Document O1qB69vpoM9vrV2XkNB8jp6Zv

VU1ML * SPA 674 P, E. - Burlington P. F. Albaneae M, G. Caine H. 8. Carr H. H. Duhamel E. Farber J, C. Fisher C. W. Johnston R. W. Eulicfc 10 E, Rad u G. I* Rozand is P, R. Scarito I IX W. D. Wesely i 14 M. W. Williams 15 R & D Log Book 16 Extra 17 Extra m CObORITE 015668 CONFIDENTIAL cbpY_____ OF_____ TENNECO PLASTICS DIVISION Research and Development Department Process Engineering Section SPECIAL PRODUCT ADJUSTMENT REPORT Report No.: SPA 674 Project No.: 30-008 Date; February 5, 1969 DISTRIBUTION P. F. Albanese M. G. Caine H. B. Carr H. H. Duhamel E. Farber J. C. Fisher C. W. Johnston R. W. Kulick E. Rad G. I. Rozand P. R. Scarito W. D. Wesely M. W. Williams Process Enginec R & D Log Book - Burl. TITLE: Tenneco 389 AUTHOR: A. V. Wagner DIGEST Frequent complaints from Capitol resulted in the issuance of SPA 674. The major complaints were: 1. Poor audio 2. A high percentage of non-fill3 3. Poor resin flow 4. A shorter Henschel mix time. This SPA with 12 extensions resulte'd in a better quality resin at a 0.21 cents per pound increase in manufacturing cost. Acceptance of this resin by Capitol has resulted in an AMP as of November 26, 1968. COLORJTE 015669 Report No. : SPA 674 -2- TABLE OF CONTENTS Page No. DIGEST................................... ............................. .................................................... 1 RECOMMENDATIONS................................................................................................ 3 CONCLUSIONS...................................... .. ................................................................ 3 DISCUSSION......................................................................................................... .. 4 A. Background and Summary of SPA 674 and Ext ensions..................................................... ..................................... 4 B. Formulation and Processing........................................ 7 REFERENCES............................................................................................................ 8 TABLES: I - POLYMERIZATION CONDITIONS & QUALITY CONTROL RESULTS......................................... 10 II - FORMULATION AND INSTRUCTION SHEET................ 11 COLORITE 015670 -5~ Report No.: SPA 674 RECOMMENDATIONS 1. Continue to use 80-018-06 as an antistat even though this has reduced bulk densities. 2. Continue to use 90-101-05 for good audio, non-fills, and biscuit appearance. 3. Investigate the possibility of improving the cycle time by in ducing a heat kick. This should produce the same effect as the longer reaction times. 4. If a narrower particle size distribution is desired, evaluate higher agitation. 5. Increase charge agitation to reaction agitation. 6. Evaluate the use of recovered monomer in the present formulation. CONCLUSIONS 1. Since 80-018-06 has been used in the processing of T-389, flow problems have been eliminated. However, bulk density has de creased 2-3 lbs. per cu. ft. 2. 90-101-05 appears to have solved the audio, non-fills, and rough biscuit problems. During the course of this SPA, it was necessary to double the 90-101-05 level to meet Capitol's re quirements . 3* The total manufacturing cost of this resin increased 0.21 cents per pound (0.15 cents per pound-due to increased reaction times, 0.06 cents per pound due to increased raw material costs). 4. A higher conversion has further improved audio, biscuit appear ance, non-fills, and processing at Capitol. 5. Recovered monomer did not appear to affect physical properties. COLORITE 015671 \ Report No.: SPA 674 -4- DISCUSSION A. Background and Summary of SPA 674 and Extensions High levels of background audio noise and a high percentage of non-fills in records produced with Tenneco 3&9 had led to com plaints from Capitol. Capitol was also concerned about the shorter Henschel mix time, which overloaded their surge hopper, and poor resin flow, which "rat-holed" in their "funnel" test and is indicative of what may happen in their surge hopper. SPA 674 and 12 extensions were initiated to correct these de ficiencies in the Tenneco resin, SPA 674 The object of this SPA was to produce a resin with a narrower particle size distribution (10 - 50% on 80 mesh and a maximum of 5$ thru 200 mesh), a higher relative viscosity (1.66 - 1.69), and a higher brabender torque (900 - 1000). 80-029-05 was re placed with 80-018-06 in an effort to improve resin flow. Lot 698012 (47,000 pounds) was produced, but was not shipped because of low relative viscosity and a high percentage on 80 mesh. Resin flow of this lot was excellent. SPA 674-1 The object of this extension was to raise the relative viscosity and decrease the high percentage on 80 mesh. Lot 698013 (47,000 pounds) was produced and met all Quality Control tests. However, it was rejected at Capitol because of poor audio (background noise). 80-018-06 was again used as an antistat agent. This lot was later accepted as lot 698016. SPA 674-2 The object of this extension was to evaluate the effect of 80-029-05 on audio properties. 97,000 pounds were produced and divided into two lots. One lot was prepared using 80-029-05 and coded 698015; the other, with 80-018-06 and coded 698014. However, lot 698014 was contaminated with T-314 and could not be shipped. Lot 698013, which was produced by the same formu lation and had almost equivalent physical properties, was shipped in place of 698014 as 698OI6. Lot 698015 was rejected for poor audio and rough biscuit. Lot 698016 was accepted; however, Capitol commented that the biscuit appearance was slightly rough and smaller in diameter than the Borden control. COLORITE 015672 -5- Report No.: SPA 674 SPA 674-3 The object of this extension was to produce a smoother biscuit via increasing the acetate level. Lot 698017 (47,000 pounds) was produced, but was rejected by Capitol because of poor audio and rough biscuit. SPA 674-4 A review of Quality Control data conducted by the Customer Ser vice Laboratory pointed out that resins that were found accep table at Capitol had Tinius-Olsen values averaging 0.42. As a result, a lower relative viscosity was targeted to increase the Tinius-Olsen. Lot 698018 resulted in a lower than target vis cosity and was not shipped. SPA 674-5 A study by R & D and C.S.L. showed that the rheology of the Capitol resin was significantly affected by adding certain additives. 100 ppm of 9O-IOI-O5 was blended into lot 698017 and based on laboratory tests this resin was sampled to Capitol. Acceptance of this sample led to lot 698020 (47,000 pounds). However, in this case, 90-101-05 was added to the polymerization charge. Capitol reported that biscuit and audio were excellent. 1800 pounds were saved as a control standard. A sample of this lot, treated with an additional 100 ppm of 90-IO5-O5, was sent to Capitol for evaluation and was coded 698021. Capitol report-, ed that this resin was too soft (over lubricated). SPA 674-6 As a result of little or no improvement in extrusion rate and extrudate surface of lot 698020 shown by R & D testing (instron rheometer), two batches were produced to evaluate 90-101-05 levels. Lot 698023 was produced with 100 ppm 90-101-05 and sent to Atlantic Tubing. Lot 698022 was produced with 200 ppm 90-101-05. Two hundred pounds were saved as a control sample and the balance was sent to Atlantic Tubing. SPA 674-7 This extension was issued for an extended run based- on the satisfactory evaluation at Capitol of lot 698020. Seven lots (575*000 pounds) were produced under this extension and all were accepted at Capitol. However, Capitol continued to complain about the coarseness of Tenneco resin. Gelatin level was in creased in one lot in an effort to reduce the percentage on 80 mesh. COLORITE 015673 \ Report No.: SPA 674 -6- SPA 674-8 The object of this extrusion was to produce a narrower particle size distribution. Increasing gelatin did little to narrow the particle size distribution. However., increasing agitation did narrow the distribution at the gelatin level in use. 515,000 pounds were produced and accepted at Capitol. SPA 674-9 This extension was issued to continue production on the formula tion established in extrusion eight. One lot, 698055, (40,000 pounds) was produced under this extension. SPA 674-10 The object of this extension was to incorporate the use of re covered monomer in the formulation. Two of four lots produced with recovered monomer (540,000 pounds) were rejected at Capitol, lots 698056 and 698057- These lots were rejected because of rough biscuits, poor audio, staining, and fast extrusions. It was noted that lot 698056 had a high Tinius-Olsen (O.56). Lot 698057 was reluctantly accepted later by Capitol. Lots 698054 and 698055 (540,000 pounds) were produced with recovered monomer and found acceptable. SPA 674-11 The object of this extension was to duplicate lot 698022, which was approved at Capitol,-and was produced with 200 ppm of 90-101-05 (SPA 674-6). Although the resulting lot 698059 (47,000 pounds) was accepted, Capitol's laboratory reported it as border line for audio, slight staining, and a slightly rough biscuit. SPA 674-12 In order to improve the properties of the resin produced by extension 11, a higher polymerization temperature and a higher percent conversion were utilized. 660,000 pounds were produced under this extension. An AMP was issued November 26, 1968 based on this extension. COLORITE 015674 \ Report No.: SPA 674 -7- B. Formulation and Processing Four factors have led to our return to the approved suppliers1 list. 1. The use of 80-018-06 as an antistat agent in place of 80-029-05 has eliminated the flow problem as defined by Capitol's funnel test, but has decreased bulk density by as much as 3 lbs. per cu. ft. If Capitol has problems with overloading their storage bins, a program of evaluating other antistats should be initiated. Otherwise, it is recommend ed that the use of 80-018-06 be continued. 2. The use of 90-101-05 appears to have solved the audio, non fills, and rough biscuit problems. Since 90-101-05 has been incorporated into the formulation, 3,165,000 pounds of Tenneco 389 have been accepted at Capitol. During the course of production, however, it has been necessary to double the charge of 9O-IOI-O5. 3. An extra hour of polymerization, after 35 psig has been reached, has further improved audio, biscuit appearance, and processing at Capitol. However, this has increased manufacturing cost by 0.15 cents per pound of resin. It is recommended that at a reaction pressure of 65 psig, the reaction temperature be raised to 175F to induce a heat kick and finish off the batch more quickly. One batch should be produced and a slurry sample sent to the Pilot Plant for processing. This sample should be evaluated first by C.S.L. and, if acceptable, by Capitol. 4. Particle size distribution has been narrowed by increasing agitation from 100 to 110 rpm. This is illustrated in Table I, Quality Control Results. Lot 698031 was the first lot that utilized 110 rpm. particle size distribution was narrow ed after this change, with all other variables remaining constant. If a narrower particle size distribution is desired, a higher agitation (120 rpm) should be evaluated. The charge agitation specified in the AMP is 60 rpm. It is also rec ommended that this be raised to 110 (same as reaction agi tation) to produce a more uniform set of conditions in the early part of the polymerization and to insure the complete gelatin dissolution. A review of Quality Control results Table I, indicates that gelatin levels may have been higher than needed. The only COLORITE 015675 "\ Project NO.: SPA 674 -8- difference in formulation of lots 698O2O thru 698030 was gelatin level, which ranged from 20 to 25 pounds of each type, a 25$ increase. Screen analysis did not change appreciably during this period. In fact lot 698020 at 20 pounds (each type) was somewhat finer than lot 698030 at 25 pounds (each type). After the agitation was raised to 110 rpm, the gelatin was decreased from 25 pounds of each type to 16 pounds, a 36$ change. Again at the extreme levels, screen analyses were similar. REFERENCES 1. Inter-office memo, SPA-389 Copolymer, Capitol Records, to J. C. Fisher from D. Johnson, dated April 23, 1968. 2. Inter-office memo. Particle size Variation on T-389, to H. H. Duhamel from L. Medeiros, dated April 23, 1968 3. Marketing Justification, to L. Medeiros from C. B. Johnson, dated April 25, 1968. 4. SPA 674, dated April 26, 1968. 5. SPA 674-1, dated April 30, 1968. 6. SPA 674-2, dated May 3, 1968. 7. Inter-office memo, SPA 674, Capitol Records, to Route List from L. Medeiros, dated May 8, 1968. 8. Inter-office memo, Capitol Records Program, to M. W. Williams from J. C. Fisher, dated May 8, 1968. 9. SPA 674-3, dated May 9, 1968. 10. SPA 674-4, dated May 18, 1968. # 11. Inter-office memo. Lot 698019, Tenneco 389, to Route List from J. C. Fisher, dated May 31, 1968. 12. SPA 674-5, dated June 6, 1968. 13. SPA 674-6, dated June 11, 1968. COLORITE 015676 - 9- Report No.: SPA 674 14. SPA 674-7, dated June 12, 1968. 15. SPA 674-8, dated June 19, 1968. 16. Inter-office memo, Tenneco 389, to Route List from M. W. Williams, dated June 21, 1968. 17. Inter-office memo, Capitol Records, to J. C. Fisher from D. Johnson, dated July 8, 1968. 18. Inter-office memo. Evaluation of a 90-105-05 replacement, to P. F. Albanese from J. C. Fisher, dated August 5, 1968. 19. SPA 674-9, dated September 4, 1968, 20. Inter-office memo, 389 Copolymer, to D. Johnson from J. E. Kuser, dated September 12, 1968. 21. SPA 674-10, dated September, 1968. 22. Inter-office memo, Tenneco 389, Capitol, to L. Medeiros from J. C. Fisher, dated September 23, 1968. 23- Inter-office memo, Capitol Records, to M. W. Williams from D. Johnson, dated October 2, 1968. 24. Memo, Capitol Records - 389 Copolymer, to J. C. Fisher from D. Johnson, dated October 3, 1968. 25. Tenneco Call Report by D. Johnson on October 22 and 25, 1968. 26. SPA 674-II, dated October 25, 1968. 27. SPA 674-12, dated October 29, 1968. 28. Tenneco Call Report by D. Johnson on October 31, 1968. AVW/rjl Att. COLORITE 015677 Lot No. Date Relative Viscosity Bulk Density Heat Stability Average Contamination Screen +60 +80 +100 +140 +200 Thru Tinius-Olsen Brabender Plow, Seconds Pounds Produced Formulation Number 2593SPA 674Charge Agitation, rpm Reaction Agitation, rpm Gelatin Level (each), lbs. Reaction Temp., (P) Charge MVAc, % Bound MVAc, lbs. 90-101-05, ppm Extra Hour Reaction Time 698012 4/28 1.64 38.8 110 6/0 41 65 83 98 2 .35 940 297 39,000 -l6 674 100 100 16 152 12 9.6 -- ------- 698013 5/2 1.68 42.2 -- 8/0 2 22 52 82 98 2 .54 980 179 47,000 -17 -1 100 100 19 150 12 9-7 -- __ 698014 5/6 1.66 42.5 -- 33/0 3 22 46 73 93 7 34 1060 135 55,000 -17 -2 100. 100 19 150 12 -- -- 698015' 5/6 1.66 44.1 92 26/0 3 24 48 79 96 4 .58 1000 160 42,000 -17 -2 100 100 19 150 12 -- -- Lot 698013 698016 COLOR!TE 015678 l 698017 5/11 1.65 42.1 92 6/0 2 21 45 72 91 9 .37 1000 152 47,000 -18 -5 100 100 20 150 13 10.2 -- 698018 5/19 1.56 41.7 -- 8/0 4 28 52 77 94 6 .46 850 180 47,000 -19 -4 100 100 20 157 12.8 -- -- 698019 m 011 rH 0_1"11 aa' a 0 0 rH m d rH ft 1^ rH O 00 <J\ VO P a 698020 6/7 1.63 41.1 120 6/0 3 43 63 75 85 15 .44 930 182 47,000 L-20 -5 100 Low 20 152 12.8 10.4 100 698021 un 0 1 1--1 0rHj 0 cv a a a 0 0 rH m d 1--i ft O OJ 0 90 O'* VO -p 0 698022 6/12 1.66 38.7 92 24/0 4 38 63 77 87 13 .40 910 172 8,000 L-22 -6 100 Low 22 152 12.8 -- 200 698023 6/12 1.66 40.5 100 24/0 3 31 51 68 82 18 .40 930 155 8,000 L-21 -6 100 Low 22 152 12.8 -- 100 698024 6/13 1.63 40.4 -- 6/0 4 37 64 79 93 7 .40 910 213 87,000 L-23 -7 100 Low 21 152 12.8 -- 100 COLORITE 015679 > - 10 A TABLE I POLYMERIZATION CONDITIONS & QUALITY CONTROL RESULTS 698025 6/19 1.62 41.1 115 24/0 1 25 54 78 93 7 .54 820 None 88,000 L-23 -7 100 Low 21 152 12.8 11.4 100 698026 6/20 1.63 43.0 5/0 2 32 55 8l 95 5 .42 900 140 96,000 L-23 -7 100 Low 21 152 12.8 -- 100 698027 6/26 1.65 40.8 120 6/0 5 37 60 77 90 10 .45 920 156 170,000 L-23 -7 100 Low 21 152 12.8 -- 100 698028 7/3 1.64 698029 7/10 1.64 42.4 42.2 -- -- 6/0 5/0 10 7 48 43 67 66 83 83 94 95 65 .44 ,44 880 900 200 214 160,000 45,000 L-23 L-24 -7 100 Low -7 100 Low 21 152 > 12.8 23 152 12.8 -- 100 -- 100 698030 698031 698032 7/27 1.65 8/7 1.65 8/16 I.65 42.8 -- 41.6 120 41.9 125 7/0 14/0 6/0 62 1 46 40 27 68 66 53 84 85 74 92 8 .45 870 171 172,000 95 5 .47 920 235 170,000 90 10 .44 850 160 172,000 L-25 -8 100 L-26 -8 110 L-26 -8 110 LOW Low Low 25 152 12.8 25 152 12.8 25 152 12.8 10.1 -- -- 100 '100 100 COLORITE 015680 698033 9/5 1.65 41.7 -- 6980342 9/20 1.64 41.7 -- 8/0 2 14 42 69 13/0 Tr 18 51 72 92 91 89 .41 .42 950 910 145 123 165,000 170,000 L-26 L-27 -9 -10 110 110 Low 110 25 22 152 152 12.8 12.8 -- -- 100 100 -- -- 6980352 ^/22 *.64 .41.4 120 12/0 1 13 48 73 91 9 .41 -- 156 170,000 L-27 -10 110 110 22 152 12.8 10.3 100 -- 8 6980362 6980372 698039 10/4 10/14 10/25 1.64 1.64 1.68 42.1 41.0 41.6 -- -- -- 5/0 4/0 7/0 Tr 1 1 16 22 13 49 52 46 79 75 72 99 93 90 1 .56 920 7 .45 900 10 .39 1060 164 150 None 171,000 172,000 47,000 L-27 -10 L-28 -10 L-29 -11 110 110 110 110 110 60 22 20 22 152 152 149 12.8 12.8 12.8 11.8 100 -- 11.5 100 -- 10.9 200 * 698040 10/30 1.67 38.8 104 9/0 Tr 20 54 76 95 5 .43 1010 142 172,000 L-30 -12 110 60 22 150 12.8 10.5 200 Yea 698041 11/6 1.68 39.4 -- 5/0 1 27 56 71 88 12 .42 970 None 172,00C L-30 -12 110 60 22 150 12.8 9.9 200 Yea COliORlTE 015681 Report No.: SPA 674 698042 11/14 698043 11/23 1.68 38.8 -- 1.68 38.7 -- 11/1 7/0 ll 12 13 44 41 74 7^ 92 8 .44 990 93 7 .44 890 159 172,000 L-30 -12 110 None 150,000 L-30 -12 110 60 60 22 22 150 150 12.8 12,8 10.8 10.4 200 200 Y3 Yes 698044 12/14 I.67 41.6 -- 4/0 1 13 51 77 94 6 .38 960 238 86,000 L-31 AMP 110 60 20 150 12.8 -- 200 Yes 698045 12/14 1.68 4i.o 108 7/o 1 20 58 79 99 i. .42 1000 219 86,000 L-32 AMP j.10 60 ;8 150 12.8.' 10.5 200 Yes 698046 12/30 1.67 37.6 -- 3/0 Tr 27 64 84 96 4 .38 935 None 210,000 L-33 AMP 110 60 16 150 . 12.8 -- 200 yes 1. 8O-O29-O5 used as antistat. 2. 700 pounds recovered monomer added. COLOR!TE 015682 \ Formulation: Weight 9,140 (A) 1,340 (A) 72 13 (A) (A) (A) 17,105 - 11 - Report No.: SPA 674 TABLE II Tenneco 389 (C-2593) FORMULATION AND INSTRUCTION SFET^p Raw Material MVC MVAc TCE Lauroyl Peroxide Rozic Colic 90-105-05 D.M. Water Conditions Agitation: (A) Reaction Temp.: (A) Recovery Press: 35 psig(A) Antifoam: Colloids 58IB Antistat: 80-018-06 Charge Temp.: 125-135F - (A) - levels and conditions specified in Table I Special Instructions: 1. Charge initial gallons of water." 2. At 125-135F charge Rozic, Colic, Catalyst, and 90-101-05 (if specified) at 60 rpm. 3. Pull maximum vacuum (22 in. min.) then set rpm. 4. Charge MVC, MVAc, and TCE. 5. Charge final water, bring to reaction temp., and check rpm. 6. After pressure reaches 35 psig, react for one hour longer then dump (if specified by A). 7 Steam strip up to l85F for 15 minutes and down. COLORITE 015683