RZ Catalyst

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Standard Operating Procedure
OPaL/HDPE/SOP/100/02
Title : RZ catalyst batch Preparation Plant : HDPE
INTRODUCTION
RZ Catalyst is used as main catalyst. It is mainly titanium tetra chloride (Ticl 4)

catalyst supported on magnesium chloride (Mgcl2) catalyst. Generally known as
Ziegler Natta catalyst. PE-Catalyst (PZ-, RZ- or TE-Catalyst) is charged into PE-Cat.
Feed Drum D-110A/B that has been filled with a specified quantity of hexane
measured by FQ and is agitating the hexane.
From the viewpoint of controlling various polymer properties in polymerizer, the

control of catalyst concentrations is a quite important step. Therefore, it is necessary
to give careful attention to handling of catalyst and adjustment of catalyst
concentration.
REFERENCE DOCUMENTS
1. P&ID NO. : 34-102, 34-103
2. Document No.:
I. 6987-LEPC4-SH-PR-MC-1116_Rev-2 (Operating Manual), (Pages 71 to 73)

II. 6987-LEPC4-SH-IN-LJ-1001_Rev 3 (Instrument Index),(Pages 137,138, 113)
III. 6987-LEPC4-SH-PR-ZY-1113_ Rev 6 (Cause & Effect Diagram),(Pages 5 to
10 and 25)
SAFETY CHECKS
1 Ensure that all operating personal wearing proper PPE’s. FE
2 Ensure that all interlocks are healthy and are in line. FE
Prepared By SUBHODIP DEV Rev. no. 0

Reviewed By P. PRAMANIK Date : 17 May 2014
Approved By SANATH KUMAR :
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SAFETY
1. Route of entry: Inhalation, Skin contact, Eye contact.
2. Effect of Exposure:
Skin Moderate irritation
Eye Severe irritation & chemical burn
3. Emergency treatment:
Inhalation Remove to fresh air, give oxygen,
artificial respiration.
Skin contact Wash with soap water, Wash
clothing.
Eye contact Flush with water
4. Personal protective material:

Rubber or PVC gloves, safety glasses or face shield, Approved respiratory
protection for airborne particle if needed use local exhaust to keep exposure to
minimum.

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ACTION
Sl. NO. JOB DESCRIPTION
BY
CALCULATION FOR PREPARATION OF NEW BATCH
1 RZ catalyst comes as dry powder in drums of around 50 PE
kgs net weight.
The required conc. of RZ batch to be prepared is determined

by the grade to be prepared.
Equation for calculating the RZ-catalyst conc. For

adjustment of PE Catalyst in VV-110A/B is:
F = N * 50 * 103 / 15
Where,
F = Quantity of Hexane to be charged for
catalyst preparation (liters).(1/Batch)
N = Number of containers to be charged.
50 = Average amount of Ti content in one RZ Container

(mol)
15 = PE-Catalyst concentration in VV-110A/B (mmol-Ti/l-

Hexane).
In general for preparation of 15 mmol/l conc. of catalyst

system 6 drums are charged. So the total amount of hexane
to be charged as per equation is,
F= 6 * 50*1000 / 15
F= 20,000 liters
So for each wash 1000 liters of hexane is required. So a

total of 6000 liters of hexane is required for washing.
So, total amount of initial hexane to be charged is,

I = 20,000 – 6*(1000).
I = 14000 liters.

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CALCULATION FOR DILUTION OF A EXISTING BATCH TO A NEW

CONCENTRATION BATCH
1 Say X% level in VV-110A/B of Y concentration is to be made PE
up to Z concentration.
Refer the calibration chart of the vessel VV-110 A/B and find
out the volume of the material to be diluted or the volume
against X% level (say U liters)
Case 1 : Catalyst to be diluted :
RZ cat in X% level= U * Y mmol.
So to dilute to Z conc. the volume will be

V = ( U * Y) / Z
Total amount of fresh hexane to be added is

F= V – U litres
Case 2: catalyst to be made up.
RZ cat in X% level = U * Y * 10-3 mol = T mol.
So, to increase to Z conc. adds one drum of catalyst (50

mol catalyst).
So, total RZ catalyst is 50 + T mol.
So, total hexane required is,

H= (50 + T)/Z * 103 liters
So, fresh hexane to be charged is,
= { (50+T)/Z * 103 } – U
So, at first (total amount -1000) (1000 liters required for

washing of catalyst drum during charging) to be added into
the vessel before charging the fresh drum.

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CATALYST BATCH PREPARATION

1 Please see the production plan and catalyst vessel stock PE
before catalyst batch preparation. Prepare fresh RZ-catalyst
batch in either VV-110A or VV-110B by required no of 50 kg
drums as per target catalyst concentration.
2 Agitate it for 1hr after batch preparation then stop it. PE/FE
3 Running vessel to be used up to dead level after that take PE/FE

fresh catalyst on line.
4 Then fresh batch to be prepared in empty vessel as per PE/FE

batch size instructed by SIC.
5 Except catalyst transfer condition maintain catalyst vessel PE/FE

pressure 0.2kg/cm2 and temperature between 10-20°C
6 Catalyst vessel agitator rpm to be maintained strictly to PE/FE

27rpm during batch preparation.
7 Monitor PSD and BD of powder in every shift. PE

(Note: Do catalyst pump calibration periodically)
PROCEDURE FOR PREPARATION OF A NEW RZ BATCH

1 Ensure that there is sufficient inventory in TT-702 for PE
preparation of a new batch in the vessel VV-110A/B.
2 Line up FQS - 10233 in the field. Note down the initial PE/FE
reading of the Mass Flow meter in the field if it is in
cumulative mode or else if it is in instantaneous mode reset
the flow. Note the initial reading in the log-sheet for new
batch prep.
3 Line up the Mass Flow meter downstream to vessel VV- FE

110A/B (Note the meter is common to vessels VV-110A
& VV-110B).
4 Enter the amount of hexane to be received as per PE

calculation as a set point in FQS -10233.
5 Put the FSV-10233 in Auto mode with the above mentioned PE

set point after resetting FQS -10233 and restarting FQS -
10233.
6 Open the hexane distribution valve for the catalyst area PV - PE

70701 on Auto mode and regulate the flow through the Mass

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flow meter FT-10233.
7 After the total amount of hexane has been received in the PE/FE
vessel isolate the Mass flow meter in the field and close PV-
70701 on manual mode and also isolate in the field.
8 Note down the final Mass flow meter reading and note it FE
down in the log-sheet for new batch preparation.
9 Keep the required number of drums ready at site for PE/FE

charging and enter the drum details in the log for new batch
preparation( REF; log sheet for new batch preparation).
10 Close HSV-10232 and Depressurize VV-110A by setting FE

PICA-10232 at 0 kg/cm2 to 34-EE-104 Auto.
11 Keeping PE-Catalyst container in the normal upright position FE

with the inlet facing upward, connect the low low-pressure
nitrogen line to valve V-1(Refer Drawing in Page 10 of
SOP)
12 Set PCV-10232 at 0.1 Kg/cm2 slowly open V-6, V-7, V-8 PE/FE
and allow low low-pressure nitrogen to flow forward and
thoroughly purge the low-pressure nitrogen line connected
to V-1 with nitrogen. Thereafter, close V-6, V-7, and V-8.
13 Open V-1 and check the internal pressure of PZ-Catalyst FE/FE

container by PG-10212.
14 Remove the blind flange connected at the inlet to the FE

container and during the operation allow some amount of
nitrogen to flow through V-1 to purge the container and not
to allow ingress air.
15 Attach V-2 to the container. Next, close V-2 and V-1. IF the FE
flange on the container and V-2 are found contaminated,
remove such contaminant completely.
16 Purge the piping and flexible hose (34-FH-10204) between FE

valve V-3 and 34-HSV-10232 with nitrogen through PCV-
10232 to VV-110A by opening HSV-10232.
17 Lift up PE-catalyst container with lifting device for PE- FE

catalyst container and set it at the charging point in the
upside-down position. Then connect V-2 and V-3.
18 Fully open V-2, V-3 and 34-HSV-10232 to drop PE-catalyst FE

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into 34-VV-110A/B.
19 Put the vibrator on lifting device into service. Intermittently FE

check the drum is empty or not by knocking the side of the
drum.
20 Open V-1 and supply LLN to the PE-Catalyst container to FE

drop PE-catalyst into VV-110A. It will take approx. 30
minutes. And then close V-1. During this operation, never let
the internal pressure of the container exceed 0.5 kg/cm2.
21 Set FQS-10233 at a specified value of hexane and open V- PE/FE

18, and introduce hexane to the PE-catalyst container to
clean out the PE-Catalyst remaining inside of the container.
It will take approx. 1000 liters of hexane. Maintain hexane
header pressure during drum flushing operation.
22 After hexane cleaning, open V-1 and purge with nitrogen FE

approx. 2 minutes.
23 Close V-1, V-2, V-3 and HSV-10232. Put a blind flange on FE

the upper flange of V-3 after completion of the PE-catalyst
Charge.
24 Open V-4, charge VV-110A with the rest of dilution hexane PE/FE
via FQS-10233. Close V-4 upon completion of the feeding.
25 Set PICA-10232 at 0.2 kg/cm2 to seal VV-110A with PE

nitrogen.
26 Put the agitator for VV-110A in service and also increase the FE
rpm of the agitator to 57 rpm.
27 After around 1~1.5 hours of agitation with 57 rpm sent a FE

sample to the laboratory for determining the RZ solution
conc. In mmol Ti/liter hexane.
28 Set the vessel pressure controller PCV-10232 A/B on “Auto” PE

at a set point of 0.2 KG.
29 After the sampling is over stop the agitator unless the FE

catalyst vessel is scheduled to be lined up within 3 hours.

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TRANSFER OF A BATCH FROM ONE VESSEL TO ANOTHER

1 Pressurize the vessel from which the catalyst has to be PE
transferred using PICA-10232 (Open the bypass valve of the
nitrogen valve PV-10232A to faster the pressurization cycle).
2 Start the agitator of the vessel from which the catalyst has to FE
be transferred.
3 Line up the transfer from the bottom of the vessel of the FE

vessel from which the catalyst has to be transferred to the
top of the vessel to which the catalyst is to be transferred.
4 Line up hexane to the line keeping the bottom valve of the FE

vessel from which the catalyst is to be transferred.
5 After proving the line thoroughness ,open the bottom valve PE

and observe the drop in level of the drum (LT-10232) close
the hexane flushing valve simultaneously.
6 At around 9~10% level of the vessel stop the agitator and PE/FE
observe the drop in level of the vessel, if the drop in level is
reduced close the bottom valve and flush the line with HHX
and reline up the line.
7 When the vessel completely empties out (as seen in the FE

level indicator LT-10232) the pressure of the other vessel
will simultaneously rise and nitrogen will blow through the
line which can be observed in the field. Stop the transfer
operation and flush the line with hexane and isolate the line.
PROCEDURE FOR DILUTION OF A EXISTING BATCH

1 Note the initial reading of the vessel VV-110A and VV-110B. PE
2 Calculate the hexane to be added for dilution to the desired PE

concentration (Ref: Calculation sheet for dilution).
3 Start the agitator of the vessel where the dilution is to be PE/FE

done and run at 57 rpm.
4 After running the agitator for 1 hour line up the Mass Flow FE
meter FT-10233 downstream to vessel VV-110A/B (Note the
meter is common to vessels VV-110A/B.)
5 Enter the amount of hexane to be received as per PE

calculation as a set point in FQS-10233(SP).

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6 Put the FSV-10233 in Auto mode with the above mentioned PE

set point after resetting FQS-10233 and restarting FQS-
10233.
7 Open the hexane distribution valve for the catalyst area PV- PE
70701 on Auto mode and regulate the flow through the Mass
flow meter FQS-10233.
8 After the total amount of hexane has been received in the FE

vessel isolate the Mass Flow meter in the field and close
PV-70701 on manual mode and also isolate in the field.
9 Note down the final Mass flow meter reading and note it FE
down in the log-sheet for new batch preparation.
10 Agitate for another hour and sent sample to the laboratory FE

for analyzing the concentration of the diluted catalyst in
terms of mmol TI/ltr hexane.
11 After the sampling is over stop the agitator if there is no plan FE

of using the vessel in the next 3 hours.
Interlock Details
Interlock No.: I-0441, I-1011, I-1021, I-1022, I-1023, I-1024,

I-1031
** Reference Documents: 6987-LEPC4-SH-PR-ZY-1113_ Rev 6 (Cause

& Effect Diagram) (Pages 5 to 10 and 25)

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Alarm & Trip Setting

Tag Name Description Unit L Alarm set LL Alarm set H Alarm set HH Alarm set
point point point point
PIAS-10201 VV-110A Pressure switch Kg/cm2.g 0.1 0.8
LIAS-10232 VV-110A Level switch % 28 80 82
PIAS-10301 VV-110B Pressure switch Kg/cm2.g 0.1 0.8
LIAS-10332 VV-110B Level switch % 28 80 82
PICA-10232 VV-110A Pressure controller Kg/cm2.g 0.1 0.7
PICA-10332 VV-110B Pressure controller Kg/cm2.g 0.1 0.7
TIA-10232 VV-110A temperature 0C 40
TIA-10332 VV-110B temperature 0C 40
FQICA-10221 Flow control alarm for RZ-cat
FQICA-10211 Flow control alarm for RZ-cat
FQICA-10422 Flow control alarm for AT-cat
FQICA-10412 Flow control alarm for AT-cat

TIA-10705 EE-104 downstream temp. 0C 5
LIA-10770 Level indicate alarm of VV-127 % 89
LIA-10801 Level indicate alarm of VV-101 % 83

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CHK List ––
CHK List
HDPE
HDPE Process
Process Check
Check List
List
HDPE/CK/100/02
HDPE/800/1
HDPE UNIT
PZ Catalyst Preparation
CHECK LIST – FIELD/PANEL
SHIFT : A / B / C DATE : / /
Inform Control Room
all operating personnel are wearing proper PPE’s.
S.N CHECK POINTS YES NO REMARKS
New Catalyst Batch Preparation
01. Line up FQS-10233
02. Note Initial reading of FQS-10233
03. Calculate amount of HX required
04. Arrange number of catalyst container required
for batch.
05. Open PV-70701 for receiving HX.
06. Receive initial HX for batch.
07. Note FQS-10233 reading after initial HX
receiving
08. Depressurize VV-110A/B
09. Connect Catalyst container with V1
10. Open V-6, V-7, V-8, purge LLN to V-1 and
close V-6, V-7 & V-8.
11. Check catalyst container Pressure PG-10212
12. Remove blind of Catalyst container under
nominal amount of LLN purging.
13. Attach V-2 to container. Close V-2 & V-1.
14. Purge the piping and flexible hose (34-FH-
10204) between valve V-3 and 34-HSV-10232
with nitrogen through PCV-10232
15. Connect V-2 & V-3 after lifting Catalyst
container. Open V-1 to charge Catalyst by
LLN.
16. Open V-2, V-3, HSV-10232. Start vibrator.
17. Wash container with 1000Lt of HX by opening

V-18.
18. Purge container with LLN by opening V-1.
19. Close V-1, V-2, V-3 and HSV-10232
(FIELD OPERATOR ) (FIELD ENGINEER) (PANEL ENGINEER)

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CHK List –
HDPE Process Check List
HDPE/CK/100/02
HDPE UNIT
PZ Catalyst Preparation
CHECK LIST – FIELD/PANEL
SHIFT : A / B / C DATE : / /
Inform Control Room
all operating personnel are wearing proper PPE’s.
S.N CHECK POINTS YES NO REMARKS
Catalyst Batch Preparation
20. Put blind between V-2 and V-3.
Repeat step. 13 to step 20 as per container
21. no.
22. Open V-4 for makeup HX.
23. Set PICA-10232 @ 0.2 Kg/cm2.
24. Start agitator of VV-110A/B @ 57 rpm.
25. Stop agitator after 1~1.5 Hr.
Transfer of A batch from one vessel to another

Pressurize the vessel from which the catalyst
01. has to be transferred using PICA-10232
02. Start agitator of VV-110A/B @ 57 rpm.

03. Line up transfer line and HX flushing line.
04. Flush transfer line if required.
05. Stop agitator of transfer vessel
Flush transfer line with HX after completion of
06. transfer.
PROCEDURE FOR DILUTION OF A EXISTING BATCH
01. Note initial reading of VV-110A/B.
02. Calculate amount of HX to be added.

Start agitator of respective vessel and run it for
03. 1 hr. @ 57 rpm.
Open PV-70701 and receive required HX. And
04. close PV-70701.
05. Run the agitator for 1 hr.
(FIELD OPERATOR ) (FIELD ENGINEER) (PANEL ENGINEER)

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RZ Catalyst

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Doc No.

Title : RZ catalyst batch Preparation Plant : HDPE

RZ Catalyst is used as main catalyst. It is mainly titanium tetra chloride (Ticl 4)

From the viewpoint of controlling various polymer properties in polymerizer, the

I. 6987-LEPC4-SH-PR-MC-1116_Rev-2 (Operating Manual), (Pages 71 to 73)

2 Ensure that all interlocks are healthy and are in line. FE

Prepared By SUBHODIP DEV Rev. no. 0

Title : RZ catalyst batch Preparation Plant : HDPE

4. Personal protective material:

Prepared By SUBHODIP DEV Rev. no. 0

Title : RZ catalyst batch Preparation Plant : HDPE

The required conc. of RZ batch to be prepared is determined

Equation for calculating the RZ-catalyst conc. For

N = Number of containers to be charged.

50 = Average amount of Ti content in one RZ Container

15 = PE-Catalyst concentration in VV-110A/B (mmol-Ti/l-

In general for preparation of 15 mmol/l conc. of catalyst

So for each wash 1000 liters of hexane is required. So a

So, total amount of initial hexane to be charged is,

Prepared By SUBHODIP DEV Rev. no. 0

Title : RZ catalyst batch Preparation Plant : HDPE

CALCULATION FOR DILUTION OF A EXISTING BATCH TO A NEW

Case 1 : Catalyst to be diluted :

RZ cat in X% level= U * Y mmol.

So to dilute to Z conc. the volume will be

Total amount of fresh hexane to be added is

Case 2: catalyst to be made up.

RZ cat in X% level = U * Y * 10-3 mol = T mol.

So, to increase to Z conc. adds one drum of catalyst (50

So, total RZ catalyst is 50 + T mol.

So, total hexane required is,

So, at first (total amount -1000) (1000 liters required for

Prepared By SUBHODIP DEV Rev. no. 0

Title : RZ catalyst batch Preparation Plant : HDPE

CATALYST BATCH PREPARATION

3 Running vessel to be used up to dead level after that take PE/FE

4 Then fresh batch to be prepared in empty vessel as per PE/FE

5 Except catalyst transfer condition maintain catalyst vessel PE/FE

6 Catalyst vessel agitator rpm to be maintained strictly to PE/FE

7 Monitor PSD and BD of powder in every shift. PE

PROCEDURE FOR PREPARATION OF A NEW RZ BATCH

3 Line up the Mass Flow meter downstream to vessel VV- FE

4 Enter the amount of hexane to be received as per PE

5 Put the FSV-10233 in Auto mode with the above mentioned PE

6 Open the hexane distribution valve for the catalyst area PV - PE

Prepared By SUBHODIP DEV Rev. no. 0

Title : RZ catalyst batch Preparation Plant : HDPE

flow meter FT-10233.

9 Keep the required number of drums ready at site for PE/FE

10 Close HSV-10232 and Depressurize VV-110A by setting FE

11 Keeping PE-Catalyst container in the normal upright position FE

13 Open V-1 and check the internal pressure of PZ-Catalyst FE/FE

14 Remove the blind flange connected at the inlet to the FE

16 Purge the piping and flexible hose (34-FH-10204) between FE

17 Lift up PE-catalyst container with lifting device for PE- FE

18 Fully open V-2, V-3 and 34-HSV-10232 to drop PE-catalyst FE

Prepared By SUBHODIP DEV Rev. no. 0

Title : RZ catalyst batch Preparation Plant : HDPE

19 Put the vibrator on lifting device into service. Intermittently FE

20 Open V-1 and supply LLN to the PE-Catalyst container to FE

21 Set FQS-10233 at a specified value of hexane and open V- PE/FE

22 After hexane cleaning, open V-1 and purge with nitrogen FE

23 Close V-1, V-2, V-3 and HSV-10232. Put a blind flange on FE