Document pm1q4745ORMR6ynkkwQ3V3nq6

STATUS REPORT THE UTILITY OF PROCESS 11 VINYL CHLORIDE RESINS IN FLOORING APPLICATIONS PHASE 1 - UNFILLED COMPOUNDS Authors: P. T. McCoy A . W. Conkling Date: April 22, 1966 File No.: ABSTRACT The performance of three ethylene modified vinyl chloride resins in an unfilled vinyl tile formulation are compared to conventional poly (vinyl chloride) resin. The resins exhibit greater flexibility, more resiliency, improved brittle temperature, greater ex tensibility, and easier processing characteristics than conventional Union Carbide Corpora tion suspension PVC counterparts. The level of ethylene contained in the sample of QXOM-7 did not exhibit the degree of influence on the tile properties or processing as that shown for QXOH-7 and QXOS-7. Union Carbide Corporation - Chemicals Division Research and Development Department Tarrytown, New York ucc 03953R THE UTILITY OF PROCESS 11 VINYL CHLORIDE RESINS IN FLOORING APPLICATIONS PHASE 1 - UNFILLED COMPOUNDS INTRODUCTION The first of a three phase program designed to compare the performance of Process 11 vinyl chloride resins in vinyl flooring applications with conventional poly (vinyl chloride) homopolymers has been completed. SUMMARY AND CONCLUSIONS The performances of QXOH-7, QXOM-7, and QXOS-7 as compared to QYSJ, QYTQ-7, and QYSL-7, respectively, in a typical unfilled vinyl tile formulation may be summarized, in general, as follows for the examined physical properties. 1) The influence of ethylene at three levels of external plasticization with FLEXOL plasticizer DOP (20, 40, and 60 PHR) promotes softer, more flexible, less brittle, easier processing, and more extensible compounds. Larger differences are shown at the higher levels of plasticization. 2) The influence of ethylene is more pronounced on QXOH-7, and \\ ' QXOS-7 than on QXOM-7; the respective levels are 1.05, 0.89, l and 2.06 per cent. ' ^ it $ il t * .06 3) The Process 11 resins require lesser amounts of external plasti cization to achieve a desired physical property as indicated: Tt> 0 CSf^Ti'^T' QXOH-7 11 pfer cent of total plasticizer in QYSJ QXOM-7 r cent of total plasticizer in QYTQ -7 QXOS-7 er cent of total plasticizer in QYSL 4) Neither plasticizer incompatibility nor resin contribution to staining appear to be a problem . 5) QXOH-7 and QXOS-7 exhibit wider differences in processability than QXOM-7 when compared to their respective homopolymer controls. Higher torques are encountered during the fusion of the Process 11 resins when tested on the Torque-Rheometer. 6) QXOH -7 and QXOM -7 are suitable for conventional all vinyl tile; QXOS-7 may be used but higher processing temperatures are required. 2. DISCUSSION This study is designed to show the effects of comonomer level, molecular weight, and plasticizer level on several important unfilled vinyl tile properties. The data are shown in Tables I thru III and in Figures 1 through 17. The observations reported herein are based more on trends rather than single points. Comments relative to the specific tests conducted in this investigation follow: Shore A and D Hardness - Both tests, a measure of indentation of the approximate hardness of rubberlike materials,were run to insure comparative ratings on the soft to hard compounds. The Process 11 resins are indicated as exhibiting consistently lower readings (softer) than the controls as follows in a table (and others that follow) to indicate relative differences. Please refer to Table II for specific comparisons. Resin QXOH-7 [,c& QXOM-7 & QXOS-7 i-.Ov y Average Test Units Lower Than Control Shore A Shore D 2.0 (2%) 2.0 (2.5%) 4.0 (9%) 4.4 (7.2%) 5.3 (6.0%) 8.7 (18.0%) This indicates the effect of comonomer level and external plasticization on the sub ject resins; QXOS-7 is indicated as the most sensitive or most efficient in terms of internal plasticization. McBurney Indentation, a measure of indentation resistance, indicates that the Pro cess 11 resin is more susceptible to external plasticization than their homopolymer counter parts as shown below: Resin Average Test Units Lower Than Control McBurney 1 Minute,, mils 10 Minute, mils QXOH-7 l 09 5.9 (12.5%) 3.9 (11.0%) QXOM-7 '/, QXOS-7 0 8.8 (14.0%) 3.4 10.0 (11.1%) (13.6%) Again, QXOS-7 is indicated as the most efficient of the Process 11 resins tested. Residual Indentation is a measure of indentation and of indention recovery. The differences between the Process 11 resins and the controls are very slight as indicated below: ucc 029538 3. Resin QXOH-7 Average Test Units Higher Than Control Residual Per Cent Indentation, mils Recovery 0.96 (24.5%) -4 (5%) QXOM-7 0.06 (1.9%) -3 (3.7%) QXOS-7 0.68 (25.0%) +17 (21%) All resins except QYSL exhibited a recovery of greater than 75 per cent, the minimum acceptable limit (Federal Specification L-T-751). Tensile and Elongation are measures of extensibility. The Process 11 resins show a slight loss in tensile strength and a slight gain in elongation as expected. A com parison with the control resins follows: Resin Average Test Units Compared With Control Tensile, psi Elongation, % Lower Higher QXOH-7 162 (6.3%) 32 (13.8%) QXOM-7 89 (3.0%) 18 (6.3%) QXOS-7 286 (8.5%) 33 (11.1%) The slight loss in tensile is not considered as serious for most flooring applications. 100 Per Cent Modulus is a measure of room temperature stiffness. The Process 11 resins exhibit a consistently lower value than the respective homopolymer control i.e. less stiff. A comparison with the controls follows: Resin Average Test Units Lower Than Control Modulus, psi QXOH-7 222 (10.5%) QXOM-7 165 (7.6%) QXOS-7 433 (22.0%) QXOS-7, again, is indicated as the most efficient of the resins tested. Brittle Temperature (ASTM-D-746) is a measure of low temperature performance in impact. The Process 11 resins exhibit consistently better performance as shown by the following data: 03953 4. Resin Average Test Units Lower Than Control Brittleness, *C QXOH-7 4 (67%) QXOM-7 3.3 (36%) QXOS-7 6.7 (59%) Apparent Melt Viscosity is a measure of processability. These compounds were tested at the standard conditions for plasticized compounds. The comparison with the con trols follow: Resin Average Test Units Lower Than Control Apparent Melt Viscosity Equilibrium Temperature m-g/sec C QXOH-7 QXOM-7 QXOS-7 * 40 phr only 210 (15?6) 13 (0.8%) 200 (5%) 2 (1%) 0 1 (0.7%) * The melt characteristics of QXOH-7 and QXOS-7 are in general agreement with previous findings that indicate easier processing; the performance of QXOM-7 did not follow these previous results and is not consistent with the QXOH-7 and QXOS-7 performances. Fusion Characteristics are a measure of the energy requirements in the initial processing operation. The Process 11 resins are more easily fused as indicated below: Resin Average Test Units Lower Than Control Fluxing Time Fusion min. Temperature, C QXOH-7 QXOM-7 QXOS-7 * - 60 phr 1.2 4.2 11.0 (20%) (43%) (81%) * 7 (6%) 11 (10%) 25 (22%) Higher maximum torques are obtained with the Process 11 resins which may be related to differences in particle geometries. The faster fluxing of the Process 11 resins is thought to be related to the higher torques and thus higher frictional heat. QUO 039540 5. Stain Resistance - The Process XX resins exhibit a stain level comparable to the controls. The stain levels of all resins were directly proportional to plasticizer concen tration. A . W. Conkling a uj r. P. T. McCoy /jb Attachments: 3 Tables 17 Figures ucc 039541 TABLE I PROCESS 11 - VINYL CHLORIDE RESINS CHEMICAL AND PHYSICAL PROPERTIES Ethylene, % Inherent viscosity, ASTM A Heating Loss, % QXOH-7 Blend 1 1.05 0.775 0.3 Contamination, slurry Apparent density, lbs/ft^ Particle size, median Thru 200 - mesh, % 2 32.5 160 7 Hard resin particles, 17 .5 mil, ft. 10 mil, ft.'2 Clear fisheye test Initial color mill test 40 1152 8 102 Resin flow time, sec/400 cc Dry blend time, min. C 3.4 4.8 81 QXOM-7 Blend 3 0.89 0.98 0.2 1 29 181 2 0 25 2 113 3.3 79 QXOS-7 Blend 4 2.06 1.31 0.6 2 27 215 2 0 83 2 114 2.0 77 ucc 03954 Resin QYS) Plasticizer Concentra tion, phr Durometer "A" "D" Indentation, Mils 1 min 10 min Indentation Mils Recov- ery % Tensile Strength, psi 20 97 73 4.8 6.4 0.16 84.5 3290 40 84 38 30.9 37.4 2.3 93.8 2700 60 71 22 36.5 51.0 6.4 73.8 1820 Ultimate Elongatlon, % 140 240 310 100* Modulus, psi 3280 2050 1070 Brittleness, * +20 -14 -24 Stain * Relative^) Asphalt Sandura 11 34 55 Apparent Melt Viscosity m-g/sec *C 2000 1Z70 860 154 146 141 Characteristics Time, Temp. Max. min C Torque 4.0 111 4600 6.8 109 1270 7.0 107 860 QXOH-7 20 96 68 7.3 9.8 0.99 78.3 3090 210 Blend 1 40 62 33 34.4 36.0 2.5 94.4 2590 260 60 68 20 48.4 60.8 8.3 68.2 1640 330 3040 1810 880 +10 1 -16 3 -24 5 1 1720 151 3.3 110 4650 4 1090 144 3.8 97 3350 5 690 140 7.0 98 1800 QYTQ-7 2k) 98 74 4.6 6.4 0.16 79.2 3550 200 40 35 40 33.2 40.0 2.8 93.2 3040 280 60 70 23 45.0 49.6 6.1 B3.3 2330 380 3420 2080 1050 +16 1 -16 3 -28 5 1 2400 158 4.7 114 4700 4 1540 149 11.4 120 2550 5 1050 144 13.2 114 1050 QXOM-7 20 96 70 6.3 9.6 0.45 79.3 3340 200 Blend 3 40 83 35 28.3 39.6 2.3 94.2 2960 300 60 68 22 47.8 57.5 6.5 72.3 2350 400 3230 1840 990 +12 1 -18 3 -32 5 1 2440 157 2.5 101 2440 4 1490 148 7.2 109 1490 5 1020 144 7.2 106 1020 QYSL-7 20 97 76 4.0 5.0 0.0 16.7 3800 220 40 89 43 25.8 37.2 1.8 94.5 3590 300 60 75 25 35.0 39.6 4.3 79.1 2700 370 3650 2410 1250 +18 1 -20 3 -32 5 1 DNF ENF 4 2100 152 ENF 5 1500 147 19.9 138 1350 QXOS-7 Blend 4 20 97 67 9.2 13.6 0.82 84.6 3700 260 40 81 31 36-2 43.2 2.2 94.1 3060 320 60 67 20 45.9 55.2 5.1 71.2 2470 410 3010 1740 970 +10 1 -26 3 -38 5 i 3050 162 DNF 4 1900 151 7.7 117 3000 5 1170 145 8.9 113 2150 <i'anj O O Test Formulation Resin FLEXOL DOP Mark KCB Stearic Acid 100 pans aB shcnra 3 0.25 1) Relative rating System 1 = Good 5 Poor Specimen Preparation Two roll 8" x 16" mill Roll speed - 70 fpm Roll Temperature - 170*C Mill time - 4 minutes after fluxing Hydraulic press - platen temperature - 170C * -T 2 TABLE III PROCESS 7 AND 11 POLY (VINYL CHLORIDE) RESIN UNFILLED VINYL TILE PROPERTIES PERFORMANCE SUMMARY Test Shore A Shore D McBumey One-Minute, mils Residual Indentation, mils Tensile Strength, psi Ultimate Elongation, % 100% Modulus, psi Brittleness, C Apparent Melt Viscosity, m-g/sec Efficiency Parameter 80 50 22 4.0 3000 300 2000 0 1500 Per Cent Less Plasticizer Required By Process 11 Resins Than Control QXOH-7 QXOM-7 QXOS-7 8.6 6.4 24.1 10.3 14.3 27.3 5.1 10.6 24.4 3.2 22.0 8.5 9.8 6.9 0 6.9 7.7 25.7 9.1 22.7 9.6 24.1 4.3 12.4 21.5 0 20.7 uec 039544 Shore Hardness ' Figure 2 iw eeo q q j -j Me Burney Indentation, One M inute, M ils Figure 4 039548 100 Per Cent Modulus, p si x 10 000 B rittle Temperature, | Fluxing Temperature, SSiticU Fluxing Torque - m -g/sec i G9j'6EG >5 vw,K,<*&&(? -v--v, ,, ,. .... ., Notebook Reference: 443 - pages 23 - 34 Period Covered: March 21 to April 15, 1966 Account Number: 224A90 Distribution Mr. W. H. Bauer Dr. F. E. Bailey Dr. J. J. Brezinski Mr. F. D. Dexter Mr. D. L. Engle Mr. J. F. Erdmann Mr. C. R. Field Mr. N. R. Gimber Mr, D. E. Richardson Mr. J. R. Wilkinson Mr. E. R. Weidlein, Jr. 1 jQC 039562