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FILE NAME: Johnson & Johnson (JAJ) DATE: 1960 Mar 8 DOC#: JAJ034 DOCUMENT DESCRIPTION: Report - Phase Report on Pilot Plant Beneficiation of Italian Run-of-Mine Talc- Presented to J & J Research Protected Doeument-SuWeetto Protective Order JNJAZ65JW0000677 BATTELLE FIELDS OF RESEARCH AfKMAUIK Al INfilHI IWHI. A6irin iuiai rm mu ai;. Altor nrvnorMibii ANAi.riifAi (iiiMiMity Amito MAtlIlMAlll s mocmmimkv monn(.k 5WIOIMO AND IN'.INIIIINl. MAIIIIAl.'i CAUIYIS AMI SIHFAI I (tilMI!.IIV chamo CHCMICAl INCINCUIN< CHGMtCAl NIOCHin COMOHON ICCHNOIOHY COMPUItl CNOINtrKINCl (CONOMICI n td M rA i in o in iih n o UlECtlOCHfcMlCAl moiMUMNIi mtlIOCHlMItlIY TRACIIVl MUAIMIim i *cTMo nim MMOUS MllMHmr.Y EOUNBIY PIACIKI POOO TlCHNOIOOY fUflt ANO COMUSIION CIAHIIC AHI ICCHNOIOOY OIAH Iff HNOIOOY ihoh.iimmuiaiuy MPiAiiumv HUMAN MNUNIIIMn IMMllNOlORY ANI f'ANCIl SUIOIRi INPUtlMAl HIYSICS INKMMAIION PIOtlSSINU INONSANir riIIMisil IN SlIUM tN lATtO N llt '.lll A llO YS ANO M il MOTAIS IUM ICANT TCCHNOLOOV M TQtANJCAl IN S IN K NQ MI1AI PIM IM NO M IIA IIU M IC A t H O CU SES MINI IA IO O Y ANO MlCIOSCOPY mmumu mocumno M lCtOUOIOOY NOFEMOOS M lTAUUIOV NUClfQ M CS OPUAHONS IIS lA lC H O lA N lC C H lM IS m O tCAN IC COATINOS rrn o C H M iC A is it ik s h u m in o in im k io PHYSlCAl CHEMISTRY p h a im a c e u t ic a i CHCm U T I FIO IU C IIO N ENOINECUNO M IU ANO PA N TtCHNOlOOY RADIOISOTOPES ANO IAOIATION IIIIA M U 1Y R W IN in iIN C H A C rO I 1 K K N M 0 9 V WEPIACTOIMS IM in AND HASTICS HMtCONOWCTOM AMO SOLID-STATE D CVICS s y s iim s n n ih in c le im o s a n o p u r s Y H C O ie riC A t A N O A P P U M EC H A N IC S THCBMOOYNAM1CS WILDtNO ANO METAIS-JOINPTO TECHNOLOGY wood ano routr piooucts t Mb Protected Documont-Subjoctfa>ProtaetfvOrder JNJAZSSJM0000578 BUSINESS CONFIDENTIAL PHASE REPORT on PILOT-PLANT BENEFICIATION OF ITALIAN RUN-OF-MINE TALC to JOHNSON AND JOHNSON M arch 8 , 1960 by R, W. Schatz BATTELLE MEMORIAL INSTITUTE 505 King Avenue Columbus 1, Ohio Batttll* is not engaged in research for advertising, sales promotion, or publicity purposes, and this report may not be reproduced in full or in part for suck purposes. BUSINESS CONFIDENTIAL Protected Document-Subject to Protective Order JNJAZ55_000000579 BUSINESS CONFIDENTIAL Battelle Memorial Institute 5#B KI HO AVENUE COLUNEUS I. O H I O M arch 28, I960 M r. W. H. Ashton Johnson and Johnson Research Department New Brunswick^ New Jersey Dear Mr. Ashton: We a re p lea se d to tra n sm it six copies of o u r P h ase R eport, "P ilo t-P lan t Benefielation of Italian Run-of-Mine Talc". As pointed out in the report, the runs w ere quite successful in that a superior talc product of high luster and platlness was obtained at a high recovery. Sincerely yours, OFT/m in Enc. (6) cc: D r. W. H. Lycan M r. 0. V. Swank BUSINESS CONFIDENTIAL D E D I C A T E D TO THE A D V A N C E M E N T OF SCIENCE Protected Document-Subject to Protective Order JNJAZ56_000000580 BUSINESS CONFIDENTIAL TABLE OF CONTENTS 4 INTRODUCTION AND SUMMARY......................................................................... PB* 1 SCOPE OF PILO T-PLA N T WORK. ...................................................................................... 2 GRINDING IN V E S T IG A T IO N ................................................................................................. 2 C rushing ............................................................................................................................. 2 Grinding ............................................................................................................................. 2 B E N E F IC IA T IO N ............................................. 7 OPERATIONAL P R O B L E M S .................................. ' ......................................................... 7 CHARACTERISTICS OF PILOT-PLANT PRODUCTS....................................... 14 SAMPLES SHIPPED TO JOHNSON AND JO H N S O N ........................................'. , . 14 CONCLUSIONS AND FUTURE WORK............................................................................................14 B.A T U L L E MIMOAIAL INSTITUTE BUSINESS CONFIDENTIAL Protected Document-Subject to Protective Order JNJA25SJM00MSS1 BUSINESS CONFIDENTIAL PHASE REPORT on J PILOT-PLANT BENEFICIATION OF ITALIAN RUN- OF-MINE TALC to ' JOHNSON AND JOHNSON from BATTELLE MEMORIAL INSTITUTE by R. W. Schatz M arch 8, 1960 INTRODUCTION AND SUMMARY Laboratory work* had shown that a superior talc product could be produced by wet grinding and flotation of Italian run-of-m ine** talc. Consequently, Italian run-of-m ine talc was processed in the pilot plant to dem onstrate the technical feasibility of the proc ess and to obtain drum quantities for panel testing. The treatm ent procedure was as follows: after ham m erm ill crushing to minus 1/4 inch, the talc was ground wet in a pebble m ill, in closed circu it with cyclones, to approxim ately 98 p e r cent m inus 200 m esh. A fter rem oval of the m a jo r portion of the minus ld-m icron fraction in other cyclones, the platy talc was recovered by flotation, filtered , and spray dried. Sixty to sixty-five p e r cent by weight of the feed to the plant was reco v ered as a su p erio r talc'product. Deionized w ater was used throughout the process. The beneficiated talc was a t le a s t 99 p e r cent platy, analyzed from 0. Z to 6. 3 per cent COg, contained about 12 to 13 p e r cent of m inus 10-m icron m a te ria l, and had a lu s te r higher than e ith e r the p resen tly sold baby powder o r the beneficiated Italian No. Z talc. Progrs, Report, "The Phytictl Concentration of T slc Ores'Flotation of Italian Run-of-Mine T ile ", December 31, 1969. ** Hereafter abbreviated n ROM. BATTELLE M EMORIAL, INSTITUTE BUSINESS CONFIDENTIAL Protected Document-Subject to Protective order JNJAZ55JW000052 BUSINESS CONFIDENTIAL 2 SCOPE OF THE PILOT-PLANT WORK The pilo t-p lan t study of the beneficiation of Italian ROM talc was com posed essentially of two phases.. The firs t was to determ ine the operating conditions required in the grinding circu it to produce a suitable wet-ground talc for flotation. The second was to establish flotation conditions for the beneficiation of the wet-ground talc. Thel first phase was completed in the last half of September and the firs t half of October, 1959. The flotation phase was completed by the m iddle of Novem ber, 1959. GRINDING INVESTIGATION The g rin d d e sire d on the Italian ROM tale was 98 p e r cent m inus 200 m esh with a minimum of minus 10-m icron m aterial. Equipment in the crushing and grinding c ir cuit included a h am m erm ill (4)*, pebble m ill (8), two cyclones (10, 10a) together with the n e c e s s a ry pum ps (9, 9a), conveying (3-5), storage (6), and feeding (7) fac ilitie s. A feed ra te of about 450 pounds p e r hour to the grinding circ u it was d e sire d because this rate was the approxim ate capacity of the beneficiation section of the pilot plant. Crushing The ROM talc was received in burlap sacks (150 pounds p e r sack) and had been crushed to about m inus 2 inches. In o rd er to m aintain a fixed storage'bin level, three sacks of talc w ere erufched p e r hour; two on the hour, one on the half hour. The ham m erm ill product was nominally minus 1/4 inch in else. Table 1 .presents typical screen analyses of the ROM talc before and a fte r ham m erm ill crushing*. Grinding The following general plan was used to determ ine the operating conditions required far the desired grind. F or each set of conditions the circuit was first operated for about 4 hours to establish equilibrium. After equilibrium had been reached, as de term ined by pulp density and volume m easurem ents throughout the circuit, the required samples were taken over a period of 2 to 3 hours. Based on the analyses of these samr p le s , changes w ere m ade in' the operating conditions, and a fte r equilibrium was reached, the circuit was again sampled. This procedure was repeated until the desired operating conditions w ere established. * Foe oqjitpmsM pacification* ise coneiponding identification number in die Hiaie Report "Design and Construction of a Tate Flotation Pilot Plant", December 30, 19*9. BATTELLE MEMORIAL INSTITUTE BUSINESS CONFIDENTIAL Protected Documm t-Subjact to Protective order BUSINESS CONFIDENTIAL 3 The initial te s ts , started on Septem ber 18/ 1959, were made using die pebble m ill (8) with 1500 pounds of 1-1 /4 -in ch porcelain b alls and die 4-inch (No. 1) sh o rt cyclone (10). It was soon apparent that insufficient grinding was being obtained in the m ill, and, th e re fo re , die pebble load was in cre ase d to 2900 pounds. Additional runs were made using the one cyclone with various apex (discharge) openings, feed and over flow d ischarge p r e s s u r e s , and pulp densities. The fin est grind reached was 90 p e r cent m inus 200 m esh with about a 20 p e r cent m inus 10 m icrons. It appeared that, to reach the d esired grind, it would be n ecessary to use No. 1 and No. 2 cyclones in series, i. e . , the second cyclone retreating the overflow from the firs t, with the underflow from both cyclones returning to the pebble m ill. A fter con siderable experim entation with this circ u it, operating conditions w ere established which gave a grind of 98 p e r cent m inus 200 m esh with 25 to 30 p e r cent m inus 10 m icrons. This grinding investigation was com pleted on October 15, 1959. Figure 1 shows the flowsheet of the grinding circuit. Typical operating date, as well as an approxim ate w ater-solids balance also a re shown. Table 1 gives typical screen sice analyses for the various points in the grinding circuit. Tables 2 and 3 p resen t additional operating date: volum es, pump densities, w ater requirem ents, cyclone operating p ressu res, and efficiency calculations. The circulating load and classification efficiencies of Table 3 are worthy of com m ent. The circulating load of 660 p er cent is rath e r high for a conventional ball m illcyclone c irc u it. - In addition, the classificatio n efficiency of 21 p e r cent (based on r e covery of minus 200-mesh m aterial fed to the cyclone circuit) is low. At le a s t two factors contribute to these conditions. One is the platy character of talc. As p article shape deviates from a sphere o r cube,, classification becomes m ore . difficult, and in a one-pass operation m ore inefficient. In addition, a 98 p er cent minus 200-m esh grind with le s s than 0. 3 p e r cent on 100 m esh is a difficult g rind to rea c h , particularly with a platy m aterial. Excellent rejection of the plus 200-mesh fraction m ust be obtained, and fids is only accomplished at the expense of recirculating a con sid e ra b le quantity of finished (minus 200 m esh) product to the pebble m ill. The effi ciency of rejection of plus 200-m esh m aterial was excellent: 99 per cent, a s shown in T able 3. F u rth er experim entation with the grinding circuit m ight lead to a grind of 98 per cent m inus 200 m esh with le s s than 25 to 30 p e r cent of 10-m icron m a te ria l, as well as lower circulating loads and im proved efficiencies. For an investigation of this sort, 24-hour (continuous) operation would be necessary with m inor changes in the circu it from tim e to tim e. This type of an investigation is one that is b est made in an operating plant because the effect of each m inor change will be email and a number of days of operation under each set of conditions a rs necsssary to establish the effect of the change. It is B attelle's opinion that im provem ents in the grind can be m ade which will reduce the quantity of minus 10-m icron talc. IATTIU I MEMORIAL INSTITUTE BUSINESS CONFIDENTIAL Protected Docum snt-Subjsct to ProtecUv Order BUSINESS CONFIDENTIAL 4 FIGURE 1. PILO T-PLA N T GRINDING CIRCUIT FLOWSHEET FOR TREATMENT O F ITALIAN RUN-OF-MINE TALC l A T T K L L ' E * M E M O ft V A L I N -S Y I f U T * BUSINESS CONFIDENTIAL Protected Documnt-Subjectte ProteeKv* Order JHJAZ55_OOOOOOSI BUSINESS CONFIDENTIAL 5 TABLE 1. TYPICAL SIZE-DISTRIBUTION DATA, CRUSHING AND GRINDING C IR C U IT ^ Pilot-P lant Treatm ent of Italian Run-of-Mine Talc Mash + 3 - 3+ 10 - 10+ 20 - 20+ 35 - 35+ 6? - 65+100 -100+200 -200 Sis a D istribution, p a r cant by weisrht H am m erm ill B all-M ill No. 1 Cyclone Faadfc) Product^) ' D ischarge U'flow 0'fl.ow 41.8 m _ 22. 7 12.0 11.7 15.3 5.8 17.3 6.6 16.8 2.9 6.5 3.2 6.1 5.3 26.0 tr 0 .4 1.7 8.3 14.5 14. 2 60.9 e m -- tr -- 0 .4 -- 2.5 -- 10.9 5.0 16.3 3.2 14.5 2.2 55.4 89.6 No. 2 Cyclone U'flow 0 > fW d) -- tr tr 0.5 3.2 10.4 85.9 me m* -- -- tr tr 2.0 98.0 - 10 m icrons 0. 3 .1.0 6.8 (a) Run of October SS, 1866. (b) All pitting 2 inch. (0 Bill-mill feed. (d) Peed to prlmtiy cyclone* preceding fioutlon. -- -- -- 29.6 TABLE 2. TYPICAL ORINDING-CIRCUIT OPERATING DATA P ilot-Plant Treatm ent of Italian Run-of-Mine Talc Circuit Pebble Mill . New Feed (dry) D isch arg e No. 1 Cycloae Feed Overflow Underflow No, 2 Cyclone Feed Overflow Underflow Solide, lb/m in 7.5 57 17 40 17 7.5 9.5 Weights, Volumes, and Pulp Densities Slurry New W ater, SoUds, % QPM gpm 1 51 9, t . ; . ..T 22 27 18 9 21 -- 53 6 -- 8 25 4 . 4 23 -- 42 2 ATTILLI MEMORIAL INSTITUTE BUSINESS CONFIDENTIAL Protected Document-Subject to Protective Order JNJAZSSJMOMOSU BUSINESS CONFIDENTIAL 6 TABLE 3. TYPICAL GRINDING-CIRCUIT OPERATING DATA Pilot-Plant Treatment of Italian Ruh-of-Mine T ile Grinding-Circuit Circulating Load Per. cent circulating load Weight cyclone underflow `` Weight new feed New feed * 7 ,! lb/m ih Underflow, No. 1 cy clo n es 40 lb /m in Underflow, No. 2 cyclone 9. 5 lb /m in P e r cent circulating load = ^ x 100 660% i 7.5 Grinding-Circuit Classification Efficiency {At 200 Meeh) Recovery of Minus 200-Mesh Fraction Efficiency nt - Weight of m inus 200-m esh No. i cyclone overflow .. 10fl ' Weight df m inus 200-m esh No. 1 cyclone feed Efficiency, % g 0; | y * % * 100 * a l- 2* R ejection of P lu s 2Q0-Mesh F ractio n >E f f i c i e n c y , % (Weight of plus 200-m esh No. 1 cyclone feed) - (Weight of plus 200 -xnestrNo. cyclone overflow) Weight of plus 200-m esh No. 1 cyclofie feed aclOO Efficiency, %= ` T f j r 8 * 0Z) x .100 * 99. 3% ' . 3 i X 0 e 3/1 Cyclone Operating Data No. 1 Cyclone (e) No. 2 Cydone(b) ___________________ P r e s s u r e , paig Qpm Feed Feed Overflow 27 22 2 ` 25 16 6 () 4-ineh hott cyclone - B /lf-lncb inlet 1-ineh vettea findet 3/4-ineh tpex. (ti 4-ineh long eyelone - i/4-tn eh islet 3/4-tneli vtactex findet 8/8-lneh apex. Underflow `. ( c ) (c) (c) free difchuge. l A T T I L t 'l fcj C M O R I Ar C - I N S T I T U T S BUSINESS CONFIDENTIAL Protected Document-Subject to Protective Order JNJAZS6.SOOOOWW7 BUSINESS CONFIDENTIAL 7 BBNEFICIATION B eneficiation of the w e t - ground ROM talc was s ta rte d on O ctober 19, 1959. The f ir s t c irc u it u sed was that employed in the concentration of Italian No. 2 talc. * M icroscopic examination of the froth from each cell.showed that the talc being floated in all of the first 6 flotation cells was of good quality and that recirculation of the concentrate from Cells 5 and 6 (as p rac tic e d on Italian No. 2) was not n e c essa ry . Consequently, circu it changes were made which elim inated Float 2, the scavenger cyclones, and the scavenger flotation cells. Thus all 6 cells of the previous Float 1 and F lo at 2 c irc u its becam e F loat 1. After, s e v e ra l hours of operation with this stra ig h t rougher (Float 1) c irc u it on October 21, it was apparent hat insufficient quantities of flotation reagents were being used. (This was because there was now no circulating load to retu rn reagents to the flotation c irc u it.) Additional amounts of reagents w ere added for the balance of the shift. The low weight reco v ery , 49 p e r cent, obtained on this day is believed to be the result of several hours of operation with insufficient reagents. This circ u it, as shown in Figure 2, was Operated on October 22, November 3, and N ovem ber 4 with no changes. On Novem ber 5 and 6 reagents w ere in c re a se d 10 p e r cent. The m etallurgical results obtained during these 6 days of operation a re given in T able 4. R ecoveries of 60 to 65 p e r cent, based on plant feed, w ere obtained in p ro ducing a superior talc product. Typical operating data a re given in f ig u r e 2 and Tables 5 , 6, and 7. These in clude sise an aly ses, weights, volum es, pulp densities, cyclone operating data,- p rim ary cyclone efficiency calculations, and flotation reagent quantities. OPERATIONAL PROBLEMS The usual start-up and break-in problem s wefe' encountered in'the grinding c ir cuit, but once these had been solved, the entire circuit ran smoothly. Minor problem s that occurred, and should be kept in mind in designing a com m ercial plant, have been discussed in the Phase Report of December 30, 1959, "Design and Construction of a Talc Flotation P ilot Plant". * There Repeu, "Pilot-Flint BeaeficUtlon of Iu liia Mo. 8 Talc", Much 1, i860. A TTILLI M EM O RIA L IN ST ITU T S BUSINESS CONFIDENTIAL Protected Document-Subjectto Protective Order JN JA Z6SJM M M SSB BUSINESS CONFIDENTIAL 8 FIGURE 2. PILOT-PLANT FLOTATION-CIRCUIT FLOWSHEET FOR TREATMENT O F ITALIAN RUN-OF-MINE TALC ATTEllC MEMOItlAU INSTITUTE BUSINESS CONFIDENTIAL Protected Document-Subjectto Protective Order JNJAZMLOOOOOOH BUSINESS CONFIDENTIAL. 9 TABLE 4. SUMMARY O F PILOT-PLANT BENEFICIATION OF ITALIAN RUN-OF-MINE TALC D ate, 1959 Feed Rate, lb /h r Operating Tim e, min Oct. 21 435 359 Oct. 22 432 380 Feed(a > Platy Talc, C 0 2, % -10 M icron, % 91-92 0.61 29.5 91-92 0.64 29.6 Benefielated Talc Platy Talc, % COg, % -10 M icron, % O ver-A ll Weight Recovery, L u ster 99 0.15 9-0 48.8 . nd 99 0.17 10.4 58.0 nd Combined Tailinge(c) co2> % -10 M icron, % .1.05 61.9 1.29 59.0 (a) Orincling-circuit cyclone overflow. (b) Baled mi COa antlyiM. (c) Primary cyclose combined with flotation tailing. Nov. 3 467 366 91-92 0.68 27.0 99 0. 26 13.0 61.8 1.59 1. 36 ad Nov. 4 440 390 91-92 0.61 25. 2 99 0. 19 13.6 61.1 1. 56 1.27 nd Nov. 5 442 390 Nov. 468 330 91-92 0.68 28.9 91-92 0.61 26. 2 99 0.32 13.0 61. 3 l - 54 99 0.28 12.4 *'i 65.9 .. 1.59 1. 25 1.25 nd nd ATTELLE MEMORIAL INSTITUTE BUSINESS CONFIDENTIAL Protected Document-Subject to Protective Order J N1IAZSSJMOOOO8SO BUSINESS CONFIDENTIAL io TABLE 5. TYPICAL SIZE-DISTRIBUTipi P T A , FLOTATION CIRCUIT^) . . Mesh + 65 P ilot-P lant Treatm ent of Italian Rua-of-Mlne Talc P rim ary Cyclone U'flowO*) O 'ew 1.0 -- Flotation Tallin* -- Combined T a llin n (e) es . . -----' i f 1 Prye r . Product 0. 2 - 65+100 1.6 -- -- -- 1.3 -100+200 -200 0.6 -- -- 96.8 ea 97.9 -- 98. 7 1.0 97. 5 - 10 m icrons 9-4 7. 2 (a) Run of October 23, 1969. (b) Flotation lend. (e) n en n en tailing combined with primaiy cyclone overflow. 15.4 59. 0 10. 4 BATTE LC* M E M O R IA L I N<S T- 1 T U T E - BUSINESS CONFIDENTIAL - Protected Document-Subject to Protective Order JNJAZMJDOMOOM1 BUSINESS CONFIDENTIAL 11 TABLE 6. TYPICAL PRIMARY-CYCLONE AND FLOTATION-CIRCUIT OPERATING DATA P ilot-Plant Treatm ent of Italian Run-of-Mine Talc C ircu it P rim a ry Cyclones Feed Overflow U nderflow ^) Flotation Feed F ro th (b) Tailing Solids, lb/m in Weights, Volumes, and Pulp Densities Slurry New W ater, Solids, ft ' GPM gpm 7.5 4 23 -- 2.25 1.4 20 -- 5. 25 7 9 6 . 5.25 7 9 -- 4.5 15 3 2 . 0.75 1 .3 ' 8 -- F iltra tio n Feed F iltra te Cake 4.5 15 0 0 4.5 60 3 JC) . 3.6 -- 0 .4 -- By-Product Thickener Feed 3.0 1.3 28 -- Overflow 0. IB -- 27 -- Underflow 2.82 26 1 -- P rim ary Cyclone Classification Efficiency (At 10 m icrons) Rejection' of Minus 10 -M icron F ra ctio n Efficiency, ft a W eiaht o f m inus 10 m icro n s in cyclone overflow Jt 100 WWght of m inus 10 m icrons in cyclone feed Efficiency, ft = 3. 25 x 0. 712 ,, IAV eest t*afVt. 7. 5 x . 2 9 6 ----- Cyclone O peratisi Data - P rim a ry Cyclones ggM 23 reed 32 P r e s s u r e , g e il_______ Overflow 10.5 Underflow 6.5 (a) A tei dilution wtter. (fe) Altar launder iptay watet, (e) With water on Alter. ATTILLI MIMONIAL INITITUTt BUSINESS CONFIDENTIAL Protected Document-Subject to Protective Order JN<tA2SS_800000n2 BUSINESS CONFIDENTIAL 12 . . t TABLE 7. TYPICAL FLOTATION-REAGENT DATA Pilot-Plant Treatm ent of Italian Rua-of-Mine Talc . Reagent HClj 37 %W Dowfroth 250fa) Aerosol isfa) . Flotation R e a se n ti nound o e r . flotation Cells 1 2 3 1 Conditioner 5 o(*) 41. 0.06 4 0. 24 -- -- 0.06 0.06 0.03 --0 .2 4 -- 0.12 -- ton new feed r B y -P ro d u ct' Thickener -- -- Total *1.0 0.21 0. 60 Separan AP30fa) 0.10 0.10 (> 10 % solution. (b) 0 .4 "jbelution. (c) 2 4 solution. (d) 0 .2 4 tolutlon. (e> To pH 8.9-7.1. 8 . AT T E L L E MEMORIAL' INSTITUTE- BUSINESS CONFIDENTIAL- Piotcettd Document-Subject to Protective Order JNJAZ65_0Q0000593