump 105P001B drops while the level in the LP-
flash vessel 105C003 remains unchanged and the flow rate is constant, the 105P001A is started
and the former shut down (standard value for pressure loss in strainer approx. 2.0 bar).
Hydraulic turbine 105MT01 may be started too. The suction strainer must be removed and
cleaned. Then the pump is to be made ready for operation again.

In equipment filled with gas the pressure decreases during the test period due to the liquid-
solubility of the gas and must, therefore, be increased to approx. 15.0 to 25.0 bar in absorber
105C001.

During the further course of the test period, the flow rate of the liquid is to be increased and
decreased at irregular intervals until trouble-free functioning of the cycle with the measuring and
control instruments installed is ensured.

Alarms, trip valves or safety and change-over valves are to be checked operationally, i.e. by
changing the response conditions. The same applies to electrical interlocks.

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Section 4
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4. Start-up and operation of the system

4.1 Preparation of the operating solvent
4.2 Initial start-up of the system
4.2.1 Filling the system with operating solvent
and start of the solvent cycle
4.2.2 Operation of the carbon dioxide scrubbing system while circulating
the nitrogen and steam feeding in the primary system
4.2.3 Heating the solvent cycle
4.2.4 Passivation of the System
4.2.5 Gas feed to absorber 105C001
4.2.6 MDEA solvent concentration for operation
4.2.7 Operation of the semi lean solvent pump 105P001A/B
4.2.8 Operation of the lean solvent pump 105P003A/B
4.2.9 Operation of the stripper feed pump 105P002A/B
4.2.10 Operation of the LP Steam generator 105E001
4.2.11 Operation of the Polished water preheating
4.2.12 Operation of process condensate system
4.2.13 Operation of the CO2 vapor steam condensate system
4.2.14 Addition of antifoam agent
4.2.15 Operation of slop drum 105D001
4.2.16 Operation of MDEA_filter 105F005
4.2.17 Operation at partial load

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4. Start-up and operation of the system

Normally, the plant shall be operating with as many controllers in automatic mode. If a critical
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operating parameter is off its normal value an alarm is given in the DCS to alert the operator.
This alarm is not to be seen as an information only but it is a request for corrective action to be
taken by the operator. It can be a hint for a malfunction of a controller or an irregularity in the
process. The reason for the alarm has to be identified and rectified. If the process parameters
can not be brought back to their normal values it has to be checked whether the process can be
continued with the parameter being in the alarm range. Otherwise the unit has to be shut down.
If the amount of incoming alarms does not permit such evaluation the operator also has to shut
down the respective unit for reasons of safety.

4.1 Preparation of the operating solvent

The operating solvent contains:

40.0 % by weight activated methyldiethanolamine

60.0 % by weight water

For filling the system, appr. 685 m3 resp. 698 t of solvent are required.
That is appr. 280 t activated MDEA
appr. 418 t Polished water

The MDEA will be supplied as a premix in ISO-tank containers. The containers will be emptied
into the slop drum 105D001 where the Polished water will be added. After mixing by using the
slop pump 105P004 and the return line MS34-105236-2" (PID 105-8) the solvent is pumped into
the solvent storage tank 105T501 via line MS34-105233-2" (PID 105-8) and MS34-105234-
2"(PID 105-8). Since the slop drum contains approx. 39 m³ solvent, charges of about 32 m³ can
be prepared. The charges are to be prepared with approx. double concentration so that the
content of one MDEA container (19,5 t) is diluted with approx. 12.5 t of Polished water. The
correct operating concentration of the solvent can be adjusted during start up of the system.

The aMDEA Premix is very viscous at low temperature. When ambient temperature is low it
might have to be preheated before charging it to the system. Make sure to empty the containers
or drums completely, i.e. without leaving any possibly-precipitated activators behind.

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An initial charge of antifoam agent, should be added to the system after the circulating solvent
is heated up, approximately one or two hours before gas shall be charged to the system. The
concentration of antifoam should be approx. 50 ppm (wt.), i.e. per 100 m3 of solvent, 5 l of
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antifoam agent should be added, that means approx. 30 -35 l of AMAREL 1500.

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4.2 Initial start-up of the system

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4.2.1 Filling the system with operating solvent and start of the solvent cycle

The plant must have been cleaned according to 3.2.1 and 3.2.4 and stays nitrogen-blanketed. All
equipment, valves, machinery, and instruments must be ready for operation. The operating
solvent required is ready in MDEA storage tank 105T001. The product gas route must be shut
off at the inlet and outlet of the system. All inlets and outlets are to be closed. For filling the plant
with operating solvent, 15.0 to 25.0 bar pressure has to be maintained in absorber 105C001 by
means of which the operating solvent can be forced to the top of HP-flash vessel 105C002. For
this purpose the manual block valve in the gas inlet upstream of the absorber as well as the
outlet XV 106001 must also be closed. All control- and block valves at inlets and outlets of the
absorber must be closed. Then the absorber system pressure is increased by means of a
suitable gas (refer to 3.2.4) to approx. 15.0 to 25.0 bar.

The HP-flash vessel 105C002 is pressurized by means of nitrogen to approx. 6.0 bar, via line
NI20-105302-1" (PID 105-5) which is connected to the gas outlet of the HP-flash vessel
downstream of 105F004.

The pressure within the CO2 system is maintained via PV 105016A in line CD21-105108-16"
(PID 105-7) to the atmosphere, the shut-off valve in line CD21-105103-40" (PID 020-1) is
closed.

Prior to filling, a solvent sample is to be taken from solvent storage tank 105T001 and checked
for deposits.

The operating solvent is pumped from the solvent storage tank to the bottom of LP-flash vessel
105C003 by means of slop pump 105P005 via slop tank 105D001. The bottom of LP-flash
vessel 105C003 is filled to max. level LIXH 105010A. The LP-flash vessel bottom may be
flooded to provide sufficient liquid for semi lean solvent pump 105P001A/B and stripper feed
pump 105P002A/B.

Parallel to this procedure, stripper feed pump 105P002A/B and lean solvent pump 105P003A/B
are to be made ready for operation. Instruction of the pump manufacturer are to be followed.

The stripper feed pump 105P002A or B shall be started at first.

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Initially sealing medium for the mechanical seals of stripper feed pump 105P002A/B and lean
solvent pump 105P003A/B will be supplied from the respective pump discharge via a cyclone to
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the mechanical seals .

105P002A/B Stripper feed pump

The stripper feed pump is provided with a minimum flow non return valve. The block valves in
the min. flow lines of 105P002A and 105P002B MS28-105277-6” (PID 105-5) are to be opened.
The intake block valves of stripper feed pumps 105P002A/B are to be opened and the pump
casings are to be vented thoroughly.
The discharge block valves of 105P002A/B will be opened next, thus filling the line MS32-
105220-16" (PID 105-1), the lean/semilean solvent exchanger 105E005 as well as line MS33-
105221-16" (PID 105-1) up to the control valve LV 105014. Simultaneously the line MS32-
105237-4" (PID 105-6) feeding the MDEA-filters 105F005 is filled. These discharge lines are to
be vented too.

After start up of stripper feed pump 105P002A or B the upper sump of the stripper 105C004 is
filled via LIC 105014. Simultaneous the reboiler 105E002 (shellside) is filled. The reboiler
105E002 and the lower sump of stripper 105C004 fills up via MS20-105222-20" (PID 105-1) and
MS20-105223-20" (PID 105-1).

LIC 105014 should be operated in such a manner that the level in LP-flash vessel 105C003 will
not drop below minimum.

As soon as the level in the lower sump of 105C004 builds up, the Filter 105F008AB, the
lean/semilean solvent exchanger 105E005 and the solvent cooler 105E003 is filled via lines
MS20-105902-16" (PID 105-1 & 8) MS20-105224-16" (PID 105-1 &8) and line MS21-105225-
16" (PID 105-1) and subsequently the suction of lean solvent pump 105P003A/B is filled via line
MS22-105226-16" (PID 105-1 & 2) up to the suction block valves.
The system described above is provided with suitable vents which have to be operated prior to
each start up of lean solvent pump 105P003A/B.

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105P003A/B Lean solvent pump

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The next step in starting up the liquid cycle is to commission the lean solvent pump 105P003A
and B. Both suction block valves are to be opened, and the pump casings to be vented carefully.
The pump discharge line up to the flow control valve FV 105002 shall be filled and vented by
opening XV 105005 resp. XV 105006. As this valves are kept closed by trip functions (trip
105.7 / trip 105.8) an override switch is provided. As long as the override is activated it's
recommended to keep the manual block valve downstream of control valve FV 105002 closed.
Prior to start up of lean solvent pumps 105P003A/B the override must be removed.
10 seconds after start of the lean solvent pump 105P003A or B, discharge valve XV 105005
resp. XV 105006 opens automatically. Since this set of pumps is not provided with a minimum
flow device, a flow of at least 150 m3/h shall be adjusted as soon as possible while opening FV
105002. The lean solvent pump 105P003A/B is tripped automatically after 3 minutes if the flow
at FI 105002 is not above 120 m3/h.

The MDEA solvent flow to absorber 105C001 is now to be controlled by FV 105002. If the level
in LP-flash vessel 105C003 and stripper 105C004 cannot be maintained the lean solvent pump
must be switched off, stripper 105C004 refilled and the pump 105P003A or B restarted.

In the event of suction pressure failure the pump is to be shut-down immediately to avoid
damage to the machinery.

As soon as the level in the bottom of absorber 105C001 is above the switchpoint acting on trip
E1, level controller LIC 105004 is to be prepared and the bypass around shut off valve XV
105001 to be opened. First, the bypass LV 105004B of hydraulic turbine 105MT01 is used. Line
MS26-105209-28" (105-3) is filled up to LV 105004B by opening the upstream gate valve slightly
and the 1"-vent upstream of LV 105004B. The gate valve downstream of LV 105004B is to be
opened. Then the upstream gate valve shall be opened fully and last at least the LV 105004B
slightly.

Level controller LIC 105004 is to be put into operation, and the operating solvent is sent to the
top of HP-flash vessel 105C002. As soon as the bottom level of HP-flash vessel 105C002 rises,
LIC 105009 is used to feed MDEA solvent to top of LP-flash vessel 105C003 by gradually
opening. The lean solvent cycle is now closed. Open the shut off valve XV 105001 and close its
bypass

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Increase the flow through FV 105002 to approx. 300 m3/h.

Prepare filters 105F006A/B and 105F007A/B, check all strainers in sealing medium lines to
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each pump, flush and vent the lines. Now the supply of sealing medium to the pumps
105P002A/B and 105P003A/B shall be changed from "self sufficiency" to external supply via
filters 105F006 / 105F007.

Increase the level in LP-flash vessel 105C003 and take semi lean solvent pump 105P001B in
operation.

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105P001A/B Semi lean solvent pump

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Before start up of semi lean solvent pump following steps have already been done:

 The block valves in suction lines are opened.

 Pump suction line, pump casing and the discharge up to the quick acting valves XV 105003 /
XV 105004 are filled and vented as far as possible. Line downstream XV 105003 / XV
105004 up to flow control valve FV 105001 is filled and vented by opening XV 105003 rep.
XV 105004 This can be achieved by overriding the relevant trip signal (trip 105.5 / trip 105.6).
As long as the override is activated it's recommended to keep the manual block valve
downstream of control valve FV 105001 closed. Prior to start up of lean solvent pumps
105P001A/B the override must be removed.
 Strainers in sealing medium lines are checked, the line is flushed and vented, flow of sealing
medium is adjusted.
 The oil system is put in operation.

10 seconds after start of the semi lean solvent pump 105P001A or B, discharge valves
XV 105003 resp. XV 105004 open automatically. Now the discharge line MS29-105208-28"
(PID 105-3) is to be vented, a vent is provided upstream of FV 105001. Since this set of
pumps is not provided with a minimum flow device, a flow of at least 1500 m3/h shall be
adjusted as soon as possible while opening FV 105001. The semi lean solvent pump
105P001A/B is tripped automatically after 3 minutes if the flow at FI 105001 is not above 1300
m3/h.

The MDEA solvent flow to absorber 105C001 is now to be controlled by FV 105001. The
setpoint of FV 105001 should be at 1700 m3/h to avoid unnecessary min. flow trip 105.14 of the
semi lean solvent pump.
The semi lean solvent cycle is closed now.

During this period the pump must be checked continuously and vent valve will be closed after
complete venting. If the level in LP-flash vessel 105C003 cannot be maintained the semi lean
solvent pump must be switched off, LP-flash vessel refilled and the pump restarted.

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Slop (filling) pump 105P005 is to be switched off as soon as the normal level of column sumps
are reached in the cycle operation. The control system of the solvent cycle is to be checked and
adjusted. The pressure in absorber 105C001 is maintained by adding gas to the system.
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4.2.2 Operating of the carbon dioxide scrubbing system while circulating the nitrogen and
steam feeding in the primary system
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The solvent cycle is operating satisfactorily according to 4.2.1.

Up to this point all work within the carbon dioxide scrubbing system could be carried out
independently of the operation of the primary system.

To preheat the primary system, nitrogen is first circulated, followed by steam. During this period
of operation, reboiler 105E002 may be used for heating of solvent cycle.

4.2.3 Heating the solvent cycle

The solvent cycle should be operating satisfactorily according to 4.2.1. Methanation system is
shut off. If no process gas is available at this stage low-pressure steam can also be used.
a) Mode of operation using desulphurized process gas (hydrogen sulfide content less than
0.5 ppm)

The HT-conversion catalyst is desulphurized. The gas is vented to flare via PV 104003.
The valve HV 104004 (bypass of the inlet gate valve XV 104004 to the heat exchangers
105E001, 105E002, 105E004) is to be opened carefully and the pressure is to be
increased gradually. After pressure equilibrium is established, the quick acting valve XV
104004 is to be opened. The bypass line GV24-104022-12" (PID 105-1) around 105E001
and 105E002 is to be kept closed during this operation.
The inlet gate valve to the absorber 105C001 will remain closed during heating up the
solvent cycle. The pressure upstream absorber 105C001 will be maintained by pressure
controller PIC 105013, therefore the pressure transmitter must be connected to the
pressure tap upstream of the absorber 105C001. The process gas is vented through
PV 105013 to the flare 106V801. Solvent heating is now performed by process gas within
the tube side of reboiler 105E002. Thermal stresses in the piping of the solvent cycle
must be avoided during the heating-up process. Slow increase of the heating rate can be
achieved by gradually shifting the process vent from PV 104003 to PV 105013.
The quantity of gas is to be adjusted so that the solvent is heated by approx. 20 ° C/h and
a sump temperature of 119° C is finally achieved in the stripper 105C004.

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As a general principle the heat exchangers 105E001, 105E002, 105E004 must not be
heated with process gas unless BFW level is adjusted on shellside of 105E001, the
solvent cycle is in operation and Polished water is fed to the shellside of 105E004.
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The entire quantity of condensate from separator 105F001 is drained until it is pure. Then
it is switched over to the water treatment system via condensate stripper 180C001.

The level in 105E001 is controlled by LIC 105001 by means of adding boiler feed water.
The LP-steam generated in 105E001 is supplied directly to the Deaerator 182D001 via
line SL30-105327-12" (PID 105-1) the pressure of 105E001 controlled by PIC 105001.

Vapors condensed in CO2-coolers 105E006A-E are collected in separator 105F003 and

drained to trench (DR 054) until it is pure, then the condensate is returned to the LP-flash
vessel 105C003 by means of reflux pump 105P006A/B. The water loss during
commissioning of 105F003 will be made up by adding boiler feed water to the absorber
via line WF25-105451-1" (PID 105-4).

b) Operation with low pressure steam

The inlet gate valve XV104004 to heat exchanger 105E001, 105E002, 105E004 is closed.
The inlet gate valve to absorber 105C001 is closed too. LP steam will be admitted to
105E001 via lines SL21-105333-4” (PID 105-1), SL21-105326-4” (PID 105-1), GV24-
104024-4"(PID 105-1) and GV24-104005-28" (PID 105-1). Setpoint of PIC 105001, LP
steam from 105E001 to Deaerator 182D001, is to be set to approx. 5.0 bar abs in order to
minimize condensation in 105E001. MDEA solvent is heated up by condensing LP steam
in the tubside of reboiler 105E002.
LP steam generator 105E001 and Demin Water Preheater 105E004 must be filled on the
shellside during this operation in order to avoid thermal stress on the tubes. Condensate
from 105E002 will be collected in separator 105F001 and is drained until it is pure. Then
the condensate will be lined to the condensate stripper 180C001 via stripper feed pump
180P001A/B.
The quantity of LP steam admitted to 105E001, 105E002, 105E004 has to be adjusted
manually so that the solvent is heated up by approx. 20 °C/h and to a sump temperature
of stripper 105C004 of 119 °C.

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4.2.4 Passivation of the System

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General: The aMDEA system does not require long time passivation, but it is strongly
recommended to operate the CO2 removal system for the first start-up preferable 3 consecutive
days (minimum 24 hours) without introducing CO2 containing gas to the system (just circulation
of solution). Establish first a flow of 50 % of the normal flow rates, increase this flow gradually to
100% and keep the normal operating temperatures by adding steam and cooling the solution.
Circulation of the lean amine promotes the formation of a very stable, corrosion-resistant
passivation layer of the metal surface of equipment and packing material and avoids corrosion
and formation of sludge.
Check the solution for foam activity and amine concentration.
For a restart of the CO2 removal, after every regular inspection, it is recommended to repeat this
passivation procedure.

If the plant has been shut down for a short time (a few days) with no exposure to air, a restart
without full re-passivation is probably satisfactory. To avoid corrosion it is recommended, that 24
hours before the process gas is fed into the absorber 105C001 to start the circulation of solution.

4.2.5 Gas feed to absorber 105C001

Solvent cycle and gas flow are to be in operation according to 4.2.3. Separator 105F003 must be
filled with Polished water up to the normal level, if not enough vapors are condensed.

See 4.2.4. for passivation of the system.

One or two hours before gas feeding to the absorber add the initial charge of anti foam
agent (see 4.1)

When the hydrogen sulfide content of the process gas from the HT-shift conversion is lower than
0.5 ppm, the gas may be fed to absorber 105C001. At that time it is absolutely necessary that
the steam line GV24-104024-4" (PID 105-1) is closed by closing the double shut-off valves
and by removing the spool piece so that process gas cannot enter backwards into the steam
system.

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Pressure equalization between gas line and absorber must be performed carefully, to prevent
pressure surges that might cause damage to internals. Therefore, pressure equalization and
introducing gas to the MDEA system is carried out as follows:
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The feedgas rate to the MDEA process can be increased to 25 % of the design value within less
than 15 minutes if the temperature of the regenerated solvent is adjusted before the feedgas
enters the absorber. During the initial start up the capacity should be increased to 100 % in four
steps:
- to about 50 % within 30 minutes
- from 50 to 80 % within 30 minutes
- from 80 to 90 % within 15 minutes
- from 90 to 100 % within 30 minutes

The solution flow should be adjusted to the gas flow, but in general the solution flow is not lower
than 70% of the normal capacity to ensure a uniform distribution in the columns.

Foaming tendency has to be observed carefully, specially at loads above 80%.

If a smooth operation of the system is observed, absence of any foam-active components,

changes in capacity can be performed from 0 to 100 % within less than 1 hour.

4.2.6 MDEA solvent concentration for operation

The CO2 removal system is designed for a solution strength of 40 wt-% of amine. The tolerance
range for the solution strength during operation is as follows:

Target Figure: 40 wt-%

Tolerance range: 37 to 45 wt-%

Note that during a test run the solution strength shall not be lower than the design figure.

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4.2.7 Operation of the semi lean solvent pump 105P001A/B

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The operation of the semilean solvent pump 105P001A/B is described under 4.2.1.
See also manual of manufacturer.

4.2.8 Operation of the lean solvent pump 105P003A/B

The operation of the lean solvent pump 105P003A/B will be as described under 4.2.1
See also manual of manufacturer.

4.2.9 Operation of stripper feed pump 105P002A/B

The operation of the lean solvent pump 105P002A/B will be as described under 4.2.1
See also manual of manufacturer.

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4.2.10 Operation of the LP Steam generator 105E001

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The LP Steam Generator 105E001 supplies low pressure steam directly to the deaerator
182D001. The LP Steam Generator shall not be operated without sufficient water level at
the shell side.

The heat duty of this heat exchanger can be controlled by:

a) de- or increasing the steam pressure in the heat exchanger with PIC105001

A higher pressure in the LP-steam generator increases the shell-side temperature and the
driving force (temperature difference) between shell- and tubeside is reduced which results in a
lower heat exchange. This increases the heat availability for the reboiler 105E002. The operating
pressure shall be adjusted between approx. 2.5 bar abs (Deaerator operating pressure is 2.3 bar
abs) and 5.0 bar abs. If the pressure is higher than 5.0 bar g, TRIP 105.09 will be initiated, the
reason for this higher pressure can be a tube rupture in 105E001; the system has to be checked.

b) operating the bypass (for 105E001 and 105E002) GV24-104022-12"

If the bypass valve in line GV24-104022-12" (PID 105-1) will be opened (or partly opened) heat
will be transferred to the Demin Water Preheater 105E004. It has to be ensured, that enough
heat is available for the reboiler 105E002 to regenerate the MDEA solution.

4.2.11 Operation of the Polished water preheating

When the feed water supply to the deaerator is started, the Demin Water Preheater 105E004 is
not yet in operation from the gas side.

As soon as the heating of the solvent cycle is started up the Polished water will be preheated.
There is no control of the Polished water temperatures. The temperature can be monitored by
TI 182003.

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4.2.12 Operation of process condensate system

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The obtained process condensate is collected in separator 105F001, which is the suction vessel
for stripper feed pump 180P001A/B. Separator 105F001 is level controlled by LIC 105002 acting
on level control valve LV 105002 located on the discharge side of 180P001A/B.
In case of failure in system 180 or during start up the process condensate must be drained.

The process condensate stripper is described in II/1.12 of this operating manual.

4.2.13 Operation of the CO2-vapour steam condensate system

The operation of this system is described under para 4.2.3. Operation of the reflux pumps
105P006A/B is described in manufacturer's manual.

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4.2.14 Addition of antifoam agent

Antifoam agent is added:

a) when the solvent foams, especially during the initial period of operation, due to foam-
forming impurities in the plant. The solvent is to be continually checked for resistance to
foaming. Separator 105F002 is to be checked for entrained solvent.

b) to improve the hydrodynamic properties of the loaded solvent. Foaming of solvent will be
indicated by PDIH 105002 for absorber 105C001. Antifoam agent will be injected on the
suction side of semi lean solvent pump 105P001A or B and the suction side of lean
solvent pump 105P003A or B. Foaming in HP-flash vessel 105C002 is indicated by PDIH
105009. In this case, antifoam agent will be injected into the outlet line of hydraulic turbine
105MT01, resp. bypass valve LV 105004B. All the antifoam dosing will be performed by
dosing pump 105P301.

Antifoam agent is introduced into a small solvent flow taken from the discharge of lean
solvent pump 105P003A or B to the above mentioned injecting positions, in order to
assure a good distribution of the antifoam agent within the solvent.

Amerel 1500 will be used as antifoam agent and an initial concentration of 50 ppm (wt)
(see 4.1) of Amine is recommended by the manufacturer of the antifoam agent.
Experience of the licensor BASF shows, that injection of antifoam agent shall be started
only in case of foaming tendency. Checks should be made during operation what quantity
has to be used.

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4.2.15 Operation of slop drum 105D001

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All solvent leakage fluids are collected in the slop system of the CO2-removal system and fed
to the slop drum.
When a certain level has been reached all the leakage fluids will be drained by means of slop
pump 105P004 via solvent filter 105F005 into MDEA storage tank 105T001. Slop-pump
105P004 is shut down automatically by low level switch LISL 105021 (Trip 105.2). As in the case
of all other pumps, the operating instructions of the manufacturer must be observed for slop-
pump 105P004.

4.2.16 Operation of MDEA-Filter 105F005

This Filter is designed for a continuous filtration of a side stream of the MDEA solvent
circulation. If the pressure drop across the filter is above the allowable figure (PDI 105123), the
cartridges of the filter have to be changed. For start-up of the solvent filter the instructions of the
manufacturer are to be followed.

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4.2.17 Operation at partial load

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During operation at partial load, the solvent flow rate should be reduced proportionally to the gas
flow rate, in order to load the solvent highly with carbon dioxide. This aids regeneration of the
solvent. Limitation of the liquid load of absorber packing should be > 20 m³/m²/h. However, the
semi lean solvent (FV 105001) should be reduced first, and only then the lean solvent sent to top
of absorber 105C001, till the proportion is settled again. When reducing the solvent which is sent
to the top of absorber 105C001, it is to be observed that the carbon dioxide content does not
increase at the outlet of the absorber. A too low liquid loading might lead to maldistribution and
to a breakthrough of CO2.

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Section 5
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5. Shut-down of the system

5.1 General notes
5.2 Voluntary shut-down
5.3 Emergency shut-down
5.4 Restarting the system

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5. Shut down of the system

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5.1 General notes

For every shut-down, especially in the case of a voluntary shut-down, each step must be carried
out with a view to minimizing the operations for a subsequent start-up.

The duration of the voluntary shut-down is the decisive factor in determining whether the plant is
to be shut down completely and drained, or whether only the production flow is to be interrupted
while operation of the scrubbing liquid cycle, for instance, is maintained.

In so far as shut-down of a piece of equipment or a machine is not directly due to repairs on that
equipment or machinery, all machinery, equipment and instruments are to be made ready for
start-up again as soon as it is possible after shut-down.

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5.2 Voluntary shut-down

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Shut-down of the CO2-removal system is to be seen in coherence with a voluntary shut-down of

the entire ammonia plant. The solvent cycles are to be reduced proportionally with the
decreasing process gas flow when reducing the front end load. However, the semi lean solvent
(FV 105001) should be reduced first, and only then the lean solvent sent to top of absorber
105C001, till the proportion is settled again. Special attention is to be paid on the CO2 content in
the process gas outlet absorber 105C001.

At approx. 50% plant load the process units downstream of the CO2-removal system are taken
out of operation.

- Process gas is vented downstream absorber 105C001 via PV 105013 to flare, the
methanation inlet valve XV 106001 is closed.
- At latest now the CO2 fed to the UREA-plant shall be stopped and vented to atmosphere via
PV 105016A/B.
- Fuel gas withdrawn from the HP-flash vessel and supplied to the primary reformer fuel gas
system shall be rerouted via PV 105006B to flare.
- Gradually reduce the solvent circulation through FV 105001, FV 105002 and TV 105007
- Gradually transfer the venting process gas from PV 105013 to PV 104003
- Keep the absorber under pressure for solvent circulation
- Initiate trip 104.1 by HS 104005 (PID 104-3)
- Close wash water to absorber top (105C001)
- Divert process condensate form 105F001 to dump
- Continue operation of the liquid cycles until the entire solvent inventory has been
regenerated. If it is intended to shut down the system for a short period only continue
operation of the liquid cycles ( see also 7.1 - Drainage of Solution, hot work at Storage Tank
105T001).
- As soon as the front end is completely shut down or the shut off valve XV 104004 has been
closed, isolate LP-steam generator 105E001 on BFW-side and LP-steam-side.
- Isolate online CO2 analyser A105001
- Stop hydraulic turbine 105MT01 by shifting absorber level control from LV 105004A to LV
105004B. Close motorized valve 105X90 at outlet of 105MT01.
- Stop semilean solvent pump 105P001A. Check closing of control valve FV 105001 and
discharge valves XV 105003 resp. XV 105004. Close manual block valves
upstream/downstream FV 105001.

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- Provide "self supply" of sealing medium for stripper feed pump 105P002A/B and lean
solvent pump 105P003A/B. Start draining solvent (partially) to storage tank via filter.
- Stop lean solvent pump 105P003A/B Check closing of control valve FV 105002 and
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discharge valve XV 105005 resp. XV 105006. Close manual block valves

upstream/downstream FV 105002.
- Stop stripper feed pump 105P002A/B and reflux pump 105P006A/B and close
suction/discharge isolation valves.
- Keep normal levels in all columns for start up/restart of system.
- The CO2-removal system can be isolated from the upstream process system by closing shut
off valves XV 104004 and HV 104004.
- Depending on purpose and duration of shut down it shall be decided to depressurize and
purge the system with nitrogen or to lower the absorber pressure and leave the system
under process gas atmosphere. However the HP-flash vessel and LP-flash vessel shall be
superimposed by nitrogen avoiding vacuum and thus penetration of air into the system.

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5.3 Emergency shut-down

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An emergency shut-down is required if an essential utility supply fails or if damage is detected in

the system which would not permit further operation nor voluntary shut-down of the plant due to
lack of time. The internal interlocks of the carbon dioxide scrubbing system are described in the
trip schedule which is a part of the process manual. These interlocks do not cause a complete
shut-down. Only sections of the plant are being by-passed or shut-down.
An emergency shut-down of the entire plant can only be effected by the plant trip. In the event
that this is actuated, the following measures shall immediately be taken.

Close outlet valve of hydraulic turbine 105MT01.

XV 106001 at outlet of CO2-scrubbing system has to be closed as far as not yet closed by trip.

BFW to absorber 105C001 and condensate to LP-flash vessel 105C003 must be shut off.

BFW to LP-steam generator 105E001 must be shut off.

Check close position of pump discharge valves XV 105003, XV 105004, XV 105005 and XV
105006

After an emergency shut-down followed by a prolonged shut-down, regeneration of the solvent is

to be restarted as soon as possible. If no gas is available, the reboiler is heated by steam for
regenerating the solvent (see 4.2.3).

Power failure is equivalent to an emergency shut-down. The operations described above are to
be carried out by hand immediately.

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5.4 Restarting the system

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When the carbon dioxide scrubbing system is being restarted, basically all steps of the initial
start-up are repeated, omitting, of course those start-up actions, which are to be performed only
once, e.g. filling with operating solvent, setting of control characteristics etc.

As a rule with exception of local start-up of machinery and opening of valves, the carbon dioxide
scrubbing system is started from the control room by adjusting the set points of the control
instruments. Initially, start-up is effected without product gas (only for a very short interruption
process gas may be used). The carbon dioxide scrubbing system is nitrogen-blanketed,
absorber 105C001 is pressurized (refer to 4.2.1); separator 105F003 is filled with water up to
normal level. The HP-flash vessel 105C002 and the LP-flash vessel 105C003 bottom is filled
with MDEA solvent as well as the stripper 105C004 and the solvent level in the absorber
105C001 bottom is visible. Check, whether re-passivation is required (refer to 4.2.4).

MDEA solvent pumps started acc. to chapter 4.2.5 to 4.2.7. Flow controllers FIC 105001 and
FIC 105002 are at manual operation. The solvent flow is run up quickly. The solvent level in
absorber 105C001 is adjusted by means of expansion valve LV 105004B. Solvent cycle is to be
stabilized.

Then product gas may be fed to the system. If the solvent was not regenerated completely
during the previous shut-down, this has to take place well before feeding gas into absorber
105C001. During this process, the methanator 106R001 must be closed (refer to 4.2.3). The
solvent temperatures are increased. Water losses are made up by feeding BFW to the top of
absorber 105C001. Before process condensate is discharged from separator 105F001 via
condensate stripper into the water treatment system, the condensate must be checked.

As soon as the MDEA solvent cycle is operating normally, the product gas may be fed to
absorber 105C001. As long as the carbon dioxide content of the product gas has not yet
reached the set point, the gas is discharged to the flare via PV 105013 upstream of the inlet to
methanator 106R001.

The analytical checks according to section 6 are to be carried out. Any corrections required,
such as corrections of the solvent concentration or of the degree of regeneration of the solvent
are to be carried out.

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Section 6
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6. Operational checks
6.1 Methods and schedule of analyses
6.2 Other checks

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6. Operational checks
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6.1 Methods and schedule of analyses

The methods of analyses to be applied are listed in the 'Sampling Schedule'.

Analyzer recorders are provided where continuous analysis is needed for reliable process
control.

Sampling points are provided where regular analyses are sufficient to ensure adequate
monitoring of the process. These samples are analyzed in the plant laboratory.

The following are listed in the sampling schedule:

- Tag number of sample
- fluid to be analysed
- location of sampling point
- state of the sample
- frequency of sampling
- properties to be analysed
- expected value
- method and/or apparatus
- P&I No

The following symbols are used in the schedule:

C = continuously analysis
R = on request of plant supervision
A = at delivery
M = once per month
0,5H = every two hours
H = once per hour
2H = twice per hour
0,5S = every two shifts
S = once per shift
2S = twice per shift

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0,5D = every two days

D = once per day
2D = twice per day
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0,5W = every two weeks

W = once per week
2W = twice per week

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Insert Sampling Schedule

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Insert Sampling Schedule

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6.2 Other checks

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Visual checks of the operating solvent are to be carried out once per shift (lowering the
temperature of the solvent from operating temperature to ambient temperature in a beaker).

As a preventive measure all level indicators in the solvent section shall be drained and cleaned
periodically.

In similar systems it was found expedient to open and close all controllers for a brief period by
hand, about once a week.

Stand-by pumps should be operated briefly in parallel to the operating pump at appropriate
intervals, which should not be too long, in order to ensure that the machinery is always ready for
operation.

The system is to be checked continually for leaks. All mechanical checks are to be carried out in
accordance with the manufacturer's instructions.

All measured values, such as flow rates, pressures, temperatures etc. must be checked and
recorded periodically.

It is recommended to plot the analysis results for loaded and regenerated MDEA solvent.
Tendencies can be noticed more easily this way and suitable measures can be taken in time.

When the carbon dioxide scrubbing system is running steady at full load, carbon dioxide
analyses are to be taken at the following analyses elements: AP 105102 to AP 105104. These
analysis results are to be plotted graphically above absorber height. A graph will result.

These analyses are to be repeated approx. quarterly. While comparing the new values with
those taken before, possible disturbance occurring in a packing material layer will be noticed.

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Section 7
7. Troubleshooting, Trip- and Interlock System
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7.1 Troubleshooting
Trouble Action
7.1.1 Differential Pressure high in add Antifoam AMAREL 1500
columns 105C001, 105C002
and 105C003
7.1.2 High temperature rise in Urea 1. add Antifoam
H2 removal Reactor 2. Check Absorber and HP-Flash vessel level
7.1.3 MDEA solvent concentration is Open FV 105005 and dump the condensate from
to low 105F003
7.1.4 MDEA solvent concentration is Close FV 105005 and feed condensate direct to 105C003
to high
7.1.5 Absorber 105C001 level LI 1. Increase the level in 105C001 by 2 -3 %
105005 AB low 2.Check the individual level transmitters
7.1.6 Suction Pressure of 105P003 1. Change over the pump to the stand-by pump
low 2. Clean strainer
7.1.7 If semi lean solution pump 1. After 30 seconds time delay, Trip F1 will be initiated.
105P001 A or B trips According to the situation use override for this.
2. Start standby pump (inform Power Supply).
3. If the situation is unchanged (no pump running) vent
gas partially through PV 104003.
4. Monitor Methanator temperature. Initiate Trip F1 if
required.

7.1.8 If lean solution pump 105P003 1. increase semi lean solution circulation.
A or B trips 2. Monitor Methanator temperature.
3. Confirm the stand-by pump and establish the
circulation
4. Vent slightly via PV 104003 if CO2 slip is still
increasing and take care of 107K001 suction pressure.

7.2 Trip- and Interlock System

The trips and interlocks of the system are shown in detail in Part I, section 9 “ Trip and Interlock
Schedule Ammonia Plant” of this Operating Manual. The trips and interlocks are also shown in
the corresponding P& I-diagrams.
A schematic diagram of the Trip-and Interlock system for this Process unit is attached

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Section 8
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8. Safety instructions
8.1 Drainage of Solution, hot work at Storage Tank 105T001

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8. Safety instructions
R:\AP_10_0_VT\10.71_Operating Manual\NH3\Operating Manual SORFERT Ammonia Plant 1\Part_II-1\Revision 01\Oper_Man_Unit 105_Rev01.doc

Operational safety measures and safety instructions are comprehensively covered in Part VI, of
the Process Manual.

8.1 Drainage of Solution, hot work at Storage Tank 105T001

If the CO2 removal has to be emptied (e.g. for inspection) the MDEA solution will be drained to
the storage tank 105T001. Non regenerated solution may contain combustibles. It is strongly
recommended to regenerate the solution completely before filling it into the storage tank.

1. Therefore, if the solution is to be drained into the storage tank, the synthesis gas flow to the
absorber 105C001 will have to be isolated. The gas phase in the absorber is to be replaced
by nitrogen. The solution circulation is to be in operation (at a lower circulation rate if
required) and heat (e.g. produced by LP steam) is to be introduced into the stripper
105C004. If the solution is free from hydrogen (after 1-3 hours of circulation), the solution
can be drained into the storage tank 105T001 using the connections from the LP-Flash
vessel 105C002 and/or the absorber 105C001.
2. Before starting hot work (especially welding, cutting etc.) at the storage tank, make sure that
the tank is free from hydrogen, methane or other combustible gases. It is strongly
recommended to flush the tank with nitrogen. Therefore, the nitrogen connection N20-
105307-1" (PID 105-8) may be used, before introducing nitrogen open the vent valve of the
storage tank (1" bypass of the safety valve RV105001 at the top of the tank). Before starting
the hot work check the tank gas phase whether any explosive mixture is still available, if so,
continue purging with nitrogen.

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