2018

Operating / Troubleshooting
‘STEPS’ for off-line grade
changeover from Series Grade
(F55HM0003N)
TO
Parallel ‘A’ Grade (W55A004N)
in HDPE Plant
Operating and Trouble Soothing Steps for ‘Off-Line Grade Changeover’
from F55HM0003N TO W55A004N in HDPE

1. SCOPE:

Change Over in Normal Operation (Off-line) from F55HM0003N (Series

mode) to W55A004N (Parallel “A” mode) for production @ 10 MT/Hr.
2. RUNNING CONDITIONS FOR SERIES MODE:
Plant Load from existing running grade (i.e. F55HM0003N) should be
reduced to minimum load (10 MT/Hr).

For F55HM0003N

Reactors conditions for F55HM0003N

PLANT LOAD 10 TPH PELLET 0.952~0.955
DENSITY
MFI 0.07~0.09 COLOUR < +1
UNIT RB-201 RB-221
Ethylene feed rate MT/hr 4.95 5.05
Co-monomer feed rate Wt. % of C2 -- 2.0
Reactor temperature °C 85 80
DC ratio % 50 85
PZ catalyst feed rate Kg/hr 130~145 -
(Conc. 8.0 mmol/lt.)
AT catalyst feed rate Kg/hr 25~35 -
(Conc. 200 mmol/lt.)
PZ conc. In reactor Mmol/lt Hx 0.085 -
AT conc. In reactor Mmol/lt Hx 0.5 -
Reactor pressure Kg/cm g
2
6.5 ~ 7.0 3.0
Ethylene part. Press. Kg/cm2 g 0.55~0.63 0.55~0.65
H2/C2 ratio in MAPS Mol/Mol 09~10 0.12~0.15
Slurry Conc. gm/l-Hx. 400 350
Additive Dosing
AE-IRGANOX 1010 PPM 450
AK-IRGAFOS 168 PPM 1200
HA- CALCIUM STEARATE PPM 1600
OB PPM 0.5

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 3. RUNNING CONDITIONS FOR PARALLEL “A” MODE:

For W55A004N

Reactors conditions for W55A004N

PLANT LOAD 10 TPH PELLET 0.954~0.957
DENSITY
MFI 0.4~0.5 COLOUR >60
UNIT RB-201 RB-221
Ethylene feed rate MT/hr 5.0 5.0
Propylene feed rate Wt.% of C2 0.32 0.32
Reactor temperature °C 85 85
DC ratio % 90 90
PZ catalyst feed rate Kg/hr 35~45 35~45
(Conc. 3.0 mmol/lt)
AT catalyst feed rate Kg/hr 25~35 25~35
(Conc. 200 mmol/lt)
PZ conc. In reactor Mmol/lt HX 0.011 0.011
AT conc. In reactor Mmol/lt HX 0.5 0.5
Reactor pressure Kg/cm2 g 4~5 4~5
Ethylene part. Press. Kg/cm2 g 1.6~2.0 1.6~2.0
H2/C2 ratio in MAPS Mol/Mol 0.4~0.55 0.4~0.55
Slurry Conc. gm/l-Hx 400 400
Additive Dosing
AE-IRGANOX 1010 PPM 450
AK-IRGAFOS 168 PPM 1000
HA- CALCIUM STEARATE PPM 1200
AJ PPM 300
PPA PPM 200

4.0 REACTOR SHUT DOWN FOR OFFLINE GRADE CHANGEOVER:

4.1 Reactors Shut Down and dumping

1. Reduce plant load to 10 T/Hr.

2. Take out both slurry coolers from the system.

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3. Dump each slurry coolers to respective flash drums (VV203 & VV 223) in such a rate so that there is no
significant change in vessel pressure & as well slurry concentration.
4. After dumping fill both slurry coolers with fresh hexane and again dump out same hexane.
5. Actuate normal shutdown of RB201 from MAPS while reaction is running on in RB221.
Precaution: RG flow should be maintained above 3500 M 3/hr. to avoid reactor nozzles chocking.
Keep reactor jacket in heating mode so that reactor temperature can be maintained as high as
possible (@ 50oC).
6. Stop PZ catalyst & TEAL dozing pumps (PA 105 A/B/C & 106 A/B/C). Flush & isolate PZ catalyst and
TEAL lines to RB-201 with Hexane for 5 minutes to avoid any further chocking.
7. Isolate slurry in DC 1 lines & flush with Hexane for at least 3-5 minute to avoid chocking and isolate its
jacket hot water too.
8. Dump Reactor RB-201 to RB-221 via first flash drum at such rate as per level and pressure allowance
of vessels. During dumping empty out dilution drum VV 202 & wash with Hexane at least once.
Precaution: Flush Dilution drum outlet line properly to avoid chocking of line.
9. Actuate normal shutdown of RB-221 from MAPS.
10. Keep RG flow in reactor @3500 M3/hr & reactor jacket in heating mode so that reactor temperature can
be maintained as high as possible (@ 50oC).
Precaution: RG flow should be maintained above 3500 M3/hr to avoid reactor nozzles chocking.
11. Isolate slurry in DC-2 lines & flush with Hexane for at least 3-5 minute to avoid chocking and isolate its
jacket hot water too.
12. Dump Reactor RB-221 to second flash drum at such rate as per level and pressure allowance of vessels.
13. During dumping empty out dilution drum VV 222 & wash with Hexane at least once.
Precaution: Flush Dilution drum outlet line properly to avoid chocking of line.
14. Dumping speed although will depend upon the level of VV301 & VV701.

4.1.1 Troubleshooting during Reactors Shut down & Dumping:

Sr. Deviation Cause Effect Troubleshoot

No.
1. Low pressure  After actuation of SD,
in RB- reaction keep running
201/221 and till spent catalyst and
VV-205/225 ethylene got consumed.
So, pressure may dip
very low.
 AV-2201A/B
malfunctioned and got
 Tripping of  To avoid this, enough nitrogen
KA-201/221 supply can be fed to reactor by
and actuation of opening nitrogen bypass valve
POLY SD. in advance. AV-2201A/B
Logic will close position should be verified
dumping of from field.
reactors.
 Supply N2 /Open N2 bypass
meanwhile Hydrogen can be

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 open in field. also fed in reactor for pressure
makeup.
2. High Pressure  High rate of slurry  Actuation of  Slow down dumping rate and
in VV-203 & dumping from reactor PSHH on VV- check level of reactor and flash
VV-223 203 & VV-223 drums to verify reactor
 Reactor dumping has which will close emptiness. If reactor emptied
been completed and XV2301/2501 out then close dumping valve
Nitrogen is passing and after flushing with hexane.
LV2302A/B &  Increase load of KA-222 and
LV2502A/B. KA-881 compressors.
 KA-222 and KA-881 is
not running at optimum
load.

3. High Level in  High rate of Slurry  Actuation of  Slow down dumping rate from
VV-203 & dumping from reactor LSHH on VV- reactors
VV-223 or 203 & VV-223  Hexane flushing in
high current  Slurry transfer which will close PA-201/PA-221 suction line
of restriction in PA- XV2301/2501  Change over pump and clean
VM-203/VM- 201/221 suction or and spool piece of PA-201/PA-221
223 discharge line. LV2302A/B & to remove suspected lump.
LV2502A/B.
4. Level not  Chocking of reactor  Reactor dump  Stop dumping and flush
rising in VV- dump out line. out delayed till reactor dump out line.
203 /VV-223 further dumping  Immediately send maintenance
during  Malfunctioning of get started. team to attend any malfunction
dumping HV2303/2503 or LV- valve.
2302B/LV-2502B.  If due to any reason, reactor
dump out is not possible from
dump out line, another option
could be PA-203/223 suction
loop dump out line. This
practice should be followed
during emergency only.
5. Centrifuge  LV-2701 opening is  Centrifuge can  Control slurry dumping rate
running on high and high flow of trip on high and further reduce opening of
high Amp slurry from VV-223. amp which can LV-2701.
above 15 amp delay reactor
dumping
6. Dryer running  High slurry dumping  Less powder  Control slurry dumping rate if
on high rate conveyed to dumping rate is high.
current above  Steam condensate extruder as well  Check PPPPU pump in field
50A in HDPE- accumulation in dryer as damage to and if not working properly
1 and 80A in and volatile removal is dryer. Powder change over it. Still not
HDPE-2 low in dryer volatile content working properly then open
 Powder accumulation will increase. local drains.
in dryer because of  Check KB-401 and GF-303 in

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 restriction in field for any abnormalities.
pneumatic conveying Also observe discharge
line via KB-401. pressure of KB-401. It should
be 0.4-0.6 Kg/cm2g.
7. VV-701 level  High slurry dumping  VV-701  Control slurry dumping rate
High-High rate overflow to and never go beyond 70%
and above VV-702 which level in VV-701.
70% can further
actuate
LSHH7307
causing I9.1:
Distillation
ESD.
Distillation
ESD will
completely shut
down A-700.
8. VV-301 level  LV-2701 opening is  Centrifuge may  Control slurry dumping rate
on higher side. high and high flow of trip on HH level and further reduce opening of
Avoid level slurry from PA-223. of VV-301. LV-2701.
above 60%  LV-3109 opening is  Increase ML flow to VV-701
low and ML flow to if level permits.
A-700 is not  Changeover PA-301 pumps
sufficient. and clean suction spool/suction
 PA-301 pump flow is line.
restricted because of  Attend LT3101/3102 if
suction spool/suction doubtful.
line chocking.
 Flushing hexane may
be opened in PA-301
loop.
 LT-3101/3102
malfunctioning and
PA-301 under
cavitation.
9. Low discharge  High HX makeup flow  More time  Check recirculation valve
pressure of rate to A-200 needed for bypass and close if open.
PA-708 or  PA-708 recirculation Hexane makeup  Check HX flushing opened in
High current valve bypass in open in reactors field in any area.
of PA-708 condition unless flow is
 HX may be opened in high in reactor.
other flushing lines.

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 4.1.2 Time Line during Reactor shut down & Dumping
0 1 2 4 5 6 7
0 0 0
3
0 0 0 0
8
F55 Dumping Task
Description
Ethylene cut off in R-1
R-1 Slurry Dumping 1.5 hrs
R-1 20 Ton Washing 1.5 hrs
HX feed
R-1 HX circulation 0.5
R-1 Washing HX 1.5 hrs
dumping
Ethylene cut off in R-2
R-2 Slurry Dumping 1.5 hrs
R-2 20 Ton Washing 1.5 hrs
HX feed
R-2 HX circulation 0.5
R-2 Washing HX 2 hrs.
dumping
R-1 17T HX intake 1.5 hrs
R-2 17 T HX intake 1.5 hrs

4.2 Washing of Reactors:

1. Take 20 MT fresh washing hexane in Reactor-1 and start HX circulation for 45 minutes, while RB-221
slurry is being dumped. After HX circulation in Reactor-1, isolate slurry cooler, dump washing hexane.
2. After completion of RB-221 slurry dumping, take 20 Ton fresh Hexane in Reactor-2 and start HX
circulation for 45 minutes.
3. After HX circulation in Reactor-2, isolate slurry cooler, dump washing hexane.
4. Feed 17 Ton Hexane in both reactors one by one for plant start-up.

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5.0 Fresh Reactor Batch Start Up:

5.1 Concentration Build up in reactor:

1. Before Ethylene feeding, Initial Hydrogen concentration is maintained in reactor which is more than
normal running condition. Pressure of reactor should not be below 1.2 Kg/Cm2g to avoid RG blowers KA-
201/221 tripping. Initial parameters for parallel polymer grades are as below,

W55A004N
RB-201 RB-221
Initial % H2 Conc. 40% 40%
In reactors

Running %H2 20~25% 20~25%

Conc. In reactors

H2/C2 in vapor 0.45~0.55 0.45~0.55

phase (mol/mol)

Initial Reactor 1.5 1.5

pressure (Kg/Cm2g)

2. Take 17 MT hexane in Reactor (RB -201/ RB-221) through fresh make up hexane line.

Note: In series mode, we can start catalyst feeding in RB-201 before completion of 17T HX in RB-221
considering time margin of 2 hrs. between start-up of both reactors.

5.2 Catalyst (PZ) & Co-catalyst (AT) Feeding

1. Start PZ (Conc. 3 mmol/lt.) & AT (Conc. 200 mmol/lt.) feeding in both Reactors.

2. Start 1 T/hr. HX simultaneously in both reactors for catalyst nozzle flushing till reactor overflow.

3. Catalyst flow rate should be maintained as below:

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 RB-201 RB-221
Ti concentration in reactor mmol/l-Hx 0.011 0.011
Al concentration in reactor mmol/l-Hx 0.5 0.5
PZ catalyst flow Batch lit/hr 27 45
(at conc. 3 mmol/l-HX) Continuous lit/hr 30~45 30~45
AT catalyst flow Batch lit/hr 39 39
(at conc. = 200 mmol/l-HX) Continuous lit/hr 25~35 25~35

5.3 MAPS Settings:

For W55A004N grade, following MAPS (MITSUI AUTOMATION PACKAGE OF SOFTWARE) settings
to be applied:

RB-201 RB-221

% DC 90% 90%

Reactor slurry conc. gm/l-Hx 400 400

Reactor HH temp. trip set deg.C 90 90

H2/C2 Ratio range selection 0~1 0~1

% Co-monomer % 0.32 0.32

Hydrogen FT selection FV-2109B FV-2110B

Co-monomer FT selection FV-2107B FV-2108B

5.4 Hexane Run: Ensure that vessels are lined up as per parallel-A as shown in figure;

VV- VV-
RB-201
202 203
VV- VV-
223 301
VV-
RB-221
222

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 5.5.1 Initiation of Reaction:

1. After 2 hours of catalyst feeding, Ethylene feeding will be started in both reactors simultaneously.
2. Increase RB 201and RB221 jacket temperature to up to 90o C so that reactor temperature stays around
50o C & keep reactor pressure at 1.5 Kg/cm2 and 1.5 Kg/cm2 respectively.
3. Keep RG flow of KA 201/KA221 as low @ 3500 M3/h.
4. Continue PZ catalyst / TEAL/ hexane flow same throughout the process.
5. Observe rise in reactor temperature to confirm reaction is taking place in reactor and then gradually
increase Ethylene flow after reactor temperature reaches @ 60 o C keeping temperature rise ratio < = 1 o C
per minute.
6. Increase Ethylene flow up to 5.0 T/H gradually & keep RB 201/RB221 temperature 85 o C.
7. Maintain reactor H2/C2 ratio during start-up as per sheet.
8. Reactor overflow will come around 40-45 % level of RB201/RB221 @ 2 hours after ethylene injection.

5.5.2 Time line for W55A004N Reaction Start-up:

0 1 2 3 4 5 6 7
0 0 0 0 0 0 0 0 8
W55A004N Start-up
Task Description
PZ feeding in RB-201 35-45 Kg/hr Continuous Mode
AT feeding in RB-201 40 Kg/hr Continuous Mode
PZ feeding in RB-221 35-45 Kg/hr Continuous Mode
AT feeding in RB-221 40 Kg/hr Continuous Mode
Ethylene feed in R-1 5.0 T/hr Continuous Mode
Ethylene feed in R-2 5.0 T/hr Continuous Mode
DC-1 Line up Continuous Mode(MAPS)
DC-2 line up Continuous Mode(MAPS)
Dryer residence time 0.5 hrs
Extruder start-up Continuous Mode

Ethylene Reactors O/F

Feed

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5.5.3 Troubleshooting during Reaction start-up

Sr. Deviation Cause Effect Troubleshoot

No.
1. % Hydrogen PGC Malfunctioning Reactor Hydrogen-  Use standard hydrogen
or % Ethylene or Unavailable Ethylene composition feeding to reactor by
conc. Not because of is not available which observing reactor pressure.
available on maintenance may lead to OFF-Spec
 Standby PGC AI-2401
DCS product
should be taken in line.

2. Reactor  Less Initial  KA-201/KA-221  Increase catalyst feed in

Pressure is Catalyst feed current will reactors if avg. flow is less
rising rapidly  Reaction Kill increase. than required flow.
 PGC  Reactor disturbed  In case of reaction kill,
malfunctioning conditions will increase PZ-AT flow, if no
 Nitrogen Bypass produce OFF-spec improvement observed take
opened product shutdown and do fresh start-
 Reactor pressure up.
HH switch will
actuate POLY-SD
 PGC malfunctioning may
open hydrogen continuously
in reactor. To be checked
 Nitrogen bypass to be
checked.
3. Reaction kill  Impurities in  Reactor temp. will  Increase feed rate of PZ-AT
Ethylene like drop rapidly in reactor
acetylene or CO  Reactor pressure  Keep reactor in venting
 Moisture will increase mode to vent out impurities.
ingression in rapidly  If no reaction improvement
reactors  KA-201/KA-221 observed, dump slurry and
current will rise start fresh after identifying
 Ethylene partial reason of impurity
press. will rise ingression.
4. Reactor  Catalyst  Formation of lumps  Reduce the opening of TV-
temperature concentration is in reactor 2301/2501 to control
rising high  Reactor HH temperature of reactor
 TV-2301/2501 temperature  Open LV-2201/2401 to feed
opening not tripping extra condensed hexane in
optimum as per  Not controlled reactor
load timely, reaction can  Reduce jacket temperature
 LV-2201/2401 run away and  If reaction is not controlled
opening not sintering may by above means, stop
optimum happen ethylene and open vent till
temperature become stable
5. Catalyst line  Flow of PZ in  Low catalyst feed  Catalyst lines should be
chocking W55A003N grade will slow down flushed towards vessel side.

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 is very less reaction and  Never flush catalyst line
compare to series increase pressure of towards reactor side as this
grade reactor will increase sudden increase
flow of catalyst in reactor
and reactor temp. may rise
abruptly
6. Product  Reactor condition  Generation of OFF-  Identify the root cause..
quality are not optimum Spec product

6.0 Probable Deviations and Troubleshooting in Extruder:

Sr. Deviation Cause Effect Troubleshoot

No.
1. Generation of  Vent box chock  Contamination of  Clean Vent-box before start-
Black spotted  Charing of black pellet in up and do whenever it seems
pellet polymer in prime product chocked
extruder barrel  Steam line up for extended
before start-up time may char polymer
initially, take product in OG
silo TI-453. Check pellet
colour and then take prime
silo
2. Generation of  Water Stabilizer  Dull colour pellet  Increase water stabilizer
Dull colour less flow production flow
pellet  Oxygen  After long shutdown,
ingression in Powder may be slightly
powder oxidized, take product in OG
silo
3. Tail in Pellet  Cutter back  Pellet size uneven  Increase cutter back pressure
pressure is low  Tail in pellet  Cutter grinding during cutter
 Cutter grinding assembly replacement should
insufficient be done till even grinding
 Cutter blade worn marks visible on blades
out 

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 7.0 Standard Recipe Sheet at 10 MT/Hr load:

STANDARD RECIPE SHEET FOR GRADE W55A004N

PRODUCT SPECIFICATION

RANGE MFR DENSITY

' A ' QUALITY 0.4 ~ 0.5 0.954~0.957
' B ' QUALITY 0.38 ~ 0.55 0.953~0.958

OPERATING CONDITIONS (reference load 10 MT/hr):

Sr. Parameter Unit RB-201 RB-221

1 Slurry MFR range gm/10 min 0.40 ~ 0.55 0.40 ~ 0.55
2 Slurry blend ratio % - -
3 Ethylene feed for start up MT/hr 5.00 5.00
4 Propylene as wt.% of Ethylene % 0.32 0.32
5 Total Hexane feed MT/hr 8.41 8.41
6 DC % ( theoretical ) % 90 90
7 Fresh Hexane feed (1) MT/hr 1.00 1.00
8 ML recycle - FC-3110/3111 MT/hr 7.41 7.41
9 Ti concentration in reactor mmol/l-Hx 0.011 0.011
10 Al concentration in reactor mmol/l-Hx 0.5 0.5
11 PZ catalyst flow (3) lit/hr 40 ~ 50 40 ~ 50
12 AT catalyst flow (3) lit/hr 45~55 45~55
13 Polymerization Temperature Deg. C 85 85
14 Temperature - High alarm Deg. C 88 88
15 Temperature - Trip setting Deg. C 90 90
16 Total pressure of reactor kg/cm2,g 4~5 4~5
17 H2/C2 in vapour phase (3) mol/mol 0.45 ~ 0.55 0.45 ~ 0.55
18 C2 partial pressure range kg/cm2,g 1.6~2.0 1.6~2.0
19 Slurry concentration gm/l-Hx 400 400
20 Hydrogen FT selection - 2109 B 2110 B
21 Co-monomer FT selection - 2107 B 2108 B
22 H2/C2 ratio range in MAPS - 0~1 0~1
23 Co-monomer Used Propylene Propylene

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