Document MJJa0mzEEDb9ENpM6dBQG0Lbk
\
* ? && X*'J**^
I*
TO BE RETAINED IN STANDARDS DEPT. FILES
Monsanto ConpsiQr
COMPANY CONFIDENTIAL ISSUING of additional copies must
BE APPROVED 7ROUGH THE STANDARDS
STANDARD PROCEDURE.
DEPARTMENT
SUPERSEDED
Bant ..................................................................I Department .Vloy.l...afelorlde.loljmerlzation
Numbnr ..SDP..88-632B.
$2--6^216
............. Sheets
Page.....1.......
Standard Operating Procedures For Opalon Suspension Polymerization
Section 632.0 Process Details for Opalon 600-Series Homopolymers
632.01 Summary
This procedure describes polymerization of Opalon 600 Series PVC homopolymers in 3700gallon glass-lined reactors. Summary of polymerization conditions is attached.
form tat
RSV0028348
ISSUED DEC 6 1968
STANDARDS DEPARTMENT
by d?-
632.o:
Summary of Polymerization Conditions
660 -650'
630
610
600 . * `
*A. Formulation & Measuring Technique
1. VCM
Meter
2. Water-kettle charge Meter
Water-B 1 charge vol. & meter
Water-L2O2 charge
Meter
3. B-l
Weigh
4. C-l
Weigh
5- L2Q2
Weigh
6. DAM
Volume
7. TCE
Weigh
8. Antifoam
Volume
B. Water Temp. During Purge
11,000 lbs. 1700 gal. 130 gal. 200 gal.
7 lbs. 8 oz. 30 lbs. 2 oz. 25 lbs. 5 oz. 1000 ml. None Sterox 110 4 qts. max.
54-61c
11,000 lbs. 1700 gal. 130 gal. 200 gal.
7 lbs. 30 lbs. 2 oz, 25 lbs. 5 oz, None None Sterox 110 4 qts. max.
54-61C
11,000 lbs. 1700 gal. 130 gal. 200 gal.
4 lbs. 27 lbs. 8 oz. 16 lbs. 8 oz. None 50 lbs. Hallco CPH -35N 3 qts. max. 58-61C
11,000 lbs. 1700 gal. 130 gal. 200 gal.
3 lbs. 22 lbs. 21 lbs. None 185 lbs. Nopco NXZ 4 qts. max.
58-61C
11,000 lbs. 1700 gal. 130 gal. 200 gal
3 lbs. 22 lbs. 25 lbs. 5 . None * 308 lbs. Nopco NXZ 4 qts. max.
58-6lC
C. Vacuum Purge, Minutes @ Boil
5
3 < 10 10 10
D. Batch Temp. During L2O2 Addition 49-52C
49-52c
Below 57C
Below 57C
Below 57C
*E. Reaction Temperature
53-1/2 6C
54-1/2C
59-^C
59-1/2C
59-1/2 C
F. Maximum Heat Kick 1. Pull Cold Water-Temp. rise 2. Water Injection
64 c + 1C 57C
64 C
+ 1C 57 c
66C
+ 1C 62C
66 C
+ 1C 62C
66 C + 1C 62C.
G. Final Vent
V ~
50 psig or
Same as 660 50 psig or
Same as
Same as
20 minutes
45 minutes
630
630
after 75psiS
after lOOpsig
H. Agitator Speed, RPM 1. 88 Bldg. 2. 92 Bldg.
92 86
92 86
92 86
g? 86
gf 86
*The exact batch formulation and reaction temperature for each kettle are specified daily by the Operating Supervisor, on a daily instruction card,
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
by ?. &
v
p
p(Dj ro
M Ot? Cr1Oo Cc'oO
C!YO> C'OO CB CO
RSV0028349
Monsanto Company
STANDARD PROCEDURE.
Plant ............
Numb r
D partment ...yirorl..mor.iAe...Sol^erl2atIon ............. Sheets
Page.......?.....
title Standard Operating Procedures For Opalon Suspension Polymerization
632.10 Raw Materials
632.11 Description and Hazards of Raw Materials
The raw materials normally encountered In the polymerization area are listed below with a brief description of the hazards. A more complete definition Is written In Section ll6o, Safety.
1. TCE + high heat (open flame)
2. TCE + caustic
3. L2O2 -1- glycerine
phosgene (highly toxic)
explosive mixture (dichloroacetylpne)
combustible material
4. Calcium Hydroxide (Lime) + L22
Heat and decomposition of l22 + possible fire
5. PDR-1
Doesn*t normally support combustion, will burn under application of heat and oxygen.
6. Caustic
Causes extremely bad chemical burns, es pecially to eyes, exothermic (gives off heat) when dissolved in water.
7. VCM
Extremely flammable and explosive
8. VAc
Flammable liquid and vapors present explosion hazard -- vaporization is slower than VCM.
9. DAM 10. Glycerine 11. TCE
12. L2O2
Not highly combustible
Will burn in presence of oxidizing agent
Not flammable -- store in cool dry place. Explosive at high temeratures.
Extremely flammable -- store in cool dry place. Avoid contamination with organic compounds. Avoid Spillage.
13. B-l ro*M i*
No fire but dust explosion hazard. ISSUED DEC 6 1968
STANDARDS DEPARTMENT
BY
RSV0028350
Monsanto Company
STANDARD PROCEDURE. Plant ...... .Sprlngfleld........................................ Department ...VInXl.Chlpride..Pol^eri TITLE ...Standard, OperatIn&..Proc^^
Number ??..JUffI
...............Sheets
Page.... 4.......
Suspension Polymerization
632.ll Description and Hazards of, Haw Materials (Cont'd.)
l4. C-l
No fire or explosion hazard, but will burn In presence of oxidizing agent. Slipping Hazard. .
15. Calcium Hydroxide
Not flammable, will irritate eyes, nose, etc.
16. pytol
Slightly Flammable, Slipping Hazard
17. Nopco NXZ
No fire. Slipping Hazard
1--1
CD
Sterox 110 19. Hallco CPH-35N
No fire, Slipping Hazard f
No fire, Slipping Hazard
20. Te trahydrofuran
(Solvent) -
High Flammable and Explosive,
Irritates Eyes, Nose, etc.
Must be routinely inhibited to
prevent formation of Peroxides.
21. Methyl Ethyl Ketone (Solvent) -High Flammable, Irritates Eyes,
Nose, etc.
22, Cyclohexanone (Solvent) -
Moderate Fire Hazard, Slightly Toxic Fumes, Irritates Eyes, Nose, etc.
23. Acetone (Solvent) - Highly Flammable, Large Fume Concentrations cause Headaches
form n
RSV0028351
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
BY
Monsanto rjimpawy
STANDARD PROCEDURE.
Plant ......Springfield.........................................
Number
Department ....... .Y*?ZL.9k^
............. Sheeta
Page... l
TITLE ... Standar.a...Qper^Un..PX9cp4ure.8..to..Pp^lpn...usp^n.?.ip.n...P0lym^^iaa.Uon
63S.12 Raw Material Charge Measurement
I
A polymerization log sheet. Form MS-2444, is to be completely filled out with all readings.recorded, A sample of the form Is attached.
632.121 Vinyl Chloride Mopomer Charge Quantity
Dtie to density changes with temperature, it is necessary to correct the VCM volume charge for VCM temperature as shown in the following table:
FORM 1M
Volume for 11,000 lbs, VCM
VCM Temperature
VCM-Volume (gal.)
0 " 1391 1 1393 2 1396
3 1399 4 1401
I 1404 1406
1409
8 1412
9 1415 10 1418 II 1420 12 1423 13 1426 14. 1429
1 1432 16 1434 17 1437 18 1440 19 1443 20 1445 21 1448 22 1451 23 1454
ISSUED DEC 6 1968
STANDARDS DEPARTMENT
RSV0028352
by
Himtin*" Company
STANDARD PROCEDURE.
Plant ............ Sgrlnjgfield.................................... Department ..... ................................................................................. Sheets
Page.
B B~
TITLE ....at8WdLW^...Qp.e^UDg..PxfifeteeA.^OX..tol.Q.Q.,,SW.m0.9.to.^Pl3^y.totlon
632.121 Vinyl Chloride Monomer Charge Quantity (Cont'd.)
Volume for 11,000 lbs, VCM
VCM Temperature
VCM Volume (gal.)
24 1457
25 1459 26 1462 tl 1465
1468 29 1471 30 1474
31 1477 32 1480 33 1483 34 ~ i486 35 1489
632.122 Vinyl Chloride Meter Calibration
Accurate VCM charging Is essential. Hence, VCM meters are calibrated on a weekly basis using the procedures defined in Section 610.10.
632.123 Process Water Charge Quantities
The process water is divided between:
(Si the initial kettle water charge the water used for dissolving and flushing B-l into
kettle
(e) the water used for "delayed catalyst" injection Into
kettle
.
(a) The correct initial kettle water dipstick charges . _ without B-l are:
91-98 Kettles 81-86 Kettles
87 Kettle
73 inches 80-1/2
82-1/2
When the experimental tank in 88 Bldg, is used for B-l, 60 gallons less water is used for the initial kettle
"ifettles
82-1/2 Inches
1SSUED DEC 6 1968
87 Kettle
84-1/2
STANDARDS DEPARTMENT
BY
RSV0028353
Monsanto fjttwpiiy
STANDARD PROCEDURE.
Plant ...... Springfield......................................
Number...SE?. S8-g2B
Department .... yiny0...Chl.Qr4.(le..P.Ol2TOer.laatlon ..............Sheets
Page....I.......
Standard Operating Procedures For Opalon Suspension Polymerization
632.123 Process Water Charge Quantities (Cont'd.)
(b) The B-l dissolving and flushing water charge consists of:
Dissolving Flushing Total
80 gallons 50 gallons 130 gallons
The correct dipstick for the charge water, B-l solution and flush is 4 Inches less than the dipstick readings given above.
For measurement, the 100 gallon B-l tanks are filled to
within 8 Inches from the top of the tank to obtain an
80 gallon charge. The 50 gallon flush is metered into
the tank.
t
(c) For the "delayed catalyst" water injection," a-total of . 200 gal..of water are metered into the catalyst bomb.
632.124 B-l Charge Preparation
The exact amount of B-l Is weighed into a container and the net weight is printed on. the back of the batch log sheet. Since B-l absorbs moisture from the atmosphere, it is important that the supply of B-l be kept in polyethylene lined drums and the drums be covered at all times when not in use. Use only the specified lot of B-l.
632125 C-l Charge Preparation
The exact amount of C-l is weighed into a container and the net weight is printed on.the back of the batch log sheet. The C-l viscosity increases rapidly as the temperature drops .and therefore it is necessary to keep all C-l 55-gallon drums in a warm storage area. Be sure to use only the specified lot of C-l.
632.126 Catalyst Charge Preparation
The exact amount of Lauroyl Peroxide is weighed into a container and the net weight Is printed on the log sheet. Again, use only the specified lot of catalyst.
FORM |M
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
RSV0028354
Monsanto Cnxnjmiy
STANDARD PROCEDURE.
Plant ....Spr.iRgflelfii............................................
Department ......Ylnyl...^^
Sheets
Page
jfjjjp Standard Operating Procedures For Opalon Suspension Polymerization
632.127 DAK Charge Preparation
Small variations in the amount of DAM charged cause significant changes in resin specific viscosity.,. Therefore, the exact volume should be accurately measured in a graduated cylinder.
632.128 TCE Charge Preparation
The TCE weigh tank system is used to accurately charge the speci fied amount of TCE. The weigh tank is filled and the red pointer set at the weight to be delivered. The starting weight (tare weight) and discharge weight (net weight providing starting weight is zero) are printed on the back of the log sheet. (Further details
in Section 612.10)
632.13 Dissolving and filtering B-l
'-
At least two hours before kettle is to be charged, start the B-l makeup. As B-l solution can be held indefinitely, prepare the next batch as soon as the tank Is empty.
1. Weigh the specified quantity of B-l into a B-l container and position near tank. Record lot number on log sheet.
2. Add approximately 20 gallons - 2 to 3 inches above bottom Impeller of hot water - 75 to 90C on tank
thermometer.
3. Start tank agitator.
4. Slowlyvadd the B-l to the hot water over a 1-2 minute period taking care to avoid excessive dusting of the B-l.
5. After the B-l is thoroughly wetted, 1-2 minutes, add cold water until outage is eight inches. Temperature should be below 30C.
6. Record time and solution temperature on log sheet.
7. Allow B-l to mix and dissolve for two hours before filtering. After two hours shut the agitator off to avoid spillage.
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
RSV0028355
Mmuanto Cnmpwy
STANDARD PROCEDURE.
Plant .......Sprlngfield......................................... Department ....nPJl. CM9ri.de..PoljmerlzMlon
Number ........... Sheets
Page...... S....
TTHE ...^feaudard...^pei:atlJQg.,,Pr.oxie(iur.e&..Px)r,,.Qpaloa..Suspenslon..BoXyiBei!,lJsati-on
632.14 Charging Water, B-l, C-l and DAW
1. The Instrument settings to be used during the water charge are as follows:
A. 88 Bldg.
Batch Temperature Controller and Recorder (BTRC) ......................................................................... On Manual
Jacket Temperature Controller and Recorder (JTRC) ......................................................................... 62C.
Charge Water Temperature Controller Set Point .... 58C.
B. 92 Bldg.
/
Batch Temperature Controller and Recorder1 .(BTRC)............................................................................ On Manual
jacket Temperature Controller and Recorder (JTRC) ............................ On Automatic Set Point.......... 70C.
Charge Water Temperature Controller Set Point .......... 74c.
If during the water charge these settings appear to be unsatisfactory, adjust the JTRC set point and/or the charge water temperature controller set point as necessary.
2, When the kettle is ready for polymerization (kettle has been spaced, VCM is available, etc.) start addition of hot charge water.
At the start of the water charge, after the T on bottom of kettle has been filled with water, close the diaphragm valve, and check piping downstream of the Durco plug valve for indication of leakage (pipe would be hot). If pipe is hot, and both valves shut,,notify kettle floor to stop water charge and take action to correct cause of leakage. The dump line check should be made before the start of the vacuum purge.
FORM )*
RSV0028356
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
by
Monsanto Company
STANDARD PROCEDURE.
Plant .... Springfield.........................................
Number
D partmsnt ....Y.tol... Chl.Qrld.e...P.QJksmsr.!;?.& 1 on ...............Sheets
Page...lQ.......
jmjg Standard Operating Procedures For Opal on Suspension Polymerization
632.14 Charging Water, B-l, C-l and DAK (Cont'd.)
3. When water charge is started, charge B-l by:
a. Pressurizing system between B-l tank bottom valve and kettle valve with water .to 30 psig to be sure of no leaks.
b. Pump B-l solution to kettle.
c. Add 50 gallons (metered) of cold water to the tank when 1/5 full to flush out system. Pump out flush water while adding to tank. If a flush of more than -80 gallons is necessarynotify the kettle floor so that a proper adjustment can be made in .the amount of charge water.
When using the experimental B^l tank, the following changes to above procedure should be followed:
a. Have steam on tank jacket while adding hot water to 4 Inches above bottom agitator.
b. Turn off steam before adding B-l.
c. After the B-l is wetted turn on cold water to jacket and add cold water to tank until outage is 4 Inches.
d. After pumping B-l to kettle, shut off pump and add cold water to tank to a level of one inch above the bottom impeller. Pump this flush water to kettle.
4. As soon as both the water and B-l are being added (visually check through manhole)., add C-l and DAM (if required) to the kettle and dog,down manhole cover.
5. Turn kettle agitator on high speed, (92 Bldg, only)
632.15 Vacuum Purging
1. Check all kettle valves, except water and B-l if being used, are closed.
fORM IM
RSV0028357
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
BY
Monsanto Company
STANDARD PROCEDURE.
Plant .......... ..........................................................
Number..
Department ........yiiwl..ChlQrlde..P.?Iyme^ation ............. Sheets rm.p... ;tands^.ipirating..:rocedur^
Page...... 11....
632.15 Vacuum Purging (Conf'd.)
2. Determine and record maximum vacuum controller level. Do not proceed unless level Is less than 3.`5 Inches of mercury. Notify foreman If level is above 3.5 Inches. Water must be flowing through the precohdenser.
3. Open- vacuum valve on kettle; manhole cover must be closed at this time.
4. After adding B-l and the specified volume of water* the batch temperature should be in the desired range (54_6lC*for Opalon 660, 650 or 58-61*0 for Opalon 630 6l0, 600) and approaching a constant temperature. If it is necessary to adjust batch temperature after water and B-l charges are complete, hold vacuum on kettle until temperature is within specified range, then start time.'
(
5. If the kettle contents are boiling, l.e., the vacuum controller is reading less than the theoretical boiling preseure listed below and the actual pressure is not dropping faster than 0.2 inches per minute, hold the vacuum for the specified boil time (5 min. for Opalon 660, 650 or 10 min. for Opalon 630, 6lO,,oOO). If the kettle contents are not boiling, continue to purge.until a boll is reached,and then hold the vacuum for the specified
boll time.
*If the system is under vacuum, complete the water charge -in 88 Bldg, by:
aj closing T-valve above flexible line bl close Durco valve on kettle c) relieve vacuum in water line by opening valve below
antifoam bomb. d) release flexible line.
If water meters are more than 30 gallons apart at end of water charge:
a) shut off vacuum b) break vacuum through water charge line c) opennanhole cover and dipstick.
ISSUED DEC 6 1968 STANDARDS DEPARTMENT lf SS *
by
RSV0028358
Moxunmio Company
STANDARD PROCEDURE.
Plant ..... Springfield........... ............................
Number ...?.PP..8|:63|B
D partment .. Vinyl...Chloride;..Pol^erization .............. Sheets
Page...l2.......
TTTXE ...at.^d.axd..<^exat;log...Pro.Gedy^e.?...Ssr...Ppaion..3.u.?j?gnsion..poijme?:.i^fi^pn
632.1$ Vacuum Purging (Cont'd.)
1
,!
--
ye.
For undercharge of water - add proper amount. For overcharge
of more than 3 inches on dipstick, drain kettle contents to
sewer and recharge.
If only one water meter Is operable, dipstick kettle after completion of water charge before dogging down manhole cover and pulling vacuum.
Batch Temperature
Theoretical Pressure at Boll
53.0C
53.5 54.0 5^.5 55.0
55.5 56.0
56.5 57.0
57.5 58.0
58.5 55.0
59.5 60.0
60.5 61.0
61.5 62.0
4.22 Inches of mercury 4.32
4.43 4.52 4.-61
4.73 4.86 4.98
5.10 -5.20 5.40
5.50 5.60
5.75 5.90 6.00
6.15 6.3 6.45
6. At the end of the boll close the kettle vacuum valve.
632.16 Charging TCE
1. At the end of the vacuum purge, charge the specified amount of TCE from the weigh tank.
2. Print the discharge weight on the log sheet.
FORM 1t
RSV0028359
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
BY
Monsanto {jfiny
*
STANDARD PROCEDURE. 1 Springfield
SDF 88-632B Number.. SDF .iMS.?.?..
Department .......Y.injl ..Chloride...Foljme
.............. Sheets
Page.13.......
T1TIE Standard..Ppe.^atiing,..^ppedures..For..Opalon .Suspension,,Po
%
632.17 Charging VCM
1. After completion of the vacuum purge, and TCE charge (if required) charge all the VCM to the kettle. Do not use any recovered VCM unless directed to by super vision. If recovered VCM is used reclassify batch as defined lh Section 632...31
2. As the VCM is added, the batch temperature will fall off. Allow the batch temperature to drop to 49-52C for Opalon 660, 650, by cooling the jacket water, as follows:
a. BTRC is switched to manual control.
b. JTRC is switched to automatic control.
c. The jacket temperature is dropped to 48-50C at the start of the VCM addition.
d. As soon as the batch temperature fells below 54C switch the BTRC to automatic control and adjust the BTRC set point to reaction temperature. This will, start to heat the batch and prevent the batch temperature from dropping too low when the cold water is added with the catalyst.
For Opalon 630, 610 and 600 control the batch temperature by keeping the BTRC on manual and adjusting the jacket temperature ,to 60-65*0, As soon as the batch temperature falls below 57*0, switch the BTRC to automatic control and adjust the BTRC set point, to' reaction temperature,
3. During the VCM charge, read the VCM thermometer and determine the proper gallonage figure from the chart.
Panes tn
ISSUED DEC 6 * 1968 STANDARDS DEPARTMENT
RSV0028360
Httkawta
STANDARD PBOCTOUBE. Flout .....................................................................
SDP 88-632B Number ...SJQB...92-632b
* ....Vinxl...Chloride.. Pol^grlz
Sheets
TRIE Standard..Operailing..-Pr-on.cdure a.-Enr...Opalon, 3uspenal on ..Pal ymeri gat i on
632.17 Charging VCM (Contd.)
4. When the VCM charge is completed, close the valve at the VCM meter first, then the valve at the kettle to allow the liquid in the vertical line at the- kettle to drain. This will lessen pressure buildup problems caused by thermal expansion of VCM.
5. Keep the Durco T.valve and the Durco -Plug Valve down stream of.the meter open unless.lt becomes necessary to valve off for repairs.
632.18 Charging Lauroyl Peroxide
Before completion of VCM charge/ charge lauroyl peroxide to the catalyst bomb. ;Both the overhead bombs and the bottom kettle bombs are charged in the same basic manner.
1. Make sure water is flowing to the jacketed nozzle on the kettle. Nozzle will build up with PVC if not water cooled.
RSV0028361
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
STANDARD PROCEDURE.
Plant ............. Springfield,
Number
Depaitmul ..YinylJ^hlorlda^Qlymeiilzation
..............Sheets
Page.. .15.......
TITLE ...Stanjaaxd...0perA.tiAg..r.QC.edurja3...F.Qr...0pal.Qn...SwSP.ens.ipn..^oly7nerizatipn
632.18 Charging Lauroyl Peroxide (Cont'd.)
2. Weigh out correct amount of lauroyl peroxide into container and position near bomb. Record the lot number on the log sheet.
3. Pour lauroyl peroxide through funnel into bomb.
4. Add water to bomb until level reaches the base of funnel valves to displace extra air from the bomb.
5. Close the funnel valve, then close water injection valve.
6. Upon- completion of the VCM charge check the batch temperature before charging lauroyl peroxide. For Opalon 660, 650 the temperature should be below 52aC, for Opalon 630, 610, 600 it should be below 57C.
7. Open fully the high pressure water line to the catalyst bomb. Bomb pressure must be above 175 psl.
8. Chec'k bomb to make sure there are no visible leaks,
9. Open valve between bomb and kettle.
10. Meter in the specified amount of high pressure water. 250 + 5 gallons for Opalon 660, 650 or 200 + 5 gallons for TJpalon 630, 610, 600.
11. First close valve between bomb and kettle.
12. Then shut off high pressure water.
13. Slowly bleed off'bomb pressure to drain line.
^
14. Open funnel valve and drain bomb.
632.20 Polymerization
632.21 Reaction Temperature Control
1. As defined in Section 632.17, Charging VCM, both the BTRC and the JTRC are on automatic control.
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
BY
RSV0028362
Mnmntii ^nyr
STANDARD PROCEDURE. ____ Springfield
ram ............ ..................................................................
Dvpartmaiit
Number
SDP 88- 632B .... 9" 632b
.Sheets
Page.. 16
TTHE ..5^d6J?(l..Dj^ra,ting...Er.0.<?.e.dW.ea..F.Qr....QB^0R..Suspe.QBion..]polirmeri2atipn
t,,
632.20 Polymerization (Cont`d.)
632.21 Reaction Temperature Control {Cont'd.)
2, Hie reaction temperature Is controlled at the exact specified temperature (defined on Instruction Card),
632,22 Instrument Setting
1, The'correct Instrument settings are defined below. Any deviation should be Immediately reported to Foreman,
f
Batch Temperature Controller and Recorder (BTRC) ... On automatic Proportional Band ................................. ............... 18 - 20 Reset ........................................................... ..................................... 10 Derivative ......................................................................... ........... 10 Set Point ................................................ *...................... at reaction temp.
Jacket Temperature Controller and Recorder (JTRC) ,,, On Automatic
%Proportional Band .............................. ............... ...................... 10 Pneumatic .................................................................................. 50
2. The correct instrument charts to be used are:
Batch Temperature Recorder and Controller (BTRC) .. 898523 - 88 Bldg. & 808629A - 92 Bldg
jacket Temperature Recorder and Controller (JTRC).. 898423
Vacuum Purge Controller
892282
632.23 Heat Kick Control
1. When the batch"temperature starts to rise during the heat kick, start full cold water at one degree above the reaction temperature.
2. Start water Injection for Opalon 660, 650, at 57*0. For Opalon 630, 610, 600 start the water injection at 62*C. Use the minimum quantity of water possible. Do not exceed 500 gallons.
FORM IM
RSV0028363
ISSUED DEC S 1968 STANDARDS DEPARTMENT m
Springfield
92-632B
632.20 Polymerization (Confd?
632.23__ Heat Kick Control (Cowt'd)
3. Turn off water injection at 2C below reaction temperature. Do not knock batch temperature too low.
4, Should reaction temperature rise again, water inject again at the temperature specified in Step 2 and add only the remaining volume of water. Do not exceed a total of 500 gallons of water for all combined injections.
5. If heat kick cannot be stopped and reaction temperature reaches 66C start the final vent immediately. It is important that the batch temperature be prevented from reaching 70C to prevent partial batch coagulation. Having started the final vent, complete the operation and downgrade the batch according to instructions in Section 632.31
6. Near the end of the cycle, the pressure will start to drop off. When the batch temperature is under control:
. a. Shut off full cold water.
b. Switch BTRC to manual
c. Control the jacket temperature - manually - so as to maintain the batch temperature between 50 to 57C during the entire final vent.
ISSUED DEC 6 1968 STANDARDS DEPARTMENT BY
RSV0028364
Springfield Vinyl Chloride Polymerization
___
SDO 88-632B
92-632B II
Standard Operating..fxj^Q.^.u.^x.^.J.gr..-Qx>^j^..,,?.UgJfeD.$iP-D..-Qlymer.iza.tion
632.24 final Vent
1. Begin the final vent at 50 psig or 48 minutes after.100 psig, whichever comes first. (Note: for 660 or 650, begin vent at 50 pai or 20 minutes after 75 psi, whichever comes first).
2. Listed below are the recommended antifoams along with the alternat antifoams and the maximum amount of each which can be used. Note that the alternate antifoams are not as effective and are to be used only if the recommended antifoam is not available.
Product Recommended Antifoam Max. Amt. Alternate Antifoam
OP. 660 650 630 610 600
Sterox 110 Starox 110 - Hallco CPH-35N Nopco NXZ Noecp NXZ
4 qts. 4 qts. 3 qts. 4 qts. 4 qts.
Hallco CPH-35N
Hallco CPH-35N Sterox 110 Hallco CPH-35N Hallco CPH-35N
3. Prior to starting final vent, add one gallon of antifoam to antifoam boobs.
Max. Amt.
a3 qts
3 qts 4 qts 4 qts 4 qts.
4. Pressurise antifoam bomb with nitrogen. Boob pressure should be 10 psi higher than kettle pressure.
Note: Make sure bomb pressure is 5-10 lbs higher than kettle pressure during vent.
5. One minute before starting final vent, open antifoam valves to kettle for continuous addition during vent.
6. If foaoing occurs, slow down rate of venting.
7. Do not exceed maximum amount of antifoam allowed.
8. After final vent is completed, drop jacket temperature to 45C
ISSUED DEC 6 1968 4|
STANDARDS DEPARTMENT ^
RSV0028365
Monoanto
y STANDARD PROCEDURE. Plant .........Springfield....................................
Number
SDP 88-632B 9922--- 6-3 g
Department ....yii^l..CJal.Qrl(l?...P.Qlxm8rIzation
Page....?.?.....
TiTT-F. St^dard Ope^
Opalon Suspension Polymerization
632.25 Emergency Action
If for any specific reason there Is danger of a set-up batch, add one gallon of styrene monomer to the kettle via the antifoam bomb. Specifically, styrene injection should
be employed for the following conditions:
1. Power Failure - See Section 637.0 Emergency Procedure; (add 1/2 gallon of styrene monomer to each batch).
2. Water Failure - same as above.
3. Mechanical Failure of Equipment Causing Loss of Agitation If for any reason (such-as seal leak, spark generation, motor.overload, excessive vibration.at both high and low speed agitation, reducer failure, belt breakage) it becomes necessary to stop agitation, immediately add 1/2 gallon of styrene to the batch.
If repairs cannot be effected In 30 minutes, vent off remaining VCM with batch temperature reduced to 35-40C. If repairs can be completed, start up agitation (by Jogging agitator on-off) and complete batch polymerization.
5v Suspending Agent Omission or Failure - If the B-l charge is accidentally omitted (or only partially charged) or if the B-l suspending agent,is destroyed by an impurity -- such as caustic -- batch set-up will occur. An early indication of this problem is a sudden drop in the
Jacket water temperature after only 4 to 5 hours of polymerization. A heat kick will follow immediately,
. with these symptoms, add 1/2 gallon of styrene to the batch.
6 Discretionary Action - If for some reason-batch temperature
and batch pressure show.abnormal performance, contact
kettle foreman. If he cannot be reached and it is your opinion that a set-up batch may occur, add 1/2 gallon of styrene to. short-stop the reaction.
632.30 Dumping Batches
632.31 Reclassification of Batches in Kettle
1. Downgrade to Code 6 (Technical Crade) for the following reasons;
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
RSV0028366
Monsanto Company
STANDARD PROCEDURE. Plant ...................Springfield..........................
Numb r....^
D partment ....Vinyl.. Chloride. Polymerization ............... Sheete
Page.... 20
Standard Operating Procedures For Opalon Suspension Polymerization
632.31 Reclassification of Batches in Kettle (Cont'd.)
1. a. Batch is mischarged.
t>. Agitator is off more than 15 minutes after the L2O2 charge has been started.
c. Recovered VCM is used.
d. Heat kick exceeds 64C for Opalon 660, 650, or 660C for Opalon 630, 610, 600.
a. Particle size is obviously too coarse.
632.32 Segregation of Batches
1. Complete wash-out of lines and slurry tanks is required between all product changes; l.e., going from 650 to 630, 660 to 650, etc.
2, Code 1 (A-grade) and Code 6 (Technical-Grade) are normally kept completely.segregated. .If it becomes necessary to dump a Code 6 batch into a partially full tank, then the entire contents are Immediately downgraded to TechnicalGrade .
632.33 Dumping Batches and Flushing the Kettle
A. Opalon 660, 65Oj 630
1. .Line up kettle to be dumped to correct slurry tank.
2. Start up dump pump on water and check line for clear, unobstructed .flow.
3. If necessary, clear resin chips from dump strainer and tank strainer before starting slurry flow.
4. Two men will station themselves at the kettle to be dumped-one on the kettle floor and one at the dump valve. They will both confirm that the correct valve Is being opened, before the dump valve is turned.
FOItM 126
RSV0028367
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
BY &&
Monsanto Company
^
W
STANDARD PROCEDURE. .........SK!S*^2y-...................................
Number
D partment .Vinyl..Chloride,.Pol^erlza
.............. Sheets
page. 23,.......
pnXE Standard Operating Procedures For Opalon Suspension Polymerization
632.33 Dumping Batches and Flushing the Kettle (Cont'd.)
A, 5.
Start dump as follows:
a. At batch pressure of 0 psig and with line to atmosphere closed, open dump and shut off water to pump.
b. As batch level drops, the pressure in the kettle will decrease. When pressure drops below 0 psig, open line to atmosphere.
c. Ten minutes after the line to the atmosphere is opened, < open the kettle manhole.
6. If normal dumping is not possible due to plugged dump line, use ''Siphon Unloading Technique", Section 639-70-
7. When.the slurry level is such that the agitator blades are plainly visible (600-800 gal. slurry left), stop the agitator and place the Sellers rotojet in position. Pump 600 gal. of high pressure water through the Jet. Be sure Jet rotates and that the backs of the baffles are covered by the spray.
NOTE: <
Considerable attention must be given to cleaning out all loose polymer before proceeding with next batch. Residual polymer will result in an out-of-spec batch.
8. After 600 gal. of water have been flushed, stop Jet and insnect kettle. If no slurry remains, direct flow from kettle to sewer. .Start agitator and flush the front of the baffles and agitator (turning)^ using the high pressure
water hose for 2-3 minutes. Make/sure all loose resin 3s out of the kettle since even a handful of loose PVC will result in a high out-of-spec resin flsheye level.
NOTE:
If slurry remains in the kettle after the Sellers flush, pump this to the slurry tank. When kettle is empty, direct flow to sewer and proceed with high pressure water flush for 2-3 minutes, being especially careful to flush clean the bottom of the kettle.
RSV0028368
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
by
Monsanto Company
STANDARD PROCEDURE, plant .......Springfield..........................................
Nmnber..???...8^||
Department ....X^L Chlpr^
.............. Sheets
Page.. 22......
Standard Operating Procedures For Opalon Suspension Polymerization
632.3-3 Pumping Batches and Flushing the Kettle (Cont'd.)
A. 9. Line to and from the pump should be flushed 2-3 minutes after dump to prevent plugging.
10. It should be noted that meticulous kettle cleaning on a scheduled basis is necessary to prevent excessive kettle
buildup which contributes to high fisheye level resin.
B. Opa-Ion 610 and 600
1. Line up kettle to be dumped to correct slurry tank. e
2. Start up dump pump on water and check for clear, unobstructed flow,
3. If necessary, clear resin chips from dump strainer and tank strainer before starting slurry flow.
4. Two men will station themselves near the kettle to be dumped - one on the kettle floor and one at the dump valve. They will both confirm that the right valve is being opened, before the dump valve is turned.
5. Start dump as follows:
a. At kettle pressure of 0 psig and with line to at mosphere closed, open dump valve and shut off water to pump.
b. As batch level drops, the pressure in the kettle will decrease. When pressure drops below 0 psig,
open line to atmosphere.
c. Ten minutes after the line to the atmosphere is opened, open the kettle manhole.
6. If normal dumping is not possible due to plugged dump line, use `'Siphon Unloading Technique", Section 639-70.
7. After the dump has been completed (no slurry remains in kettle), flush the kettle with high pressure water for 2-3 minutes in the following order:
ISSUED DEC 6 1968
STANDARDS DEPARTMENT
RSV0028369
bv
Monsanto Company
STANDARD PROCEDURE. Plant ...... Sp-ingj'i'nd.................... ..................
Numb r......fEfJfcll!!
Department ......Yinyl.Chlori^
............. Sheets
Page..... 23....
title.... S.:t&n.dar4...Qp.er.3.Ur^..i:;c.Q&edurs..^^
632.33 Dumping Batches and Flushing the Kettle (Contfd.)
B. 7. a. Dome - especially pop valves and catalyst nozzle.
b. Agitator Shaft - running
c. Baffles
d. Walls
8. Flush line to and from the pump 2-3 minutes after dump to prevent plugging.
SPECIAL NOTES:
1. Because #4 Kettle, 88 Bldg, has a raised lip on the dump nozzle, resin is not easily flushed out. Therefore, after Sellers cleaning and hosing the front of the baffles, connect the charge water line to the kettle and add approximately 200 gallons of water (100 gpm) to create enough turbulence to
cflush out the residual resin retained by dump nozzle.
2. Sellers flushing results in a large amount of dilution water being introduced to the slurry hold system. This normally will be no problem; however, when slurry hold tank capacity is limiting kettle production, flush the kettle with the Sellers after the batch has dumped, and direct all the flush water to the sewer.
3. If a kettle is Sellers flushed while the batch is dumping, do not add any dilution water to the slurry hold tank for that batch -- none required.
RSV0028370
ISSUED DEC 6 1968 STANDARDS DEPARTMENT BY
Monsanto Company
STANDARD PROCEDURE. Plant ........ Springfield.....................................
aNumber SDP |-J1
D paztnwnt ...................................................................................... .Sheet.
Page.... 24 ..
TITLE....5.t.and.er.d...Qp.e.r,eSln..P.rpceduresFor..ppal_on_Suispen3il9n_PoljTnerl2atlon
632.90 Process Adjustments
Mils section of the procedure is to assist operating supervision in making normal process adjustments.
632.901 B-l Concentration
The following are recommended charges for the start of an X-70 product run, based on B-l cjrarge being used In X-75:
X-75 Product (660, 650, 669)
B-l Charge,,
630 B-l Charge
600-610 B-l Charge
N
O 00
*tfe
CXI
Less than 6# 6# to 7# More than 7#
3# 8 oz. 3# 12 oz. 4# 0 oz.
2# 12 oz. 3# 0 oz.
Make all X-70 process B-l adjustments in 4 oz. Increments.
Reference: r, Carney 10/24/68 Supersedes SDP 88-632 A issued 4/22/64
92-632 A
po*m ia
RSV0028371
ISSUED DEC 6 1968 STANDARDS DEPARTMENT
BY
g5 3[S\
OPERATING LOG
DEPARTMENT 88
ua rt
pi;, n
1 KETTLE NO. joATCH NO.
OPERATOR RESIN TYPE*
POL'.MER I ZAT ION 5Rnd NUMBER
L22
AMOUNT
LB,
OLEND NUMBER
,1
8-1 RSunT
LB.
BLEND NUMBER
C-1
AMOUNT
LB.
LEND NUMBER
DAM
AMOUNT BLEND NUMBER
LB.
TCE
AMOUNT OLEND NUMBER
LB.
VCM
PROM TANKS TiTMiF
AMT. VIRGIN.
AMT,REC.VCM
PRODUCT CODE
OZ. OZ,
VACUUM PURGING
yesQno
IS WATER FLOWING TO PRE-COND? 0YSQNO
TIME B-l CHARGED
TIME C-l CHARGED
VALVES TO PRE-COND OPEN? BY PASS VALVE TO PRE-COMO OPEN?
STEAM TO NORTI|/eaST JET ON?
vesQno
__ _
LI LJ
QQ
TIME L2O2CHARGCO TIME DAM CHARGED VACUUM PURGE STARTED
OZ, OZ, OZ.
STEAM TO SOUTH-WEST JET ON? Q
Q
ARE ALL VACUUM VALVES POSITIONED
VACUUM PURGE COMPLETED TCE CHARGED
MAXIMUM VACUUM READING
T (ME
BATCH TEMP.
THEO.PR.
IN VCM CHARGC STARTEO ACT. PR. VCM CHARGE COMPLETED
IT I ME BTC SWITCHED
REACTION TEMP.
0 r
GAL.
TIME FCW ON TEMP.WHEN FCW ON TIME W.I. STARTED
GAL,
TEMP. WHEN V.1. STARTEO
RSV0028372
B-1 SOLUTION MAKC-UP & FILTRATION
AMOUNT V.1.
TANK NUMBER
HIGHEST TEMP. DURING H.K,
TANK HOT WATER TEMP.
TIME 8.P. AT 100 PS I
:>
c
c c
.
TEMP. AFTER COLD WATER TiME 8-1 MADE UP LINES PRESSURIZED BEFORE CHARGE? TIME TO CHARGE 0"1 SYSTEM PLUSHED?
KETTLE WATER CHARGE TIME WATER CHG.STARTED
TIME WATER CHG.COMPLETED
M1N
T HE
TIME FINAL VENT STARTEO
HOURS BATCH READINGS
TIME FINAL VENT COMPLETED
BATCH
BATCH
-- TEMP. AT ENO OF FINAL VENT JACKET
TEMP.
PRESS.
TEMP.
AMOUNT OF ANTIFOAM USED
TIME BATCH OUMP STARTED
TIME BATCH DUMP COMPLETED
SLURRY DUMPED TO TANKSj? COMMENTS:
------------- ^---------QTS
METER RDG.
DIPSTICK
WATER TEMP.
WATER TEMP.SET POINT
IN ,,
C
f.
APPROVAL SHEET CSi 8
SDP 88-MKMM- g1aft nats: October 24. 196B
Please check the attached procedure or specification and sign it if it meets with your approval. If you have any sug gestions, corrections, or add itions please note them on this sheet: DO NOT WRITE .ON SPECIFICATIOJf'OR PROCEDURE, Then detach one "RETURN TO STANDARDS DEPARTMENT" slip and return it under separate cover.
Please give this your immediate attention: REMARKS: (Please initial)
RSV0028373
DISTRIBUTION RSV0028374
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RSV0028375