Document X7zEVvKzZLLaeXYJJ4yVLbX2K

t EVALUATION^OE--QSQM-Tr^BLEND 6,RESIN AT NEW ENGLAND PLASTICS CORPORATION, WOBURN, MASS. RECEIVED JU 14 1967 R. N. Wh-I r__ CustomerJPersonnel: John Gibbons, Vice-president Bob Alexander, Plant Engineer UCC Personnel Present: W. H. Hunscher L. G. Krauskopf S. Krumm Date of Visit: April 26 & 27, 1967 summary QSOM-7, Blend 6 resin was evaluated at New England Plastics Corporation in one rigid and two plasticized (85 and 65 Shore "A" durometer) formulations. The two plasticized formulations based on "0" resin when compared at equivalent durometers did not reach the equivalent preblend dryness of similar formulations based on Escambia 2225 pearls, nor did they extrude into equivalent product quality. Escambia 2225 is considered by NEP to be the very best resin in their plasticized formulations from the standpoints of preblend and extrusion characteristics. QSOM-7 characteristics were judged equivalent to their alternate resin -- Tenneco 250-1, Powderblend performance of the "0" resin in a rigid formulation was judged equivalent to powderblend based on Tenneco 12-R resin except for higher power consumption in the preparation of the powderblend. Slightly higher extruder die temperatures were required for the "0" resin formulations in all cases to approach standard product quality and gloss. Because of the higher die temperatures, increased susceptibility to product decomposition was encountered. In general, physical properties were equivalent except in two cases where slightly poorer brittle temperatures were measured for the "0" resin based products. uco 0394?n DISCUSSION Messrs. W. H. Hunscher, L. G. Krauskopf and the writer visited New England Plastics for the purpose of evaluating QSOM-7 resin in the contour extrusion of a variety of products. The following three were selected: (1) #87 chair tubing (unfilled 85 durometer) (2) #2 channel (filled 65 durometer) (3) #RV-115 Rigid (chlorinated polyethylene modified) The competitive resins being used in the products which were run during the trials were: Resin Products Escambia 2225 Pearls Tenneco 250-1 Tenneco 12-R #87, #2 #87, #2 #RV-115 The following plasticizers were used: Blended DOP/Drapex 4.4 in a ratio of 3/1 Blended DOP/DOA/Drapex 4.4 in a ratio of 68/11/21 Drapex 4.4 The dryblend and powderblend techniques were used to prepare ' feedstocks for the extruders. The feedstock preparation area contained the following mixers: 500# - 60 rpm, jacketed ribbon blender 500# - 120 rpm, jacketed Littletown blender 100# - 2 vessel, jacketed Diosna intensive mixer The fabrication area contained eight extrusion lines, including two sheet lines. Plasticizer reductions of 15 and 20% respectively were made in #87 and #2 formulations to achieve equivalent durometers to the standard products. A straight substitution of QSOM-7 for Tenneco 12-R was made in RV-115. The resultant formulations are shown in Table I. QSOM-7, blend 6, was selected for the trial since it was considered a good resin, low in fisheyes. A recheck by Texas City of a sample taken from one of the bags at NEP showed it to have over twice the fisheye count reported on the original quality control sample (10 mil Respro, normal count: 40 versus 83), The blend data sheet is attached for informational purposes. 2- - Shown in Table II are the time-temperature relationships achieved in the preparation of the preblends. The standard procedure involved 40 minutes of heating to 220F, followed by 40 minutes of cooling to 130F. Actual material temperatures in these trials were recorded by stopping the ribbon blender, then immersing a needle pyrometer into the preblend. A recording micromax usually records temperature throughout the entire cycle, but it was inoperative at the time. The #87 chair tubing preblend based on the "0" resin appeared initially to dry faster during the first five to ten minutes of the heating cycle, but no further improvement appeared obvious to the end of the heating cycle. On the other hand, Escambia 2225 based preblend appeared "wet" during the first five to ten minutes, but thereafter a significant improvement in dryness occurred which continued to the end of the heating cycle. In checking the dryness of the cooled preblend by the hand squeeze test, it was clearly obvious that Escambia 2225 preblend was significantly drier. The two NEP preblend operators stated that the "0" resin preblend was equivalent to preblend based on Tenneco 250-1 resin. Escambia 2225 preblend can be fed immediately after cooling to the extruders without encountering feed stoppage. On the other hand, Tenneco 250-1 preblend must be dried overnight. An extrusion trial of unaged "0" resin preblend was attempted to further measure its dryness. Soon after filling the hopper of #1 (small throat) extruder, stoppage of feed occurred. Several un successful attempts were made to restore feed to the screw, but when the two hopper vibrators failed to operate consistently, the run was terminated. Overnight aging of the preblend significantly improved its dryness to the point where no caking occurred in the hand squeeze test, and no feed problems were encountered in the No. 5 extruder, which has a larger throat. The #2 channel preblend was prepared under conditions similar to the #87 chair tubing. Here again Escambia 2225 pre blend dried faster and reached better ultimate dryness than "0" resin preblend. A Diosna intensive mixer was used to prepare the #RV-115 rigid powderblend. Tabulated in Table III are amperage versus temperature of the batches. At certain temperatures, power consumption when mixing "0" resin preblend approximated 50% more than that required to mix Tenneco 12-R powderblend. After discharge from the cooling vessel, however, no apparent differences in degree of dryness were discernible. Extrusion conditions for the three formulations are shown in Table IV. Starting conditions were the so-called "standard" which NEP had established as optimum for each particular formulation. In general, "0" resin based product lacked gloss at the standard conditions. Higher die temperatures of 10 to 20F improved gloss somewhat, but product quality suffered from inadequate dispersion and/or high level of hard particles. Product output and power consumption were equivalent in the extrusion of both #87 chair tubing and #2 channel preblends. In the extrusion of RV-115 rigid, a drop in power consumption resulted in a drop in product output from a 10 to 20F increase in die temperature. 3- - ucc 1 No evidences of product decomposition were apparent in the two plasticized extrusions. However, in the white rigid extrusion, two yellow streaks were clearly visible on product based on "0" resin, and to a lesser extent on product based on Tenneco 12-R resin. Thermal decomposition occurred faster than normal in the head and die sections on all four of the extruders after "0" resin formulations had been extruded. This was particularly disturbing since it was felt the inherent lubricity of the "0" resin had adversely influenced product quality and that these deficiencies could be overcome by more water on the screw and higher die temperatures. Improvement in heat stability probably could result through the use of certain stabilizers which are not necessarily critical for conventional PVC homopolymers. Limited physical properties are shown in Table V. These properties were determined on compression molded plaques pressed from roll milled sheets of the extruded products. In general, properties of the standard and "0" resin based products are equivalent, except for a tendency of the "0" products in two cases to have poorer brittle temperatures. SK: lvm 6-8-67 S. Krumrn VINYL RESIN BLEIJD DATA REPORT QUALITY CONTROL LABORATORY, PLANT 515 . <> O/r >' CPyo^-7 />' / > r LABORATORY DISPOSITION A'T 'VvrvJi- (y^o ^ BLEND NUMBER BATCH STATUS AL PLANT DISPOSITION 'PRODUCT AIM 20 mesh EXCEPTIONS BLEND WEIGHT DATE SAMPLED 34-y 3A.Q 9 -/JT- hb -- Solution Color, $ trnns. Screen A nalysis USBS Sieve 1 th r u Ho meuh 60 mesh 80 mesh 100 mesh lH-0 mesh 200 mesh 270 mesh \f.Ksdian Particle Size7, microns 'Heating Loss, $ Polyvinyl'Chloride Content, $ Inherent Vise., ASTM D-12H3 CaO> *tOtOPoHo Melt Viscosity Brookfield Viscosity, cps Falling Ball Viscosity, sec. > Slurry Contamination Rating Apparent Density, lh/cu ft Haze (Plaque), # Catanac, $ jOO 7? 47 3o 7. 3 -- /k/f o.x -- o.n._~ \ 1 A? Hard P a rtic le s j tKi leen- C o lo r C o lo r Solution Turbidity, $ trano. Oil Bath Heat Stability, min. ICMT Rating Initial, % traris. 1 Intermediate, $ trans. Ultimate, minutes Columbia Heat Stability, min. Whiteness Index, $ reflectance Brightness, % trans. Yellowness Pigmented Film 17.5 nils 10 mils Clear Hard Resin Particles # Toluene $ Methyl Ethyl Ketone 1 $ Acetone 56 Vinyl Acetate % Solids .. 1 ! Solvent C o m p o sitio n Water, $ Maleic Acid, $ Lead, ppm Reactivity, cps Insoluble Matter, # Plasticizer Absorption, PPHR . Dry Blend Time, mln/temp C lieein Flow, sce/Hoo cc Co-monomer ( ), $ 3,3/h. 3 .S ASTM Conductance Molt Vlscooity/Tomperature C *M o/n.yt> $(Ui c - 3 -B \ Ho,- lAjJ? +0 / O-S'o A 33 mo by ,A,Qjkg Date -2AaAs 5- - I too 039424 TABLE I PRODUCT FORMULATIONS #87 Chair Tubing - Green Escambia 2225 Resin QSOM-7, Blend 6 DOP/DOA/Drapex 4.4 (ratio of 68/11/21) Vanstay HTA (Solid Ba-Cd Stab.) Vanstay RR (liquid Ba-Cd Stab.) Parts By Weight .Standard "0" 100 40 100 34 2.5 0.8 2.5 0.8 #2 Channel - Gray Escambia 2225 Resin QSOM-7, Blend 6 ' DOP/Drapex 4.4, ratio of 3/1 Atoraite Vanstay HTA 100 80 33.3 1.0 100 64 33.3 1.0 #RV-115 Rigid - White Parts by Weight Tenneco 12-R Chlorinated Polyethylene Acryloid K-120 N 0-292 (Tin stabilizer) Drapex 4.4 Stearic Acid Mg. Stearate Unitane 450 QSOM-7 directly substituted for 12-R. 100 12.5 3.0 3.0 3.0 0.75 0.25 8.0 6- - #87 Chair Tubing With neutral ribbon blender, resin and dry ingredients added; liquids then pumped in (plasticizers and Vanstay RR which have been preheated to 120F prior to addition to blender) takes approximately 2-1/2 minutes to pump in liquids. 15# steam turned on blender. Forty minutes of mixing with heat to reach 210-220F, followed by 40 minutes of cooling to 130F. Batch discharged into fiber drums. TABLE II PREBLEND PREPARATION Cycle, Minutes 23 28 33 40 80 Standard, F "O", F 189 185 200 191 210 200 215 210 Cold Water On Blender 130 130 #2 Channel Same equipment and procedure as #87 chair tubing. TABLE III POWDERBLEND PREPARATION #RV-115 Rigid Add all solids, except lubricants, to mixing vessel of Diosna intensive mixer. When mix reaches 150F, add liquids and continue mixing to 175F. Add lubricants and drop mix into cooling vessel. Cool five minutes, then discharge into Gaylord container. Cycle Time Standard "0" (minutes) Amperage Amperage 11 0.25 0.50 - 0.75 1.00 - 1.5 2.0 2.5 3.0 3.5 4.0 75 170 75 170 Liquids Added 100 170 90 180 -- 85 180 83 180 85 190 95 200 100 210 Lubricants Added 130 230 85 130 -- -- 90 140 95 150 Liquids Added 105 150 125 170 135 190 135 200 155 200 Lubricants Added 155 230 Discharge mix to cooling vessel. 8- - UCC nt'Q4 : 7 TABLE IV EXTRUSION CONDITIONS #87 Chair Tubing Unaged Preblend No. 1 Davis - Standard Extruder - 2-1/2 inch, 20/1 L/D 3:1 Compression Ratio "O" Head-Die 1 Zone 1 2 3 4 Stock Temp. Load, amps RPM Cold Water on Screw Line Rate, ft./min, 330F 325 320 320 325 350 34 amps 106 80F 146 Remarks: Feed problems - screw starved - vibrators stopped run terminated. #87 Chair Tubing Aged Overnight Preblend No. 5 Davis - Standard Extruder - 3-1/2 inch, 20/1 L/D 4:1 Comp. Ratio Standard "0" Die 1 2* Zonel Front 2 3 4 Rear Amperage RPM Line Rate, ft./min. Cold Water on Screw Remarks - see page 10. Off Off 325 330 350 345 340 335 320 320 315 325 60-70 60-70 77 77 175 175 - - - One Turn - - - 9- - TABLE IV (Continued) Remarks Run started with "0" based product at "standard" conditions. Die temperature raised 20e>F to improve gloss, but still not as good as standard product. Conditions shown above are equilibrium conditions and actual instrument readings - not settings. #2 Channel No. 2 Davis - Standard Extruder - 3-1/4 inch, 16/1 L/D 2:1 Comp. Ratio Standard "0" Head Zone 1 (Front) 2 3 Amperage RPM Stock Temp. Line Rate, ft./min. Cold Water on Screw 355F 355-375 350 350 355 355 345 345 55 amps 55 amps 106 106 350F 350F 184 184 - - - One Turn Remarks Die temperature raised 20F to improve gloss, but still not as good as standard product. -10- ucc 039429 TABLE XV (Continued) #RV-115 Rigid No. 4 Davis - Standard Extruder - 3-1/2 inch, 20/1 L/D 2:1 Comp. Ratio Standard "0" Head 1 320F 330-340"F 2 Zone 1 (Feed) 320 310 2 320 330 3 320 340 4 (Front) Amperage 330 125amps 340 100-110 amps RPM 77 Line Rate, ft./min. 12 10 No Water Cooling Provision for Screw Remarks: Gloss and dispersion were relatively poor at standard conditions. Raised die and lowered feed to improve somewhat both properties, but still not as good as standard. TABLE V PHYSICAL PROPERTIES (Measured on 8 x 8x.l25M Compression Molded Plaque) RV-115 Rigid White STD "0" Specific Gravity 1.403 1.399 Durometer, Shore A - - Tensile Strength,psi 6620 6740 Tensile Elong., % 20 17 Brittle Temp.,C +4 +14 #87 Tubing Green STD "O" 1.262 1.268 85 85 3120 3020 246 260 -12 -12 #2 Channel Gray STD "0" 1.329 1.329 65 67 1550 1670 336 332 -34 -26 -11- DISTRIBUTION Mr. F. E. Bailey Mr. W. H. Bauer Mr. J. F. Erdmann Mr. J. T. Ferguson Mr. J. A. Field Dr. C. K. Fink Mr. N. A. Gimber Mr. T. F. Hartsing Mr. G. G. Himmler Mr. J. W. Hockersmith Mr. S. Krumm Mr. P T. McCoy Mr. D. E. Richardson Mr. J. W. Shilling Mr. G. C. Shipston Mr*. J. J. Smith v4tfC N. R. Wheeler Mr. H. K. Phinney