Document nk1mbaBZqJE2Z4vvvOOKjk90a

V DISTRIBUTION Research Tiles - 2 Patent Law Department R. J. Fawcett - 2 R.C. Bauman D. E. Ley - 2 J.M. Kime E. J. Sehm M. L. Dannie J.M. Foulk A. W. McRowe W.J. Kroenke D. M. Kurts D. B. Thrasher W. B. Makinen Clreulatina Copy C. f. Gibbs G. E. Stueber E.J. Donat M. R. Frederick H. J. Dintrlck \v ; cik rt ' .V J.A T-Pa s ;. o. L-.itt - d ; > Tt-cnnical C-.-ur.ctLibrarv - Cleveland R. D Scott - B M G. / M. E- Ron* D. D Ditnu-r J, ,, ' r i' . , yir v\ f ~ r r - r jU,, '' ;Q RESEARCH LIBRARY 981001 b. :t z o a iG e o z BFG08515 C00T8602 BFG08516 s' CONCLUSION- Based 'in this 11 r-r11t r: -r ,>', ;..:o mer, we conclude 1. The levels of antimony tr:. ,x.o. .w .s. : mutations car be reduces to lower b\ i levels of metal compounds which are sv.-.erxist; oxide and with a halogen source 2. Oxides or salts oi titanium, iron. load am: effective with low levels oi antimony triuxide halogen source. a.-, J. The antimony trioxide-metal salt systen s are . PVC or chlorinated polyethvlen. :r m-: i - a 4. The antimony trioxide-metal salt systems sr.ouid a wherever antimony trioxide is now used with a ham 5. Stannic oxide might be used as an antimony irxaid. economics demand it. 6. Iron oxide might also be used as an antimur.v triux: de in compositions where color is not important 7. Combinations of two or mure iio-'al sails w.:-, a: . source should impart durabilit . " tlam. r. a-: 8. At the levels tested, oxides or m line, cadmium, zirconium at.e effect with low levels ol antin. r.v <f i - a x.d> a.-e a i 9. At the levels te sted, oxides oi titanium, -ad copper, zinc, cadmium, zirconium and r.ifn not as efficient as antimony tnuxide. ..x: ., 10. Metal containing additives, suer. a flammability of polymer blends *.il V to o is e o z BFG08517 R ecommen ja : :o:.~ Baaed on this brief aurvey. we rer ir - -r. n 1. The uae of lowe r 1 e el of Sb,Oa a it1-. a. compound! auch as salts of Ti Sr, FV am ' now using Sb^Oj-helogen iuurti :. r : ,rr.< 2. Further research should be started to letorr .re " compound particle size, distribution ar.d : nr. r. flame retardant synergist. J. Additional metal oxides or salts sr. ^. i i;, with SbpOg or alone in halogen - cant.lining ,a 4. The uae of thermal analyses >: ilarr.e r.-tar-.a creased to give additional ir.:-.rm.itior. n - >' 5. The effects of all metal-Containing adci:i\e-. additives, must be considered aren testing :.,r : 20981005 BFG08518 BFG08519 ColtTt d" \ 0 RR . 2: . 4- PROCEDURES AND METHODS We wanted to study thee metal-metal jynergiims :r. * *r. mlUblt commercial self-extinguishing formulation T- r tu*t* we ueed the following recipe, which is similar to 3 f , *9129 Nat. 022: 105EP PVC Thermolite 3 1 Tyril SAN 20X17 Stearic Acid Matal Compound* 25. 0 parts 1. 5 parts 45. 0 part* 30. 0 part* 1.0 part* 1 -8. 0 part* To this ba*ic recipe we added up to 8. 0 parts antimony triox.d- arc tnm 0. 5 to 8. 0 port* of other metal compound* both with and vntho it t-.- It* ingredient* were charged a* lited and then dry blended in aOotO* blander for one minute. The (ample* were then milled (or five rrin0*0* at U0*T and compre**ion molded at 3 50* F into 2x5xl/8 bars. The s.tgff wore cot into 1/2 i S i 1/8 property bar* and u*ed for flammability, hoot dl--ertioa and food impact teat*. Ahooa *9129 K-10 Oooo 10 SEP Tyrtt CAN Max it ^ ^ toarate IsOOd Uerth y Odd* - arc commercial *elf-extingui*hing A BS Nat 02-' Lot No. 0. 0203- 1 - Commercial chlorinated polyethylene QX 224 3. io. 36% Cl BTC commercial PVC. Lot 28 132-2 Dow Chemical Co.. MX4582. 02 Crystal Let EE 90312 Blend arG ABS toughener. Lot 000024- i 2 PVC Stabilizer (S-8) - Chatman Organic Chemicals - Lubricant (L - 3) - Lubricant - M Is T Chemical Co. (Pigment F- *( ry Grado Tttanaa BANC-1 Trihoaa ViHloo PB-S - Titanium Pigment Corporation (courtesy M. - Titanium Pigment Corporation - 3PbO' PbS04 . powder (M 6 T C-r- n1: - Titanium Pigment Corporation <r .r ort courtesy of M. Dannisi Dar-.<i BFG08520 Black Iron Oxide Red Iron Oxide Yellow Iron Oxide 7inc Oxide Zinc Phosphate Bismuth Trioxide Aluminum Oxide Cupric Oxide Stannic Oxide Stannous Octoate (Car atant Catalyst) Nickel (ous) Oxide Zirconium Oxide Cadmium Oxide Pigment 104, Pigment 107, F'^O, Pigment 1 322. hydrated F< -C , Allied Chemical Co. Ri'lirr' v j r i Fisher Scientific Co. Pur; tod Allied Chemical Co. Reagent Gr.tde Fisher Scientific Co. R eagent C. rade Allied Chemical Co. , Reagenl Grade . Allied Chemical Co. Reagent Grade, Puu. drr P' 'Ad. T Carlisle Chemical Works. Inc. Fisher Scientific Co. , Reagent Grade Fisher Scientific Co. , Purified Fisher Scientific Co. , Certified Trir-mT Tests Tbs flammability of each sample was determined by applying a pmtorck flams St a 49* angle to the cross-section area of a horizontal 1 . 1/2 a 1/1 a 5" molded bar. The head of the torch was held a. a distance of about 1 1/2 inches from the end of the sample. The flame front tboradnre colored tbs sample cross-(action and the length of the bar for about 1 1/2-2 Inches behind the cross section. FIGURE 1 SCHEMATIC DIAGRAM OF FLAMMABILITY TEST APPARATUS rS-Mig ss -rti. a 4X9/ BFG08521 We also obtained the Oxygen Index of a number uf the sir fereatlal Scanning Calorimetry (DSC) runs ere also -ota.r.eelected sample e. RESULTS AND DISCUSSION Metal Oxides or Salts with a PVC Halogen Source IMtocsr Trioxide Samples were prepared following the basic recipe withfro-nu. u :.. 8 pasts S^Ob- The results of the flammability testing are listed in Table A aamber gives under "first name," etc.. is the time in seconds require.1 for *sl sample to extinguish after the flame is removed. Other terms ir self' descriptive. The same applies to all the other tables TABLE 1 FLAMS RETARDANT PROPERTIES OF ANTIMONY TR I > ample No. Parts SbgO, First Flai 4074-1 4000-11 4000-14 4000-15 4074-7 4000-14 4000-17 4074-0 4074-1 Abeoa 04129 1.0 2.0 J.O 4.0 4. 0 5.0 6.0 8.0 8o Burns Burr, o <i <i <i <i <i <1 <1 <t SfM bsll b E rt8 6 @ e BFG08522 T Antimony trioxide doe* have * measurable eltect r. guiebiag properties at low levels But ar -no ' to o par i ajsy lM|'Urm benefit*. Titanium Dioxide TABLE U FLAMS RETARDANT PROPERTIES OF TITANIUM DIOXIDE *t--F*- No. Parts Subpig Parts RANC-I Parts Sb.O, 1st Flame 2nd Flame >r i Fiarr'.t* 4074-4 4074-3 4074-4 4074-7 4074-0 4000-i 4000-4 4000-2 4074-1 4074-4 4000-7 4000-7 4000-11 4000-3 4000-4 4000-0 4000-10 4000-12 4074-2 4074-3 4074-3 1.0 3.0 3.0 3.0 .-* -- 0. 5 1.0 0. 3 1.0 3.0 0. 5 -- -- 0. 5 10 0. 5 -- -- 1.0 3.0 1.0 0. 0 -- 2.0 7.0 5.0 10.0 0. 0 -- -- -- -- 0. 5 0. 5 1.0 -- 0 = 0. 5 1.0 -- ... ... 0. 0 -- -- -- -- -- 1.0 1.0 2.0 2.0 2. 0 2. 0 2. 0 2. 0 30 5- v i . -j JL 3 - -j 4. 0 0 b. u Burns Burn s Burn* Burns Burns Burns- 1. 5 8. 5 2.0 2. 0 <1.0 <1.0 <1.0 8.0 <1.0 <! G < . i. <. - < j <i J <. j ... -- -- -- -- 8. 0 4. 0 5. 0 8. u Burns 33 4 - - - .._ -- -- -- -- --Burns 3u r n i BurnB r- , Although neither type of titanium dioxide app-ars g-1- retardant by itself, both type* shu* levels of IhgO,. . r ***** 20981010 BFG08523 r~ 10 V* observed a trend toward* increased t'lam/i-.abill! . HtMU wai addad. Fot example, tamp . 4074-4 witn } jir:s '.C, tb* second flame application. Sample 407t>-i with 1 part T-.O, .'.r.y.nsattar S aac and 4076*2 with 0. 5 part* TiOa extinguishes after - sec OOCOad flam# application. We obtained the best results in j'j: :'.irr.>- vs v6m either 0. S parts active subpigmentary, or 1.0 parts RANC-1 ,.iudinsida was incorporated into the recipe with 3 0 parts SbaOj We incorporated lead salts into the basic recipe by replacing h. i ThermoUte 31 PVC stabiliser with 3.0 parts Tnbase (3PbO PoS04 bn 1.0 part stearic acid with 1.0 part of lead laurate . No other '. eve; li war* teeted. lit does in Table 111 ehowt that the most efficient lead-antimony ru in 4 parts load MU* and 4 parta antimony trioxld*. The use of 4. 0 part 5 load safes alane does not efficiently reduce the sample flammabil-ty. TABLE 111 fLAMS RETARDANT PROPERTIES OF LEAD COMPOUNDS hapls Mo. 40*4-1 -t 3 -4 -1 4 -T 1 Parts Load 4 4 4 4 4 4 4 4 Parts Subpig. TiO, ... ... __ -- 0. 1 0i 0. i Parts Sb.0, 0 l 2 3 4 1 2 3 1st Flam* Burns <1.0 <1.0 <1.0 <1.0 <1.0 <1.0 <10 2nd Flame ... Burnt 3; <1.0 1.0 Burn* i. s 2. 0 3rd Flarr.t -- -- Birr- Bl; r n ; .. * -- Burn* - The caenbinetion of 4. 0 parte lead salts , 3.0 pttrt so,0. *n : titanium dioxida is also efficient but f.r> _________ near just 0. 5 parts subpigmentary !i'm.::. parts antimony trioxide (sample 4080- 3. Table 11) L. TT0TS602 BFG08524 We teeted three different pigment ^rade* of iron oxides -- b'.ao : Mtie (Kgmtot 104), red (Pigment 107) and the partiallv hvdrat.-d <?" a (PiglBMt 1)22). templet 4102 1-3 and 4102 5-7 were compounded mmy TWnMUu 31 PVC etabiliter since iron oxide it a PVC ttabilizer a: mi proceaeing temperaturet. 24 And rather than 1.0 par: stt-a.-ic 1.0 part calcium atearate wat uted for lubrication in all the irun " la Table IV, tamplet 4102 1-3 ahow that 3 and 5 parts of iron inhibit burning to tome extent. But 4102-4 ihowi that 3.0 part ed iroa aside plat the Thermolite 31 ttabilixer level normally used e;v. - a TABLE IV FLAME RETARDANT PROPERTIES OF IRON OXIDES fcaaplt Me- 4102-1 -3 -4 4104-1 410V1 3 4102-9 4104-4 3 4I0V4 9 Parte Iron Oxide 1.0 ).0 9.0 3.0 1.0 1.0 9.0 1.0 3.0 9.0 1.0 3.0 9.0 3.0 1.0 3.0 1.0 3.0 Type Iron Oxide 104* 104* 104* 104 107 107 107 1322 1322 1322 104* 104* 104* 104 107 107 1322 1322 Parte bOb -- -- ... -- -- -- -- ... -- 3. 0 30 30 3. 0 3.0 3. 0 3.0 30 lit Flame Burnt 36. 0 28. 0 2.0 23. 0 14. 0 2.0 2.0 4.0 2. 0 1.0 1.0 1.0 <10 <1.0 i. u <10 <1 0 2nd Flame ... Burn s 24.0 21.0 11.0 17.0 9. 0 Burns 12. 0 13. 0 2. 0 i0 v ' i 2. ; i0 2. 1 :. - 4-O o 3rd Flame ... Burns 39. 3 45. 0 44. J -- 3 5. C 37 0 4' 1 ** 4 4 fs u 5' 4th Flam ... ... - -- *Ma Thermolite 31 added I 8 X 05 H* o is) G HK lylttm that is (elf-extinguishing in a shorter period data we conclude that the organotin staoihter is also syn.-r*: .tit eithar with tha halogen alone or with the iron oxide-ha'-'iier. The rad iron oxide (107) and yellow iron oxide i l 31 2) ai-j a- ing rate when Thermolite 3 1 is present However in. c i aide with 3.0 part* of SbyO, is a very effective flan-- n tartar: Samples of these systems (4102 5-8. 4104-4, 5. 4103-4. a tiagoishing through four flame cycles Samples 4 10 2 5-7 exhiti without the organotin stabiliser, and 4102-8 show s further i-.pr , tha Thermolite 31 in the recipe. All iron-containing samples tF colored- AU the iron oxide-containing samples had increased c caased by "blowing" of gases through the hot char After*:..u >. oa tha longer-burning samples. Iroa-Titanium Oxide Virflux PR -5 is a ground, natural'.! jcc.irrin* :> r titanium dioxide the ferrotitanate is not effective ir. t However, whan small amounts of the ferrotitanate and i foar-are added to the basic recipe, the resulting samples -.as e drcrrin inability- Again, as with titanium dioxide, onls a 0. - oar: '. j:.-. TABLE V FLAME RETARDANT PROPERTIES OF A FERR ample No. 4041- l 2 -3 4 -5 -ft -7 1 Parts Virflux PR - 8 1.0 3.0 5. 0 0% 1.0 2.0 3. 0 4. 0 Ha rt s fjbsOj __ _ -- 30 3.0 3. > 30 3. C FI Air. t: Burn* Burns Barm <; o <. 0 <i.O <1.0 <o Flu.... --- .0 3 .w" " ._ \-t if n feTOTseOK BFG08526 r r c 13 a3 Mac Oalde and Zinc Phosphate TABLE VI FLAME RETARDANT PROPERTIES OF ZINC SAL.75 Parts Parts Parts ZaO ZnPO Sb*0, Parts FetO, 1st Flame 4114*1 2 -3 4 .4 4113-1 a -3 4 4 -7 1 1.0 3.0 s.o 1.0 3.0 S.O ... -- ... ... ... ... ... -- ... ... ... -- ... -- 1.0 3.0 S.O 1.0 3.0 5.0 1.0 2.0 ... ... -- 3. 0 3.0 3.0 -- -- -- ... ... -- 3. 0 3. 0 ... Burns ... Burns -- Burns --< --1 -- <1 -- Burns -- Burns -- Burns 3.0 12 3.0 2? 30 23 -- <1 ... <1 <ind F1rr. e J j 3 i: 6 7 <i i F'.a.-.r- ... 4? 3* 3 B . ' r. s .a 44 =*0 4? 2^ - 3u 3. 20981014 ZUc oxide mad sine phosphate mlone do not efficiently crcre-r flammability of the resin system With 3 0 parts SbjO, added pkllS systems can pass three flame cycles while 'he tine ytM (sly two flame cycles. A combination of zinc phosphate x - also decreases the flammability of the system, oat the ta extinguish are rather long. Biomoth. Alummum and Copper Oxides Ths oslde of bismuth alone decreases the flammability gataaa, hat the times to extinguish are long The oxides ot a tlfpsr da aat effectively decrease the reai- flammability atthe!-\VMk ).0 parts of ShgO, present, along with a 3 0 part leve. : j modal amides, the materials can still be classified as e lev.' . aRsr faar flame cycles. a-^sm rm.mmrn * - * Wm 14 TABLE V1J C o . e rr a n RR, 2. 14- 4114-1 2 1 -4 1 -4 -7 - -4 Parts Pint Parts Parts M0. AWO, CaO Sh,0, 3.0 0.0 3.0 --- ... -- 3.0 3.0 3.0 -- -- -- -- -- -- -- -- 3.0 $.0 3.0 ... -- 3.0 -- -- 3.0 -- -- 3.0 1st Flsme 39. 5 25 0 3.0 Burns 60 <1 Burns Burns <1 2nd Flame 410 5. 0 1.0 -- Burns 1. 5 -- -- 39. 5 3rd Flame 49. 0 32 0 10 -- -- 4. 0 -- -- 4. 0 4th Fla rr.e Burn 5 B'jrni 3 5. 0 -- -- 1 0. t ... 11 M TABLE VIII Parts Parts 8*0, 4247-4 -3 -4 4233-4 3 -4 4247-7 1 0 10 4233-7 3 -0 -10 -11 -12 1.0 2.0 3.0 4.0 3.0 4.0 2.0 3.0 1.0 2.0 2.0 4.0 4.0 3.0 4.0 4.0 -- ... ... ... ... 1.0 1.0 2.0 2.0 2.0 2.0 2.0 2.0 3.0 3.0 1st Flams 45.0 23. 0 14. 0 4. 0 1.0 1.0 <1.0 <1.0 <1.0 <1.0 1.0 <1.0 1.0 1. 0 <1.0 l. 0 2nd Flame ... 27. 0 20.0 8.0 7.0 4.0 2. 0 1. 0 1.0 1.0 1.0 <1.0 1.8 1. 5 1.2 1. 3 3rd Flame .. 34, o 9. 0 4. 0 3.0 9. 0 4. 0 o. 0 5.0 8- 0 R. 0 4. 0 40 10 5. 5 20 4th Flame ^8 j 20. J ... 0 27. 0 In. 0 24 : i 3. u i> J 15 C 1J '.0.0 . la ) L 'H *T ' ' r*- lie oxide llOM appears to be in efficient ftime re'arda.-' a hlllfM MirM It ibeat 4.0 to 6.0 ptrti. It does not *e'.!-ext in* . - a ^cnir 11 does ii equivalent weight of intimony oxide lire Titi'.e : Wlf till more efficient through mo re total flame cycle, than ar.t.n. n. i low levels of itinaic oxide ire combined with low levels ,i ant. i. 1 CosaMaatioo of the effect* is seen. Simple 4235-8. contain:-,, ftftl of kO| lad 2 pirts of StfcO* i* *elf-extmguihing through four flart.n CytUl il aider 4 eecoode per cycle. This i* in improvement over t> par's of eMber oxide iloae (Tible* I, VIII). The mijor drawback* to the uir f oxide ire ll iacreieed emok* emission problem, and the cost : xide which is now about competitive with intimony trioxide Hj a use of low levels of til oxide to impart durability to the flan., property cannot be overlooked. lid Antimony Oxide* TABLE IX FLAMS BETAS DANT PROPS* TIES OF TIN WITH TITANIUM AND ANTIMONY OXIDES *5f* hrti Forte BANC-1 TiOg Ports Sb.O, 4MB-1 1.0 0. 5 WWW 2 1.0 1.0 -- -J 2.0 0. 5 -- 4 2.0 1.0 ... s.o 0. $ -- -4 2.0 1.0 W-w 7 4.0 0. 5 -- 1 4.0 1.0 -- 4249*1 1. i 0. 5 1. 5 2 l.S 1.0 1. 5 1 2.0 0. 5 2.0 4 2.0 1.0 2.0 4MT-10 2.0 WWW 2.0 1st Flimo Burns 26 22 22 7 2 11 15 <l 2 <t <1 <1 2nd Films WWW 11 4b 27 2. 5 21 3.0 5.0 -.u 1.3 <1 2..0 1.0 3rd Flame ... Burns ... 12 4 * . 54 4 4th Flame ... - * 4 TBo eee ef titiiium dioxide with tin dtos* It doe* not r ; tB* eyeteoi moeh more efficient. In fact. when titanium dioxide * 11 sdflrisst Itaaiic oxide system, it decreaece the efficiency .! BFG08529 Cole mar.. \i' .6 RR , 21 ; 4-7'. . 4 SUmobi Octoate TABLE X FLAME RETARDANT PROPERTIES OF STANNOUS OCTOATE Sample No. Parts So Octoate Pa rts Sb^O, 1st Flame 2nd Flame 3rd Flame Flarr.r- 4254-1 -2 -4 -5 3 ... 3. 0 45. 0 Burns ... 4 --- 3.0 43. 0 67. 0 -- 3 1 <1 51.0 52. 0 : i. ! 2 2 1.0 8. 0 84. 0 2 4 1.0 1.0 1 4. 0 48. l- octoate is less affective than stannic oxide either ilo.-.r vr i aatioooay trtoxide. It is of interest because it is an organornetaliic I (fee TVermolite 31) rather than a metal oxide. Stannous octoate appear- I too volatile since its effectiveness decreases rapidly with the mcreasMotor of name cycles. A less volatile organotin compound might Or o effective. Ctfmimm aad Zlrcoeium Oxides TABLE XI ME RETARDANT PROPERTIES Or CADMIUM AND ZIRCONIUM OXIDES Sample No. Parts Parts CdO ZrO. Parts ShgO, 1st Flame 2nd Flame 3rd Flame 4251-1 2 -3 4 5 4 42*2-1 2 3 4 -5 -4 2 4 6 2 2 3 ... ... mm mm m ... ... m mm ... -- -- ... - .. 2 4 4 2 2 3 ... ... -- 1 2 l -- ... -- 1 2 ' Burns Burn* Burns 40 1.0 32 Burns Burns Burns 1.0 1.0 1. 0 ... ... -- 67 i3 32 -- ... -- Burns 2. 0 6. 0 ... ... -- ... Burns 36 ... -- -- Bu rn 3-rr. s rt > TOTSGOZ BFG08530  ClfallUB And zirconium oxide* alone are not difr... ,, I daat syaorgists lathi* halogen*containing tyilem When c.Tbu lavals of 88,0, . there it tome positne elf.ct seen pn* k these HmpUl i* ttiU too high. Michel Paid* Although nickel oxide alone i* not an efficient ilame rets r nur. It Am* add *ome durability to a system with low levels ; SbaO, Tlag time* are rather long after the second flame cycle However t` r glee containing nickel oxide did "blow ' to form higher volume s f* s s - TABLE XII i>, FLAME A ITAR DA NT PROPERTIES OF NICKEL OXIDE temple No. Parts NtO Parts Sb.0, 1st Flam* 2nd Flame 3rd Flame 4t-. Fla rr. 4-l 2 3 4 *5 -6 2 ... 53.0 ... ... 4 -- 63. 0 -- ... 6-- 2.0 Burn* -- 21 5.0 20 26 22 <1 2. 0 30 31 1. 5 54 26 __ -- 8b 40 56 >* with Chlorinated PE Halogen Source T# farther demonstrate the utility of two of these metal -n gist system*. * prepared a polymer blend containing chlorir.a lyao* (X* Id, J*% chlorine) with a total halogen content j: ; 4 4' lacipa: K-10 Thermolue 31 AN BOX IT Stearic Acid 40.0 parts 1. 5 parts 36.0 parts 24. 0 parts i. 0 part*. Pregerty bars were prspared and tasted for flammability dard way* The results in Table XIII show that trie titanium d; . .d< Uteride and iron oxidn-antimony trioxiae synergism. *>*' >: s *.- la redeflag the flammability of this polymer blend. 20981018 BFG08531 TABLE XIII EFFECT OF SYNERGISTIC SYSTEMS USING CHLORINATED POLYETHYLENE *2* 41IT-1 a a Hart* A V e s s Ptrti RANC-I TiO, ... 1 -- Part* Fe.O, . . . -- -- 3 1 ft Flame Burn* <1 1.0 1.0 2nd Flame <1 4. 0 2. 5 3rd Flame ... 2.0 Burn* 6. 0 4t r, r:r. -- -- o. 0 M Ibte (b^ ), or Limiting Oxygen Concentration (LOC) i MtltaHl telt method for rating the flemmebility of pUitici 1* (ho Bar Coat oxygen In N^/O* mixture required to just i ml of n polymer tempi* under the test condition*. CorreUf1--i*MUt| wider actual u*e condition* he* not been eitebliihed. loo* (O doecrihed elaewher*. 1 > 25 We have obtained the oxygen index I vMabvefattwere the bait *elf-extingui*hing material* that Thto data era* obtained on a OE Oxygen Irdex Flammability to our laboratory. risen of the Oxygen Index data and the data from the prop*:- re a major difference in the re*ult* obtained oy difi< r-. The lover burning temperature* vn the candle-'.ixe ..v.,. toot eoboace the effectivene** of iron omde* *i ilan-.e - iron oxide*halogen *y*tem i effective at .u-*.-.' ti-rj.L : a , OV 1000-halogen ayeteme. Likewise. the SnOj ivitcti-.s a IBbo moro ftemmnble in thi* lee evert test imctr a higher tempera'. . ru^SruSt* efficiently generate the SnCl, than the FeCl, The more ic tereb teat revar*aa this order. Thermal analytes eupp.r' icanniao Calorimetry (DSC) OBCdate wr obtaiaad for samples ol PVC, AB>'HVC VFVC M**d cofttaiamg 1) 3 parte SbgO, , Z) 3 parts 61018602? T Coleman. Nierv.a19 RR. 21 1-4-70 - . TABLE XIV OXYGEN INDEX (n^) OF EXPERIMENTAL SAMPI ES tll~|`- No- 4123*1 2 3 4 -3 -4 -T 1 -* -10 11 -12 -13 14 IS -14 IT Part* *v>* t 0 3 3 3 3 4 3 0 0 3 3 3 0 1 2 Other Additive( ) WWW -- -- --- Subpig TiOs BANC-1 TiO, Vlrflux PR-5 Pb* Pb* r%o, Fe,04 FegOg- XN*0 SnOa/TiO. SnO. SnO, Part* Other(a) WWW -- -- -- 0. 5 1.0 35 4.0 4.0 3.0 3.0 3.0 3.0 3.0 3.0/0. 5 3.0 2.0 no,l*0- 27. 7 22.0 23.8 27. 7 24. 5 24 5 24. 6 24. 9 24. 2 30. 7 29.8 31.4 31.6 318 23. 2 24. b 25. 0 tibaMMlN *Aa ). Opart* Tribaae and 1 part lead laurate TVaraoUte 31 added 3) 3 part* SwOg, 4) Sparta SnO, and 1 part TiOa , and 51 3 parti Fe,0, pwlladiary run* lha that the SbgOg, SaOa and FetOa-containing . Mt different reaction pathway* during decomposition The mdica- Bat promote a earlier PVC decompoaition than SbgO, . or h* idEtiee a( TtOg appear* to retard the action of SbgOa making mi* reefleetiveat the burning temperature. The TiOg alao appea r j MiaaafbO, with HO from the PVC making tni* ccmoina- ua*U higher temperature* are achieved. Thi* data help* fcp 1*4*1 aside ayatema have a higher Oxygen Index (Table X!V ^ #* InOg syatern* lathi* thermally lee* *evere candle type tr' dal Ike low Oxygen Index for the SnOa and 5nOa-TiC, cample would not becoTie aynergiatically active until hig terr.pe re1 .: - m I r BFG08533 i? Colerr.an. N.crr.d-r 20 R R 2 1 14 - ' 0 . 1 ^ *T (WaiaH. Farther work should be done with DSC, TGAandDTAas corr.irf mm thods for understanding flame retardant mechanisms Finrttn of Some Compounded Systems The Nif profertioe, other than flammability, that we tested were the heat CMHttM lemperatare (244 pal, onaanealed) and notched Ltod impact t memONperaierw. These are listed in Table XV (or several of the sysMM> The ThM* is incomplete since not all systems were tested. However II 4mo shew that these properties are not detrimentally effected when low levels ad metal eelte are added to the basic recipe. TABLE XV wnCT or AOomvES on physical orproperties polymer blend Other AddUfarefs) Parts Otherfs) HOT, *C (244 psi) Isod Impact Ft-lbs/ia notch Mias 9.9 dNSAfi * hi 1st hh 4#" hi hi Wijr Ssi 9.9 S.I hi 4Wh LI VWUs PS-5 M Lead* lji4* NQ.t rA PegOe (#104) Pn#0, (#104) ra#ot (#1322) regO*(#1322) ... 1.0 0. s 4.0 4.0 3.0 3.0 3.0 3.0 3.0 3.0 3. 0 74-70* 75. 5 00.0 74. 5 ... 77.0 74.0 74.0 74.0 75.0 75.0 76.0 2-2. 2 6.0 3.7 5.0 3.4 3.7 3.2 2. 5 5. 7 4. 1 5. 4 3.0 *Al --%ptr and lead laerate izm sG oz TJLaA T- F. Niemann 14 a 21 Coleman. N;e.: aRR, 2114-70, = . ACKNOWLEDGEMENTS W twH like to thank Mark Dennis for his many helpful idea* and jattaaa 4vlt| the course of this work. We are also indebted to him 1 garaishtac a number of the additives studied. Ve a said eleo like to thank Frank Baron at the Avon Lake DevelopCaaCer lor obtaining some of the Oxygen Index data on our samples- it. 20981022 t T' * BFG08535  C ' . e r . d r. rr :.. 4* REFERENCES C.J. HiUdc. "Flammability Handbook (or Plastics ford. 1949. Tec.nr. .m:. M-J. Boatmans and I. L. Phillips (to Philadelphia Textile Fir.;-v-s tec.). U.s. Patent 2, 547,671, April 3. 1951 C. C. Jehaaoo and R. Thomas (to E. 1. duPont de Nemours a.'.c C. U. S, Patent 2,494,391. January 10, 1950 V. L. Dills (to E. I- duPont de Nemours and Co ), I S Patent February 9, 1994. - 0. H. Biedl(toR.S. Robe), U S- Patent 2,805, 1'fe Septemoer 1. V. 9f. Riche a (to E-I- duPont de Nemours and Co.). US Patent 1, TBS.041. March 12, 1957. W. L. Dills (to R. 1. duPont da Nemours and Co.), U- S- Patent Z. oG~ if. iT*a. W.f. SelUeaa aad LM. Paoik (to National Lead Co.). U.S. Patent 1.4IR.SP0. Noeamher 3, 1953. R. DahlStrom aad C. E. Bronson (to National Lead Co. ). U.S. Paten' 1.4TB. 297, February 23, 1954. 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