Document MN7n7w05YzoxjNVx842rgp0j
ETHYL CORPORATION
Medical Deportment 451 Florida
Solon Rouge, Louisiana 70601
4
TELEPHONE: Area 504 3870131
DISTRIBUTION
S. A. D'Armond^ W.E. Rinehart, Sc.D. T. R. Robinson, M.D. H.G. Smith H.M. Taylor M.R. Zavon, M.D.
D.E. Cooper October, 1974
ETHYL CORPORATION Medical Department Baton Rouge, Louisiana
STRICTLY CONFIDENTIAL
INDUSTRIAL HYGIENE SURVEY of
Baton Rouge Plant
Preliminary Survey of Materials and Processes in
PVC OPERATIONS
I. General
The sector of the Ethyl Baton Rouge Plant designated as PVC Operations is principally involved in converting vinyl chloride monomer (VCM), produced by the Hydrocarbon Area, to polyvinyl chloride of both the "suspension" and "emulsion" types. The area also produces a special oxygen-barrier type resin (Barex) for Sohio under contract.
A simplified lay-out of the plant is attached as Figure 1. This plot shows the Reactor Building, with its batteries of kettles, and also designates the areas for finishing, compounding, and warehousing. Figure 2 provides a simplified flow diagram, beginning with monomer, and showing the finishing stages of the "suspension" type resin. Finishing operations on the emulsion "resin" are shown in Figure 3.
Three lists of materials, originally compiled for various purposes, are attached. These are being reconciled into a common list, and MSD sheets are going to be available for most of the items. (A substantial revision of the lists has been necessitated by a recent switch of items in the product mixes of the Tiptonville and Baton Rouge plants). A fourth list shows raw materials used in Barex manufacture.
For present purposes the operations may be divided into five areas: Polymerization, Suspension Resin Finishing, Emulsion Resin Finishing, Resin Compounding, and Barex Resin Manufacture.
The writer had the benefit of a briefing by Henry Smith, Superintendent of these operations, and also of Wilbur Paulk, Mike Hopkins, and George Johnston who guided me through the various parts of the plant. Bob Callander described the Barex operations.
VCl105
II. Principal Materials (Raw Material, Product, By-product, Supportive)
2.
The materials mentioned below are only illustrative. the attached lists show, hundreds of materials, including dyes and additives, are used in producing resin products. A large fraction of the products are produced and/or compounded to customer specifications. And many of the polymerization recipes themselves are proprietary. Accordingly the following sections of this report are intended to serve simply as a rough outline and guide to assist an in-depth study of the situations with which the hygienists need to become familiar.
As
Suspension Polymerizations
The suspension polymerization kettles are designated with an Qp in the circles at the left of Figure 1. Those
four in the cross-hatched lower box are newer and larger vessels.
Most suspension polymerizations are run at pressures above 100 psi, ranging to about 240 psi. A typical reactor charge will consist of:
1) Suspending agent, e.g. "Alkatex",(polyvinyl alcohol)
2) Catalyst, e.g. dodecanoyl peroxide, or X-16, or both. X-16 is a proprietary catalyst prepared on-si te_.
3) The charge of vinyl chloride under pressure
4) Antifoam (silicone)
5) Short-stop, e.q. para-benzoquinone in chloroform
orieatdnfe.
---------
The kettle is heated to begin the reaction, but chill water is then circulated to absorb the reaction heat.
Emulsion Polymerizations
These reactions are usually run at lower pressure, e.g. 100 psi. A typical charge will contain:
1) Emulsifiers. Various soaps, (all purchased). Calsolene (ICI), a sulfonated oleate. Myristic acid plus ammonia. "Sipex" soaps. Triton N-361.
VCllOfc
3.
2) Isopropanol
3) Antifoam
4) Vinyl chloride charge
5) 10% ammonia or 1% ammonia or 25% caustic (Allied chemical) for pH control
6) Shortstop, e.g. benzoquinone in chloroform or acetone
Polymerization Operations - General
Chill Water. Water is cooled by two Freon-11, and one F-12-charged units for use around the jacketed reaction kettles, and also to cool some solution make up tanks.
De-ionized water is required in the polymerizations. Water from drilled wells is de-ionized in:
3 cation exchangers 3 anion exchangers, and then 2 mixed-bed exchangers
The beds are regenerated by caustic and sulfuric acid.
vinyl chloride recirculation. The flow diagrams trace the movement of VCM. After a polymerization reaction is complete, the kettle is depressurized, then de-gassed under reduced pressure. This unreacted fraction of monomer is sent to the holder shown in Figure 2. The stored gas is compressed and fractionated in a stripper, where the noncondensables (mainly nitrogen, with some monomer) are vented. The condensed monomer is returned to the storage feed tanks. (An incinerator is planned for disposal of this waste).
Suspension Resin Finishing
De-gassing. The slurry of resin is discharged into a de-gassing tank (see Figure 2), where vacuum pumps boil out the reacted monomer, by-product gases, and atmospheric gas (essentially nitrogen). These flow to a gasholder. The gases are later compressed and the non-condensables stripped out and vented. (See planned incinerator).
Centrifuging. The slurry is centrifuged to separate the suspension resin from the mother liquors. The resin drops into a rotary dryer. The aqueous effluent has a generally clear appearance, and appeared quite free from odor, it contains all the chemicals which do not enter the reaction, of course, plus by-products. This water is discharged into a sump and open ditch leading to one of the ponds. No analysis was available.
VC1107
4.
Drying. In a rotary dryer, the resin is blown with air filtered and heated by steam (from Gulf States Utilities). The moist air exhaust is discharged through chimneys on the roof. Besides water, the discharge contains relatively low proportions of VCM and other organic volatiles. (The moisture shows up in the form of fog on occasional winter days).
Emulsion Resin Finishing
These operations are shown in the diagram of Figure 3. Emulsion resin particles are very much finer than suspension resin, with size in the range of 30-50 microns. (These products are intended mainly for shipment as the powders to purchasers for use in making battery separators and many types of coatings.
Drying. The emulsion from the autoclaves passes through screens to 1) storage tanks to 2) pumps feeding the 3) spray dryers. In these dryers, filtered and steam-heated air flashes off the water scattered by a spinning disc. The powder is dropped out and conveyed in a blast of filtered air to cyclones which separate the product and drop it onto screens which reject oversize particles.
The air from the cyclones contains some powder, and this is removed by dacron bag filters (500 bags). The air is discharged at the roof. (Since no liquid was separated by centrifuging or filtering, the discharge air from the emulsion dryers contains all the water, as well as all the volatiles from the polymerization process).
(Occasionally a bag bursts and a cloud of resin
powder billows up at roof level. This event is not
monitored by equipment, and is detected only when
someone catches it by eye).
____
The product passing the screens goes to bagging equipment.
Grinding. For some purposes the finished emulsion resin is still too coarse, and the product is fed to a grinder to produce a powder which meets customer specifications.
Resin Compounding
Most of Ethyl's PVC compounding operation uses suspension resin. (Supplies of the resin are kept stored in a silo. For any particular recipe a weighed batch of resin is mixed with any of many varieties of dyes, plasticizers, processing aids, etc. (see list at end of tnis report) and fed into a ribbon blender. (Most
of the additives are received in bags or drums). The mixture goes to a heater, and is then formed into hunks, or "bricks''. These bricks go to a roll mill, where they are formed into a sheet and then cut into strips. The
strips are cut into "dice". Shipment is maHe^li5"^igsr" large boxes, or 180,000 lb. capacity rail cars.
VC1108
Barex Resin Manufacture
Ethyl makes Barex for Sohio under a contract with limited term. Sohio is now building a Barex plant, and they have licensed a Swiss company (Lonza) to produce the resin. Much of Ethyl's product is shipped to Vinyl Plastics, Inc., who extrudes a packaging grade film. Oscar Mayer is a principal customer for this.
As many as 28 raw materials go into Barex manufacture. (See attached list.) The process is complicated, and involves several steps. The recipe calls for a number of pre-blends to be made up.
In principle, Barex is made by preparing a nitrile elastomer latex which is stored temporarily for use in the second step. In the next step two other monomers are grafted onto the backbone of the elastomeric polymer. The final product is coagulated into short, white strands, and is shipped in this form. Much of the process information is proprietary, and for industrial hygiene purposes it should be necessary here only to identify the raw materials and understand- their roles in the operation.
Nitrile rubber latex. A soap is prepared from Emersol fatty acid and potassium hydroxide. Other ingredients:
Stabilizers and Antioxidants Polyguards and Naugards (Uniroyals1 Nos. 401, 402, 403, 404. MSDs on request through Sohio. These substances remain in the product!"^
Catalyst, dry: DuPont VA 20-64. Monomers:
Acrylonitrile (tank truck) Butadiene (tank truck) Chelator: Versene Daxad Tertiary dodecyl mercaptan
This operation is conducted under pressure at slightly elevated temperature. Two or three batches can be prepared in one day. The 6 batches from 2 days operations ("one campaign") are adequate for making 40 to 60 batches of Barex resin, and are stored for this second step.
In the second step acrylonitrile and methyl acrylate are grafted onto the 'elastomer.
Other ingredients:
5.
agent. Injected as reaction proceeds^ (Obtained from Evans or Carlyle) Polyvinyl pyrollidone MonowetT, as emulsifier. Also
Gafac.
VC1109
After 6 batches have been accumulated in the second (qraft) step, these emulsions are coagulated by the addition of an alum solution. The mixture is next extruded through a perforated disc into water kept at 180F, forming single wrinkled strands, roughly one inch long. These are screened, washed, screened, washed, and finally dried.
By-products. The autoclaves are de-gassed under vacuum, and the exhaust vented at the roof. The major organic effluent from the latex operations is butadiene.
6.
About 85-90% of the monomers used in the Barex plant goes into the product. The waste water from the first screening is hauled away in tank trucks by Rollins Environmental (Div. of Rollins International). This liquid contains a lower aqueous phase containing about 5% of unreacted monomers, and for disposal is biologically treated. The upper, organic phase-mostly monomers plus low polymers-is burned by Rollins.
The exhaust from the final drying of the resin contains some monomer vapor.
The wash waters (produced after the first screening) go to the ditch. These contain some Monowet, some monomer, and some of the resin.
III. General Notes
1. Waste PVC. The plant produces considerable material which is either particle oversized, or suspended in effluents, or below grade. Where possible, the offgrade and off-size material is sold. Floor sweepings and other solids go to landfill. Large amounts of material accumulate in the settlings of ponds. The ponds are periodically drained, and settled wastes hauled to landfill.
2. Autoclave Clean-up. The walls of the PVC autoclaves are purged with high-pressure water after every resin batch is discharged. The wash water flows to the ditch and pond, carrying PVC scrappage.
Attachments: Figures 1 to 4 Lists 1 to 4
D.E. Cooper October, 1974
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NASH VACUUM PUMPS
SLURRY DEGASSER
SLURRY
STORAGE TANKS
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DRV PRODUCT
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NOTARY DRYER
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EMULSION PTNfSHItiie SYSTEM
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MATERIALS used in COMPOUNDING AREA*
Serial Series Code (see list in following pages)
0001 1000 2000
3000
Supplementary polymers
Plasticizers
Fillers (modify opacity, color, wear, etc.)
"Special", esp. fireproofing agents, etc.
4000
Stabilizers
5000
6000 7000
Lubricant additives - internal and external
Pigments (organic and inorganic)
Impact strength and modifiers
This list is partially obsolete, and needs both additions and deletions, due especially to switches in Tiptonville and B.R. product mixes.
VCH15
RAW. MAI?;RIALS AND MISCELLANEOUS SUPPLIES - PVC AREA y y y/ y
/ta/M/if
# A# Pf /" A
"ode 0C11 0012 1008 1013 1023 1026 1028 1079 1083 1107 1175 2019 2041 2042 2047 2054 2055 2057 2058 2059 3147 4009 4020 4021
25 4032 4035
_Name Styron 685-26-7 Tyril 867*21 Natiu-al 7 DOP DIDP Drapex 4,4 Cerechlor 42 Cerechlor S-52 Santicizer 160 D0A Epoxol 7-4 Epoxol 8-2B Celite 263
j Atomite Winnofil S
% Omyabsh Fiberglass PPG Fiberglass Desertalc 57 P-414 P-413 Jayflex 205 CH-55 Advastab E-82 BC-103A TM-303 Tinuvim p Mark 356
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So\! cl
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Chemical Composition
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PAW MATERIALS AND MISCELLANEOUS SUPPLIES - PVC AREA (cont'd)
/-y* 3-
rode 4049 4056 4063 4081 4086 4088 4113 4114 4115 4129 4130 4142
54 4156 4172 4200 4210 4211 4219 4220 4221 4223 4232 4233
16 5018 5023 5027
_______________ NeMue Mark C Mark V?S Mark OHM Cardinal No. 1 Cardinal 10 Cardinal 2 AYA Cardinal Clear 54 Mark 152 Mark 577A Irganox 1076 Ferro 1827
State
Chemical Composition
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:au materials a:;d miscellaneous supplies : pvc area (cont'd).
Code 5028 5036 5037 5044 5047 .5051 5059 5064 5066 5068 5073 5075 ,002 6007 6008 6010 6011 6012 6014 6015 6023 6025 6026 6029 ^30 6031 6032 6035
Name Wax OP Flakes Calcium Stearate Stearic Acid Aldo MO Aldosperse 0-9 Kaydol Sodium Stearate MS-2 Resin Aldo S-932 Wax PA-190 Advawax 165 629 A Wax UB Blue 59-4967 Lakeoline Violet 1
t Apex 8003 Aluminum R-500 or R-100 R-101 RT-791-D Violet Ti Pure R-900 RF-1 or RF-2 FDC Violet Drakenreid 1C324 Sun Yellow Sea Amer 1162 Yellow Amer 1166 Yellow Amer 1167 Brown Amer 1198 Black Amer Yellow 1206
State So\<51
Chemical Composition
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.W .'.Uf.fiirii.s amu MISCELLANEOUS SUPPLIES - PVC AREA (cont'd)
--Code__ __
Name
o036
Amec 1204 Yellow
6039 6040
1484 Maroon
*
X-Z541 Yellow
6044 %
6045
M.B. 1049 Black Amer Orange 1026
6046
Amer 1050 Blue
6047
Amer Yellow' 1056
6049
1058 Green
6050
IMP X-2944 Perm. Green
6052
FDC Green 1100
6054
3300 Blue 18
6060
Reynolds 50 Paste
64 14-4008 Hosta Perm.
6071
Raven 15 Carbon Black
6072
Molacco H Black
6075
UMB Blue 4725
6076
Tinapol PCR
6077
10369 Brown
6080
UB 0008 Violet
's
6081
V 5100 Dark Buff
6082
Ferro V-5101
6084
.X-2I53
Yellow
6085
10380 Grass Green
6086
X-2315 Deep Yellow
"*87
X-2272 Primrose 11
6089.
Rsia3_J15-Red
6090
R--1030 114 Ol'au^e
6091
R-1Q-3G--113 Orange
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a* o-uri.j^j.-s AMU MiSCtJlANl'iOUS SUPPMKS - PVC AREA (cont'd)
. Code o094 6096 609S 6103 6104 6107 6109 61 i4 6118 6120 6123 6124
-26 6127 6128 6129 6131 6134 6136 6138 6139 7002 7003 7071 -">72 8001 8002 8017
Name Monarch 74 Black
State eoVitS.
Chemical Composition
Violet ZIRS YT '5620 Green Gold V-5102 Brown FDC Violet 1
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^Uvvn'i *-a ^aJ^h
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5011 $L
(2- k rsy*\
i *-C.
Ky-788D
K/-781D
Amer 50 M Red I2Z? R. \
Drakenfeld 10382 Brown
Mapico Tan 15
Mapico Brown 421
Mapico Red 477
X-2925 Monark Blue g
YE 42 ID Orange
Y-469-D Yellow
-------------
Raven 30 Powder
Cromoplital Yellow 3G Tone
Ti02 Cr 800 PG
Amer Cyan. Blue 55-3750
KR-980 D
K-120N
Blendex 575
Nevadine LX-509
Piccolastic D-125
Blendex 301
Blendex 401
Blendex 311S
i
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Product
/ < " r `w 9 f j__ i
Supplier
Adogen 58
Ashland Chemical Co.
Advastab T-340
Cincinnati Milacron
Advastab TM-181S
Cincinnati Milacron
Alcotex 72. 5L
Revertex, Ltd.
Antifoam 60
General Elec. Co.
Barium Stearate Blendex 436
Snythetic Pr. -Americhem Marbon Chemical
Butyl Benzyl Phthlate Hatco Chemical BBP
Butyl Stearate
Emery Industries
Butyl Diol 1, 3
Celanese Chemical
CPE 3614
Dow Chemical
Cadmium Stearate
Synthetic Products
Calcium Chi. anhy. reagent 12 mesh CX 150
AWC, Inc.
Calcoline Oil HSA
ICI America
Colloid 987
Colloids, % Chem. Soln.
Ccpper Sulfate pent. McKesson Chemical
Dibutyl Tin Laurate Cincinnati Milacron
Dioctyl Adipate DOA
Monsanto Chemical Eastman Chemical U.S.S. Chemical
Di-basic lead stearate National Lead Co. DS-107
Dioctyl Azelate DOZ Ashland Chemical
Dioctyl Phthlate DOP Ashland Chemical
Drapex 4.4 DM-7704
Argus Chemical Co. M&T Chemicals
Product Electrocarb 105
Supplier Hamm nd Lead Co.
Epoxidized Soya Oil Ashland Chemical
Epoxol 9-5
Swift & Co.
Glycomul L
Glyco Chemical
Clycosperse 05
Glyco Chemical
Kane Ace B-18A1
Mitsui & Co. Kaneka America
Kane Ace PA-11
Mitsui 8c Co.
Kaydol Mineral Oil Witco Chemical
LX-509 M&T T-66
Neville Chemical M8cT Chemicals
M&T 7888
M&T Chemicals
M&T 8494 Mark 152
M&T Chemicals Argus Chemical
Mark 417 Mark 734A
Argus Chemical Argus Chemical
Mark 971
Argus Chemical
Mark 292
Argus Chemical
Mark 1911
Argus Chemical
Multiflex MM
Diamond Shamrock
Myristic acid 1499 Parabenzoquinone
Kortman & Schultz Eastman Chemical Pr.
Pluronic L-62
Southern Solvents
RF Titanium Dioxide New Jersey Zinc
Synpron 1115
Synthetic Products
Synpron 1314
Synthetic Products
Snypron 1169
Snythetic Products
'
Product
Supplier
Sod. lauryl sulfate 5 0 90%
Alcolac Chemical
Sipex SD Sulfuric acid 93% Superfloss Tinuvin P Titanium Dioxide Triton X-3Q1
Alcolac Chemical Stauffer Chemical Johns Manville Geigy Ind. Chemical Kerr-McGee Chem. Rohm & Haas
DYES
Oil Violet Zirs
American Cyanamid
Black 1198 Black R1998-R-1
Ame richem Americhem
FD&C green 1100
Ame richem
Ivory 7487 R-l
Americhem
Violet 3342-R4
Americhem
Violet 5501
Arre richem
Masterbatch 1049 UB 0008 Violet UB 4725 blue Mapico 1100 Mapico brown 421
Americhem Chemetron Chemetron Cities Service Cities Service
Molacco H black
Cities Service
Columbian black 999 Citi s Service
Raven 30 Super spectra
Cities Service Cities Service
Pproduct
Supplier
RT -791 -D violet YE-421-D orange
E. 1. Dupont E.I. Dupont
Y49&-D yellow
E. I. Dupont
K0786-D Kroler orange E. I. Dupont
Y-488D Yellow
E. I. Dupont
V-5102 brown
Ferro Corp.
V-5100 dark buff
Ferro Corp.
Drak. 10383
Hercules, Inc.
Drak. 10324 amber brown
Hercules, Inc.
Imp. Red X-2327
Hercules, Inc.
Primrose yellow X2272 Hercules, Inc.
Kristalex 3085
Hercules, Inc.
lakolene violet #1
H. Kohn stamm
Iron Oxide brown 420D Reichard-Coulston
SOM violet cone. 1963RL- Synthetic Products
Ultramarine blue 4959-00 Whittaker, Clark, Daniels
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V VC1124
%
ill
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CODE
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