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CT- 1699
UNION CARBIDE
INTERNAL CORRESPONDENCE
PLASTICS DIVISION
To {Homo)
Company
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Mr. J. H. Field TEXAS CITY PLANT
P. 0. BOX 471, TEXAS CITY, TEXAS
March 21, 1966
Data
Copy I*
See Distribution List at End of Report
Status Report, Initial Production Run, QXOS-7
In the attached report Mr. H. H. Savage presents the detailed work done on the recent initial commercial-sized production run of QXOS-7, produced for the calendering and extrusion markets. Approximately 300M pounds of resin was produced with an ethylene concentration range of 1.53% to 2.06%. This was a fine piece of work.
Process Development and Laboratory Groups are to be commended for their valuable and timely assistance.
NAG: sh Attachment
N. A. Gimber
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SUSPENSION VINYL RESINS TEXAS CITY PLANT
Status Report Initial Production Run, QXOS-7
Author: H. H. Savage
Date: March 21, 1966
Summary
The initial production run of QXOS-7 has been completed--producing 298,280 pounds of resin. The maximum ethylene content attainable with existing equip ment is 1.6%. Pending customer acceptance, this resin could be produced at reasonably good rates. Substantial equipment additions would be required to produce QXOS-7 at the 2% ethylene level.
Discussion
The QXOS-7 run was started on March 4 and completed on March 10. Produc tion loss caused by this experiment amounted to 270, 000 pounds. Four blends totaling 298,280 pounds were produced. Blend analyses are shown in Table I. The first 21 autoclave batches were included in B-l and B-2, These batches were made with an ethylene charge that resulted in a final pressure requiring significant autoclave venting at the end of the reaction. The ethylene content was 1. 7%.
In an effort to increase the ethylene content to the desired 2%, the autoclav charge (except for ethylene) was reduced for the five batches in B-3, This blend contained only 1. 5% ethylene. This was caused by a difference in the proportion of the ethylene in the vapor and liquid phases. The final pressures of these batches averaged 290 psig and no venting was required.
The last five batches were charged with a 1/3 increase in the ethylene charge and were recovered as B-4. This blend contained 2.1% ethylene, but the auto claves required a considerable amount of venting. In two cases the amount of venting was so great that foaming plugged the 1/2" valve being used, and it was necessary to crack the hand vent valve to keep the pressure under control. Recipes used during the run and the recommended recipe for any future run at 1.6% ethylene are attached as Table II,
Other than obtaining the desired level of ethylene content in the resin, the only difficulty encountered was in attaining a reasonable reaction time at the v ry low reaction temperature of 41 *C. Fifteen pounds of IPP (75 lb. of solution)
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Status Report on QXOS-7
2.
were used per batch. This is more than a reasonable amount for the manual operation presently employed. Incidentally, the usage during full scale pro duction would be about 50% of the Non-Solvent usage.
As in the case of the QXOM-7, the resin particle size was rather large, the dry blending times were excellent, and the bulk densities lower than the com parable homopolymer. Fisheye ratings were good except for B-3 which was unaccountably high. ICMT color was good and ASTM conductance very poor. Melt viscosity results are not yet available.
The work of the Development Department in preparing the individual autoclave samples, and the many extra hours of analytical effort by the Resins Laboratory are gratefully acknowledged.
Recommendations
QXOS-7 cannot be considered satisfactorily scaled-up since the ethylene con tent that can be attained in the present system is less than the aim of 2%. For routine production, 1.6% is the maximum that can be promised. The South line is the only line on which QXOS-7 can be produced.
If full scale production at the 1. 6% ethylene level is contemplated, a charging system for the IPP catalyst system will be required. A batch charging met r and an extension of the Non-Solvent IPP circulating system would be required.
Production of QXOS-7 at the 2% level would require facilities for handling the vented ethylene and instrumentation for controlling the venting.
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TABLE I
QXOS-7 BLEND ANALYSES B -1 B-2
B-3
Pounds
Ethylene, %
Total Solids, %
Inherent Viscosity
Screens, 40 mesh 60 mesh 80 me sh
100 mesh 140 mesh ZOO mesh
Median Particle Size
ICMT Color
94,480
1. 74
99.6
1. 34
100 97 32 11 5 2
194
112
118,540
1.72
99.5
1.32
100 98 32 12 2 0
195
110
43, 520
1.53
99.4
1.28
100 90 29 15 4 0
205
115
Contamination Respro 17.5 Mil/10 Mil
3 0/52
1 0/53
1 6/1792
Bulk Density ASTM Absorption Clear HRP
27.0 112 3
27.0 118 2
29 108 3
Dry Blend, Min. /Temp.
2.4/78
2.8/78
2.3/79
ASTM Conductance
1.45
1.85
1.00
Melt Viscosity
-- Not Available --
3.
B-4 41,740 2. 06 99.4 1. 31 100
82 32 22
5 2 215 114 2 0/83 27 115 2 2.0/77 2. 10
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TABLE II
QXOS-7 RECIPES
3-21
Batches
22-26
27-31
Water, Gal,
2, 800
2,400
2,400
Methocel-15, Lb.
6. 0 5.2 5.2
Cellosize WP-300, Lb.
18.0
15.5
15.5
Sodium Bicarbonate, Lb.
13.0
11.2
11.2
Vinyl Chloride, Lb.
10,850
9, 310
9, 310
Ethylene, Lb,
625 600 800
IPP, Lb.
15 13 14
Termination Press Drop, psi
25 25 25
Reaction Temp. , *C.
41 41 41
4.
Future 2, 800 6.0 18.0 13.0 10,850 575 16 25 41
4
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Status Report on QXOS-7
DISTRIBUTION LIST
Texas City
Mr. W. D. Bush Mr. O. T. Carlisle Mr. M. E. Eisenhour Mr. J. F. Erdmann Mr. J. H. Field Mr. A. P. Fisher Mr. N. A. Gimber Mr. G. G. Harkreader Mr. J. L. Hockersmith Mr. O. A. Holt Mr. D. E. Richardson Mr. J. C. Schlichter
Tarrytown Mr. P. T. McCoy
Food Products Division, Chicago Mr. DonTijunelis
New York Office
Mr. A. A. Boehm Mr. W. J. Canavan Mr. F. D. Dexter Mr. C. R. Field Mr. W. H. Joyce Mr. J. R. Wilkinson
Bound Brook
Mr. N. H. Barton
Mr. Ed Bell Mr. A. J. Costantin Mr. F. A. DeMelio Mr. G. G. Himmler Mr. A. P. Mazzuchelli Mr. K. V. McCullough Mr. H. J. Rutherford
Technical Center
Dr. F. E. Bailey, Jr. Dr. J. J. Brezinski Mr. D. L. Engle Mr. J, W. Fields Dr. J. E. Glass Mr. W. S. Lanier Dr. W. R. Manning Mr. M. E. Sutherland
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