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SULZER
Project:
Rev.1 9018377_PT_ENERCO_TDAE_BE
07.06.2016 PROCESS BOOK Sulzer Singapore Pte Ltd

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INSTRUCTIONS Sect-1.doc

Contents

1 INTRODUCTION............................................................................................................ 2

2 GENERAL OPERATING INSTRUCTIONS FOR COMMISSIONING ............................. 3

3 CAUSES AND ELIMINATION OF OPERATING PROBLEMS FOR EXTRACTION

COLUMNS TYPE KÜHNITM ECR .......................................................................................... 5
3.1 PROBLEM: EXTRACTION EFFICIENCY IS NOT GOOD ENOUGH ................... 5
3.2 PROBLEM: COLUMN FLOODING ....................................................................... 8
3.3 PROBLEM: EMULSIFICATION ............................................................................ 9
3.4 PROBLEM: INCOMPLETE DECANTATION ...................................................... 10
3.5 PROBLEM: ACCUMULATION OF SLURRY / CRUS AT THE INTERFACE ...... 10

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 Client:
Section 7 SULZER
ThyssenKrupp
Industrial Solution
PRELIMINARY OPERATING
Sulzer Singapore Pte Ltd
INSTRUCTIONS

1 INTRODUCTION

This Engineering documentation contains the process operating manual for the extraction
column 10-R-01. The main purpose of this document is to describe the column operation
from process point of view.

The parts in this process operational manual dealing with mechanical parts and instruments
which are not yet defined only have a general character. It has to be read in conjunction
with the operating manual of the motor, drive unit, frequency converter, mechanical seal and
all other instruments and process equipment as well as the manual from the pressure
vessel manufacturer of the column shell.

The clients are:

PT. Enerco RPO International and ThyssenKrupp Industrial Solutions (Thailand) Ltd.

The supplier of the process technology and key equipment for the extraction step is:
Sulzer Chemtech Ltd
Gewerbestrasse 28, P.O. Box
4123 Allschwil
Switzerland

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way communica-ted or made accessible to third parties without our written consent.
 Client:
Section 7 SULZER
ThyssenKrupp
Industrial Solution
PRELIMINARY OPERATING
Sulzer Singapore Pte Ltd
INSTRUCTIONS

2 GENERAL OPERATING INSTRUCTIONS FOR COMMISSIONING

General Remark: The extractor is an integral part of the whole plant. As such the below
Operating Instructions are considered "as General" only. Operation shall also be in
compliance with overall operation and process requirements of the solvent recovery section.
The overall and detailed procedures will be defined during FEED/DE to maintain the
integrity of plant operation during these phases of operation.
Prior and during S/U and Initial Operation it is strongly recommended Sulzer to be present
on site as advisor.

1. First of all please check the oil level of the gear drive unit (oil type and maintenance
instructions of the drive unit are included within the technical documentation).

2. You now have to check the electrical wiring to the drive unit (see instructions
received from supplier of the motor). Please note that the direction of rotation for the
driving shaft shall be clockwise at view from top of the column downwards.

3. You now can start the drive unit and let the shaft turn for max. 1 minute at low speed
(e.g. 2-4 rpm) in order to check the direction of rotation and once more if the internal
construction was fitted correctly and consequently no turning parts are in contact with
the stator plates.

Note: Because the column is still empty (means without liquid filling) and therefore the
bearing sleeves made of PTFE "Lubriflon 904 blue" still dry you are not allowed to
rotate the shaft for a longer period of time. Otherwise this procedure may burn out
the PTFE - bearings sleeves, because without cooling there could result a kind of a
heat accumulation on the sliding surfaces of the sleeves.

4. The shaft sealing at top of the column operates with a mechanical seal. Please check
the technical documentation received for the mechanical seal and the seal media
device.

5. For the start up of the column, feed (diluted DAE9 and solvent (furfural) are started
simultaneously with a ramp up to 20% of the nominal flow rate.

6. The interface controller loop must be set to auto mode.

7. When the column is filled with liquid and the overflow to the raffinate receiver starts,
adjust the agitator speed to approx. 60 % of the expected operating agitation speed.

Remark:
Do not turn the column shaft for longer than 1 minute when the column is not
full of liquor; otherwise due to heat accumulation you may destroy the radial
shaft bearing sleeves made of PTFE "Lubriflon 904 blue"

8. Let the column stabilize for approx. 2 hours without changing the operating
conditions (flow rates, agitation speed etc.). During this time the hold up profile inside

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Sulzer Singapore Pte Ltd
INSTRUCTIONS

the column is established, the mass transfer happens and the column will reach
steady state conditions. It is recommended to take a sample of the raffinate and
extract of the column and analyze both samples. This should be repeated after
30mins unless at least two consecutive samples gives the same results. By this the
time for the column to reach steady state could be determined.

9. Slowly increase the agitator speed and the flow rates to the set point. Remind that
any change in the operating parameters takes approx. 2 hours to result in a change
in the raffinate and extract composition due to the residence time.

10. In case of flooding of the column, interrupt the feeding of the two phases and the
agitation speed for approx. 15-20 mins and restart again at a slightly lower agitation
speed (see also the following section “Causes and Elimination of Operating
Problems”).

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way communica-ted or made accessible to third parties without our written consent.
 Client:
Section 7 SULZER
ThyssenKrupp
Industrial Solution
PRELIMINARY OPERATING
Sulzer Singapore Pte Ltd
INSTRUCTIONS

3 CAUSES AND ELIMINATION OF OPERATING PROBLEMS

FOR EXTRACTION COLUMNS TYPE KÜHNITM ECR

The following sections describe typical problems liquid-liquid extraction processes and
potential solutions. The mentioned approaches for eliminating the problems are collected
from many years of experience with more than 500 industrial extraction columns so not all
of them may be applicable to this specific application and also observations from pilot scale
columns are included. However, they are included to give a better understanding of the
operation of an extraction column and help to identify the root cause in case any of the
problems occur.

3.1 PROBLEM: EXTRACTION EFFICIENCY IS NOT GOOD ENOUGH

Cause n° 1: Unstable operating conditions

Usually we will have steady state conditions approx. 2 hour after start up. As a rule of thumb
we can say after the liquid volume in the column has been replaced 3 (three)-times. If we
have unfavorable conditions (high phase ratio, low specific flow rates etc.) a longer period of
time for getting the column into equilibrium might be necessary.

However the most important point during start up of the column is to leave the adjusted
operating parameters (phase ratio, flow rates, agitation speed, composition of the feed and
the solvent, operating pressure, operating temperature etc.) unchanged during this period of
time as mentioned above.

Cause n° 2: Agitation speed is too low

The most frequent failure in case of an unsatisfactory extraction yield is a wrongly adjusted
agitation speed.

Elimination: Rise the agitation speed in small increments of approx. 10 % at hourly

intervals until the required extraction efficiency is achieved.

Do not forget to wait approx. 1 hour after each adjustment of the agitation
speed in order to allow the column to get into steady state conditions.

At a certain agitation speed the column will start to flood, we then have
reached the flooding point of the column. This flooding point depends on the
extraction system, the specific flow rate, the phase ratio, the geometry of
the internal construction etc.

Due to the fact that all these parameters are known for an industrial column
scaled up by us with process guarantee we will achieve the desired
extraction yield before getting to this "flooding" agitation speed.

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Industrial Solution
PRELIMINARY OPERATING
Sulzer Singapore Pte Ltd
INSTRUCTIONS

However a flooding of the column can either be recognized when we get an

entrainment of the dispersed phase into the outlet of the continuous phase
or in case we have a phase inversion somewhere in the agitated column
part. A phase inversion means that the former dispersed phase becomes
locally the continuous phase and the continuous phase the dispersed one.

Please note that in an extraction column only one interface should be seen.
As soon as you recognize another one this surely means that the column is
flooding.

As a general rule, optimum agitation speed is just below the flooding point.
For practical reasons, it is not always possible to run so close to such a
critical point in case conditions change.

As a rule of thumb: higher feed rates require lower agitation speeds and
hence lower feed rates permit a higher agitation
speed

Cause n° 3: Flow rate is too low

With low phase velocities (especially of the continuous phase), axial back mixing in each
agitated compartment and hence reduction of the concentration gradient becomes
excessive. This may result in a significant decreasing of the extraction efficiency.

Elimination: Raise the flow rate and readjust the optimum agitation speed (means lower
it accordingly).

In case a rising of the flow rate is impossible (only applicable for test units /
columns) replace the partition plates (stator plates) by ones with a smaller
free area.

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INSTRUCTIONS

Cause n° 4: Flow rate is too high

In order to prevent flooding of the column it is necessary to operate the agitator at lower
speed. This results in poor dispersion of the droplets (large drop sizes, small hold-up of the
dispersed phase) and hence a reduced mass transfer area.

Elimination: Reduce the flow rate and readjust the optimum agitation speed (means
higher it accordingly).

In case reducing the flow rate is not feasible (only applicable for test units /
columns) replace the partition plates (stator plates) by ones with a larger
free area.

Cause n° 5: Flow rate of the solvent phase (Extractive Agent) is too small

The required feed rate has to be established by tests or from equilibrium data (liquid-liquid
equilibrium diagram.

Elimination: Increase the flow rate of the solvent phase in order to give a higher phase
ratio (quantity of solvent phase / quantity of feed phase)

or

Decrease the flow rate of the feed phase in order to give a higher phase
ratio (quantity of solvent phase / quantity of feed phase)

It may also be necessary to adjust the agitation speed.

Cause n° 6: Purity of the solvent phase (Extractive Agent) is insufficient

Among others the minimum obtainable raffinate concentration depends strongly on the
content of solute (component to be extracted) in the solvent phase entering the column.
Difficulties often arise when the regenerated solvent does not meet the specifications.

Elimination: A better recovery by distillation / evaporation is necessary.

Cause n° 7: Gas or vapor bubbles in column

Air or inert gas entrained or dissolved in the feed / solvent or vapors from volatile fluids can
form bubbles in the column. These bubbles cause additional axial back mixing in the column
and can therefore reduce the extraction efficiency.

Elimination: If possible take suitable precautions to avoid the formation of bubbles, e.g.
degassing, checking of piping and pumps, rising of the operating pressure
by superimposing nitrogen, reducing the operating temperature (but not
below 40°C) etc.

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INSTRUCTIONS

3.2 PROBLEM: COLUMN FLOODING

Flooding occurs when a second interface builds up in the column, growing in the direction of
the outlet of the continuous phase. If left uncorrected, a portion of the dispersed phase,
mixed with the continuous phase, will flow out at the wrong end of the column. Flooding
occurs if more dispersed phase is fed to the column than the rising / falling droplets allow.
This also depends upon the droplet size so the following conditions can be shown to apply:

Agitation speed Droplet size Axial droplet velocity Flow rate of

dispersed phase
Low ⇒ Large ⇒ High ⇒ High
High ⇒ Small ⇒ Low ⇒ Low

If the flow rate of the dispersed phase is increased, the agitator speed has to be reduced
slightly to compensate for the larger amount of droplets which have to pass through the
column. If the flow rate is decreased, the agitator speed should be slightly increased vice
versa.

Droplet size depends not only on the agitation speed but also on the physical properties
(like interfacial surface tension, density, viscosity etc.) of the two phases (organic and
aqueous phase). As the physical properties may vary from one agitated compartment to the
other, so as well can these data influence the droplet size.

Cause n° 1: Agitation speed is too high

Elimination: - reduce the agitation speed

- switch off agitator and stop feeds for approx. 5 minutes
- restart the feeds and agitator (at reduced speed)
- in case the column is still flooding repeat the steps mentioned before

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INSTRUCTIONS

Cause n° 2: Flow rate is too high

The feed rate of the dispersed phase is higher than the axial droplet velocity allows, column
is flooding.

Elimination: - reduce the feed rate (keeping same phase ratio)

- switch off agitation and stop feeds for approx. 5 minutes
- restart the feeds (at reduced flow rates) and agitator
- in case the column is still flooding repeat the steps mentioned before

Note: Flooding of the column can be avoided by either reducing the agitation
speed or the flow rate. However decreasing the agitation speed is somehow
limited, because a larger droplet size automatically means a smaller mass
transfer area and therefore a reduced extraction efficiency.

3.3 OTHER OPERATIONAL PROBLEMS.

The following operational problems and measure are mentioned to have a complete
overview about potential problem which may occur in general extraction processes. None of
the mentioned issues below was observed in the pilot trials and consequently none of them
are likely to occur in the industrial column.

Nevertheless, in other processes they may occur and to give a full overview about
operational issues they are mentioned in the following sections.

3.3.1 PROBLEM: EMULSIFICATION

Please remind that the stated measures are of general nature and only mentioned to have a
complete overview. Several of them are not applicable in the industrial scale column.

Any tendency to emulsify will have a negative effect on the separation and will considerably
reduce the specific flow rate. Emulsification may be reduced by:

− reducing the agitation speed

− varying the temperature
− varying the pH-value
− raising the density difference between the two phases by adding an indifferent salt
− changing the physical properties of one phase by adding another solute (mixing
solvent
Quite often the emulsification of a system can also reduce or even avoid by changing the
dispersed phase. This means that a system may emulsify with e.g. the aqueous phase
dispersed, but no emulsification will appear with the organic phase dispersed.

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INSTRUCTIONS

A further reason for emulsion formation in a column may be that the internal construction is
not clean and does have some residues from a former operation on their surfaces (appears
quite often with our laboratory and pilot extraction columns). In such a case just clean the
internal construction with e.g. acetone and restart the extraction.

In case all the above does not solve the problem another solvent has to be used.

3.4 PROBLEM: INCOMPLETE DECANTATION

Incomplete decantation may be another effect of emulsification.

In case of incomplete decantation we additionally recommend:

− • Using an additional external separator.

It is often favorable to use storage tanks or intermediate tanks as a separator.

− • Using an additional centrifugal decanter.

Also this problem was not observed in the pilot trials.

3.5 PROBLEM: ACCUMULATION OF SLURRY / CRUS AT THE INTERFACE

The precipitation of slurry does not generally affect operation, although an accumulation
may interfere with the control of the interface. Periodic removal of sludge may prove
necessary.

Quite often the accumulation of slurry at the interface (third phase) can be reduced or even
avoid by changing the dispersed phase.

Also this problem was not observed in the pilot trials.

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