Document e77MYx6BoJoORarkXMOqXLNam
3 3274 I 59 ' '
^MONSANTO CHEMICAL COMPANY^ *
Plastics Division MAb 1 LK LUr I
Limited Procedure for Process Modlflcat1! on... -..---
TO BE RETAINED IN
quested by .. .4* .E* .mwiWTQ o e e> e e o c
STANDARDS DEPT. FIL! Number . . . .Do0-53 0 6
Technical Supervision and Reporting By . . . .A* .E*
Plant
oeco
Product Group ...
o
6eoeo*PO04&
__P. T ,, S. Supv. Eng,,.
8/11 R.A. Coffey
Plant Dept. No . ...94',. coeccoooeocccooo Research Gro. Lead. 8/11 A.W. Coaker/REP
Limited to: Amt. of Material ?9J.999^^ 0uer. Sunt.
Gen. Mfen Suot,, or Expiration Date ............ P.T.S- Manager
8/11 R.K. Perry 8/11 R.I. Dunlao
Modification of SDP
....... Standards Dept.
3/12 A. 0. Ericksberg
Reason for Requested Variation
Approval required when segregation
To manufacture a low viscosity resin
of expense is specified.
for evaluation in 85 bldg, calendering operations.
jssued/AUG 12 1960
STAN DARDS'DERARTMENT
BY (dP (jl
Details of Modified Procedure (1) See attached TOP for "Experimental Line" operations.
(2) The "Opalon X-62 TOP" will be modified by the use of 0.2$ GMS and an increas increased final vent in order to Improve resin porosity and initial color.
(3) Target Specifications Specific Viscositj^:
Dry Time: Contamination:
Moisture: Particle Size:
0.29 to 0.33 12:00 max, (Read Mixer)
8-45 max.
0.3 % max.
Trace Max. on 40 Mesh
Reference to Previous Work
1. Pinal Report II PVC Resin for Rigid Sheeting", Job No. 1583
C.G.McCubbin, May 19, 1954
RSV0026402
Safety Hazaras and Precautions (Including Toxic
3 Use protective equipment when handling TCE.
Product T sting Required and by Whom
Control Lab. - Specific viscosity, drytime, contamination, moisture, particle size, Robbin color, and heat stability.
Identification and Disposition of Material
Segregation of Product Labeling of Product Approval for Shipment
Keep segregated Plain bags, lot number only PTS (A.P. Tarrenzano, R, Coffey)
Costs
A. Estimated effect on manufacturing costs, if successful
Opalon X-62 - 12.440/lb. as compared to Opalon Xr70 - 12.30/lb, Opalon X-69 - 11.90/lb. Op Susp Res 12. 40/lb.
B. Estimated extra manufacturing cost of this experiment
Negligible
C. Segregation of Costs (by Operating Superintendent)
BNo segregation of Costs required Special Accounting number will be required D. If costs are segregated, accounting number assigned (by P.T.S. Manager) P/P.- P.2.................
Informational Copies to: (To be filled out by Standards Department)
Plant Laboratory Supervisor Planning and Control Supt. Marketing Technical Service Mgr. Qeneral Mfg. Supt. P. T. S. Manager Accounting Dept. Pruciuct Administrator Research Section Leader Overseas Mfg. Dept.. . Other Domestic Plant* Foreign Plants
L. E. Louraine J. D~^~Hincher) ___C. E. Hamlin
--3L-E--AlUiS IJualau____________________________
___J- M. Crabtoae. - P..Pas t.us.zalc_.
__ R^-E^-Clark ___1. P. Cohen __ I-L-F,.. Amstmg!
.. Ei M^u; ___Oparatlng-Supervlaor. - ,T.... SbEiv.ei-
Other 5 3274 (back) 1/59
&SV0026403
Tentative Operating Procedures
Opalon X~62
August 12, i960
The procedure described below will be employed to manufacture two batched of modified Opalon X-62, a low viscosity homopolymer resin for evaluation in 85 Bldg, calendering operations.
Briefly, the modifications include the addition of glyceryl monostearate,
GMS, and a lower conversion level, approx. 87`^j in order to improve the
m resin porosity. The 1$ trichloroethylene in the formulation is used to obtain a 0.30 specific, viscosity at the 60C reaction temperature.
I, Batch Formulation
Raw Material
Parts
Weight
Water VCM PDR-1 GMS
L2O2 TCE
135 100
0.15 0.20
0.15
0.99
14,850 lbs. 11,000 lbs.
16.5 lbs. 22.0 lbs.
l6.5 lbs. 108.9 lbs.
Charging Raw Materials
1. Charge 1700 gallons of water to the kettle at 54-56C. Correct dipstick outage is 75 3/4 inches.
-
2. Start up kettle agitator. Adjust agitator speed to 121 RPM (approximately 7.7 rheostat setting on the
variable speed controller)
3. Filter the PDR-1 solution into kettle.
4. Add the GMS and L2O2 solids.
5. Close manhole and draw a 24" vacuum purge.
6. Add TCS using kettle vacuum to draw in material via a straw arrangement.
7. Adjust instrument set point to 60C and switch instrument to automatic control.
RSV0026404
p_
8. Position the Reset Cut-Out controller to the manual position using a 13.5 psi bias level.
9. when temperature has leveled out, switch Reset Cut-Out to the automatic position.
III.
Polymerization 1. The reaction is held at 6oC for the entire cycle.
2. After approximately 8 hours the batch will heat kick. Use full cold water at 6lC and water injection' at 62C,
3. Start the final vent when the pressure has dropped to 115 psi.
4. Vent the unreacted VCM to the gasholder as rapidly as possible without foam carry-over. Use sterox 110 antifoam if necessary.
5. Take a two gallon sample of the slurry.
6. Dump batches into a cleaned #1 slurry tank. Dry as a two batch blend.
IV. Centrifuging and Drying.
1. The No. 1 dryer is to be cleaned out thoroughly before starting to dry Opalon X-62.
2. Operating Conditions:
a. Centrifuge - Feed compartment - #3 Pool depth - #5 Feed rate ~ as necessary to maintain dryer temperature Wash water - none Dilution water - 10 gprm
b. Dryer - Retention ring - none Outlet air temp. - 1S0-155F (64-66c)
' Inlet air temp. - 280-310F (136-153C)
Air velocity - 100 FPM
3. Line up equipment for direct bagging.
l-\, Package material using plain bags marked only with lot number
5. Take a 5 lb. bag sample from each blend.
#
RSV0026405
f*
MS' 3274'1/59
MONSANTO CHEMICAL COMPANY Plastics Division
Limited Procedure for Process Modification
Requested by .
, W`.tV....... e> o o O c
Number
t^OfCl^Oj?O, CO3'1
Technical Supervision and Reporting By ... Ra
..
Plant
000040000000000
Product Group .
pe&e06OffPo*6c*e
' JB .T,,S. Sudv,, Eng,,
siJio
yi-
Plant Dept. No ..
. 0000000*4**004**. Research Oro,, Lead.. AM Lr
t c'} fl'W Limited to: Amt. of Material
Oner. Sunt.
o<
tl'h*
Gen. Mftt. Sunt. ...
or Expiration Date . 0*0404*40 *P.T,,S- Manager Modification of SDP ,?&AW\ .x:... 0*0*. Standards Dept,, ....
t /'
UCjfj/Q/S- ....
/ / -7 // , / "V'' /t; A f-
//A-i
J
Reason for Requested Variation
\o v1 F ft, ci U'CL'fi- ft, Vou) M'iC o i,\4v^
Approval required when segregation of expense is specified.
Vofft ftUj &X\ (ftft \U SS
CftWcSiWw^ G^iCAO it tfVA .
Details of Modified Procedure "
^ Sttt ftA4fc.cwe.fi "TOP
*
i ,,
w-^ '
(ft) ~\c
y-L-z- TO? LoV\\ W ho&yV\i& Wj 441
twCA-.Q ^e_(D
OIUa.A vvi ooi'^v -V>
oye. <s>r o.i-% <5h^ WS>10
\ Vj \4fA
c.o\A-.
O'! IftCLfeftT <<. v<,, t^v\5
'JvbcoV'ly.
o. 4j o. Vb
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\1'.CQ Hfe*. ( t? cA h'w=0
Cov4(\t^\uj k
^ - 4-5 M ft*
O .li 9ii> nfcw
Pft<zAcW S^c '
\ lift ce Mfey- oti
Reference to Previous Work
v. "hi C eeso Td4 vU \?'b
\'
fc'fe'O s u.n (wej , C$. HcCtibSjuj
, fC] &
RSV0026406
Safety Hazards and Precautions (Including Toxlcltt" Air, and Steam Pollution)
(JmAc<_X< \j
\ V&/-A UiVt^A ViAt-i
T^C.
Product Testing Required and by Whom
C*vV\cA
J vA^
(<j^sWk) Cfelcw (ivj^ V\e_cl\ cViitoi'l>!-, .
Identification and Disposition of Material
Segregation of Product Labeling of Product Approval for Shipment
5 CC^tC-Gi ft 1-e.
\jsrr w o rOfc ca
PT1> <V$. "T&C.aC vT-kAvlO >
)
Costs
A. Estimated effect on manufacturing costs, if successful
vt-t'S. --
\2.AA- \/i,
ctsw^aw*. <Sw 4*
Of*U vio - w i <t(u,
OfAi^ X*t^ - l\- 1 l/Ua
Of 5ulp Cts. - ~4-
B. Estimated extra manufacturing cost of this experiment
Vle^U gaU<_
C. Segregation of Costs (by Operating Superintendent)
B1/
No segregation of Costs required Special Accounting number will be required
D. If costs are segregated, accounting number assigned (by P.T.S.
Manager) .. A1A . LJ. A;.
Informational Copies to: (To be filled out by Standards Department)
Plant Laboratory Supervisor
Planning and Control Supt.
Marketing Technical Service Mgr.
General Mfg, Supt.
''
P, T. S. Manager
Accounting Dept.
Product Administrator
Research Seotlon Leader
Overseas Mfg. Dept.
Other Domestic Plant*
_ ___________ _
_ ' ^
_________________________________
Foreign Plants
...........
Other MS 3274 (back) X/59
____________ ___________________________ . ---------------------------------------------- RSV0026407
I Tentative Operating Procedure
Opalon X-62
tegt is,,12.60
The procedure described below will he employed to manufacture two batches of modified Qpalon X-62, a low viscosity homopolymer resin for evaluation in 85 Bldg. calendering operations.
Briefly, the modifications include the addition of glyceryl monostearate, QMS, and a lower conversion level, approx. 87$, in order to improve the resin porosity. The 1$ trichloroethylene in the formulation is used to obtain a 0.30 specific viscosity at the 60c reaction temperature.
I. Batch Formulation Raw Material
Parts
Weight
Water VGM PDR-1 QMS <202 TCE
135 100
0.15 0.20 0.15 0.99
14,850 lbs, 11,000 lbs,
16.5 lbs, 22,0 lbs. 16.5 lbs. 108.9 lbs.
Charging Haw Materials
1. Charge 1700 gallons of water to the kettle at 54-56C. Correct dipstick outage is 75 3/4 Inches.
,, Start up kettle agitator. Adjust agitator speed to 121 RFM (approximately 7*7 rheostat setting on the variable speed controller).
3. Filter the fdr-1 solution into kettle.
4. Add the QMS and L2O2 solids.
5. Close manhole and draw a 24" vacuum purge.
6. Add TCE using kettle vacuum to draw in material via a straw arrangement.
7. Adjust instrument set point to 60*c and switch instrument to automatic control.
RSV0026408
-2-
8. position the Reset Out-Out controller to the manual position using a 13.5 psi bias level.
9o When temperature has leveled out, switch Reset 'Cut-Out to the automatic position.
III. Polymer!z&tion 1. The reaction is held at 600 for the entire cycle 2. After approximately 8 hours the batch will heat kick. Use full cold water at 6lwc and water injection at 62C. 3. Start the final vent when the pressure has drooped to 115 pel. 4. Vent the unreacted YCM to the gasholder as rapidly as possible without foam carry-over. Use Sterox 110 antifoam if necessary. 5. Take, a two gallon sample of the slurry. 6. lump batches Into a cleaned #1 slurry tank. Dry as a two batch blend.
IV. Centrifuging and Drying ^ 1. The HO. 1 dryer is to he cleaned out thoroughly before
starting to-dry Opalon X-62. 2. Operating Conditions;
a. Centrifuge - Feed compartment - #3 Pool depth - #5 Feed rate - as necessary to maintain dryer temperature Wash water - none Dilution water - 10 gptn
be Dryer - Retention ring - none Outlet air tamp. - 150-155F (64-660) Inlet air temp. - 28o~310f (136-153*0} Air velocity - 100 PPM
3. Line up equipment for direct bagging. 4. Package material using plain bags marked only with lot number. 5. Take a 5 lb. bag sample from each blend.
RSV0026409
*t&S -3274 : 59-'
MONSANTO CHEMICAL COMPANY Plastics Division
Limited Procedure for Process Modification
Requested by ... A*. P. Torrensanoo c a 0 o 0
Technical Supervision
and Reporting By .... Fe. Torrenzano.
Number
Plant
G8tp5 O O O C O O .SprlAg$t&ld.
Product Group ... Vinyl.. c#eoBOtOtte .B-T-S. Suov,, Eng. J/n R. A* Coffey
Plant Dept. No .... Pk.
Research Gro. Lead.. B/ii A.Wr Cnakrftr/k
Oper. Sunt.
8/12 H-KL Perry
or Expiration Date
Gen. Mfe. Sunt. P.T.S. Manacer
a/n R-T. hmnlAp
Modification of SDP . PP^lPO. Xr6?.. o O o * Standards Dent.
8/t& A . fi. y.r^rlr^h*
Reason for Requested Variation
Approval required when segregation
To manufacture a low viscosity resin
of expense Is specified.
for valuation in 85 bldg* calendaring operations,
D /5SUEC Ac
STANDARDS
I960
Details of Modified Procedure
Cl) Bm attached TOP for "Experimental Line" operation*
Cf
(2) The "Opalon X6a TOP" will be modified by the use of Q$ OKS and an Inc: increased final vent in order to improve resin porosity and Initial cclcz
13} Target Specifications Pl ic' Viscosity! Dry Times
Contamination; Moistures Particle Slse:
0,29 to 0,33 12s00 max, (Read Mixer)
8-45 max,
0,3 % max. Trace Max, on 40 Mesh
Reference to Previous Work
1, Final Report 15FTC Resin for Rigid Sheeting"* Job Ho, 1583
CoGcMeCubbin* May 19* 3
*
RSV0026410
af' .y Hazara vnd Pi^fcautlons (Including Toxlcl^ Air, and Steam Pollution)
Use protective equipment when, handling TCS
Product Testing Required and by Whom Centro! Lab* - Specific viscosity, drytime, contamination, moisture, particle
size, Robbln color, and heat stability.
Identification and Disposition of Material
Segregation of Product Labeling of Product Approval for Shipment
Keep segregated Plain bag, lot number only PTS (A.F. tarrenasano, R. Coffey)
Costs
A. Esj-mair^d"TfT^t"n'lnSnuTIgt'urlng^^-oa.tB 1 f succet______ f Opalon X-62 - I2,,44d/lb. as compared to^Ofiaicsir^TO - t. 3^A^<
Op&lon X-69 - :u.9&Afc* Op Susp Res :iS:.4#/LV
B. Estimated extra manufacturing cost of this experiment Negligible
C. Segregation of Costs (by Operating Superintendent)
SNo segregation of Costs required Special Accounting number will be required D. If costs are segregated, accounting number assigned (by P.T.S. Manager) . P$Q042 ........
Informational Copies toj (To be filled out by Standards Department)
Plant Laboratory Supervisor Planning and Control Supt. Marketing Technical Service Mgr. General Mfg. Supt. P. T. S. Manager Accounting Dept. Fx-uuuct Administrator Research Section Leader Overseas Mfg. Dept. Other Domestic Plante Foreign Plants
L. g. Louraine
J* Jinahan________________________ B._Hanilin----- --------------------------------1111b____________________________
%- I*.Sml&P____________________________
J* - Cmbtrae F. Ps-^tmzafe____
/.&_!E-Slaiifc__.... ,__________________ .... ____________________ _____
H. F. Amatronfe
c717 AjdjmZZZHZl_______--___
itoeiatAng..-STOCTlaor -...J. Staslvstr.
Other
VIS 3274 (back) 1/59
RSV0026411
Tentative Operating Procedures
Opalon X-62
August 12, I960
Hie procedure described below will be employed to manufacture two batches, of modified Opalon X-62, a low viscosity homopolymer resin for evaluation in 85 Bldg, calendering operations
Briefly, the modifications include the addition of glyceryl monostearatef GlfS, and a lower conversion level, approx. 87^# in order to improve the resin porosity The 1$ trichloroethylene in the formulation used to obtain a 0,3D specific viscosity at the 60C reaction temperature.
. Batch Formulation
Haw laterial
Farts
Weight
Water VCM FDR-1 GM8
135
100 0.15 0.20
0.15 o,99
14,850 lbs, 11,000 lbs.
16.5 lbs 22,0 lbs 16.5 lbs 108.9 lbs
II, Charging Raw Materials
1. Charge X?OQ gallons of water to the kettle at 54-56C. Correct dipstick outage is 75 3/4 inches,
2. Start up kettle agitator. Adjust agitator speed to 121 BFM (approximately T7 rheostat setting on the variable speed controller),
3. Filter the FDR-1 solution into kettle.
4. Add the GMS and I&O2 solids.
5. Close manhole and draw a 24" vacuum purge.
8, Add TCE using kettle vacuum to draw in snaterlal via a, straw arrangement.
7, Adjust instrument set point to 60C and switch instrument to automatic control.
RSV0026412
-2 -
8* Position the Reset Cut-Out controller to th manual position using a 135 pal bias level.
9. When temperature has leveled out, switch Reset Cut-Out to the automatic position.
XXX Polymerization
1, The reaction is held at 60C for the entire cycle.
2* After approximately 8 hours the batch will heat kick. Use full cold water at 6l C and water Injection at 62WC.
3. Start the final vent when the pressure has dropped to 115 psi*
4. Vent the unreacted VCM to the gasholder as rapidly as possible without foam carry-over. Use sterox 110 antifoam if necessary.
5. Take a two gallon sample of the slurry.
6. Dump batches Into a cleaned #1 slurry tank. Dry as a two batch blend.
XV. Centrifuging and Drying.
1. The No, 1 dryer is to be cleaned out thoroughly before starting to dry Qpalon X-S2.
2, Operating Conditions 3
a. Centrifuge - Peed compartment #3 Pool depth - #5 Feed rate - as necessary to maintain dryer temperature Wash water - none dilution water - 10 gpm
Shyer Retention ring - none
*
Outlet air temp, - 150-155 F (64-66C)
Inlet air temp. - 280-310F (136-153C}
Air velocity - 100 FBI
3. Line up equipment for direct bagging.
4e Package material using plain bags marked only with lot number.
5. Take a 5 lb. bag sample from each blend.
RSV0026413
pJi
MONSANTO CHEMICAL CQMPJ Springfield, Massachusetts
August 30*5 l!
L&r'**-^y7UsrO.?( /rl f ' ,
To: R. A. Coffey (2)
At: PTC - PTS Subject: Pinal Report: Opalon. X-62
iMRSi
Reference: (1) Final Reports "PTC Resin for Rigid Sheeting", C.G. McCubbin, May 19# 1954 Sob No. 1563
Jo Introduction
A. w. Coaker R. E. Pollard R. I. Dunlap R. Ke Perry
W. P. Willis
0 o F. Smith S* L* Shrlver Vo P Brower G w. Smith
0. Erioksberg (9) W. Fe. Gabel G0 Fo Dorval
Subject P^uumber authorised the production of 20,000 pounds of a low specific viscosity resin for evaluation In 88' Bldg, calendering operations...
On August 12 and 13, i960, two batches of Opalon X-62 were made in the Experimental line.' Ike procedure employed (detailed la P-number request) was a modification of the original; opalon X-62, as recommended in Ref. 1. Glyceryl monostearate was added to , the formulation and the degree of VCM conversion was reduced in attempt to make the resin more porous and thus improve Initial color and heat stability properties.
II o Summary and Conclusions
1. Operational: Two batches were made under similar conditions without any major operating difficulties.
2o Quality: The resin blend met all quality target specifications, except for a slightly high specific viscosity.
Property
a. Spec. Vise. b. Dry Time, minutes c Contamination
Target Specification 0.29 to 0.33 12:00 max. Read Mixer 8 45 max.
d. Particle Size, 4o mesh 60 mesh 80 mesh 100 mesh 140 mesh
200 mesh Pan e. Robbins Initial Color f. Heat Stability
Trace max. *
Blend 19010
0.335
9:00
0-19 P #1 0 * 58 P #5 0-19 P #10
T T
3
10
30 34 24 Better than Std0 Better than std.
RSV0026414
V
ft. A. Coffey
2 August 30* I960
3* ' Quantity: Production consisted of 23*4-50# A~gra.de* and 1445# of off"grade* The high off-grade production resulted from dryer difficulties at the end of the run and in no wayreflects upon the X-62 process. The low total production* approx. 15*000 lbs.* Is a result of low VCM conversion during the polymerisation. Rather than starting the final vent a 115 psig# the final vent could he delayed until pressure drop to 80 psig. In order to increase conversion to the desired 85-87$ level.
4. Rates: Cycle times were 9*9 and 10.0 hrs. for the two polymerisation batches. No difficulties were encountered with centrifuging and drying* and it Is reasonable to assume that this product can be handled at 5000-6000 lbs. per hour. The Experimental Lin equipment only permitted a. 1000 lbs. per hour rate.
5. yields : Insufficient quantities for accurate yield determinations
6. Conclusion: The resin produced under authorisation of this Prausber met the required quality properties. Desireabillty of a low viscosity resin will be determined by Citron personnel. If desired* further quantities can be successfully manufactured in the Experimental Line at improved A-grade yields and increased TOM conversions.
A. P. Tomensano
Jw
RSV0026415