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CW0-T-8T-56 0007-SWP-043714 0007-SWP-000127064 'Ci IV - _ j V. u Mineral Products Laboratory Dp t Cotober 25, 1?55 Jw - LITHCPOra, Q-ICTM- F^SARCH SPECIAL REPORT G3EOn:3 OF LITHOP5SE IN A HOCHBEPO MILL Summary - Pre liminary teats have demonstrated that "quenoh box" lithopone \discharge from oaloiner oan bo ground in netor slurry by Hoohberg Mill, bimitod tects did not in ii oats that this technique will produoe s lithopone or superior texture, horavsr, there do appear tube advantages in cost and else of equipment. Considerably more work seeds to be done to establish optlnum proosBslng conditions sad proper evaluation of product with respeot to color degradation, texture, opacity, eto. tsscrlptlon of Hills The mill ur.ee in the. work tinder disoussion waa a laboratory unit dosignac by the Dispersion Laboratory after the principles of the Hoohberg patent U.S. 2,59l,UlU. The work likewise was done with the assistance and co-oprution of the staff of the Dispersion Laboratory. The grinding ohaaber of the Bill consists of a vertical cylinder, n inches in diameter and 15 ir.ohes deep. The latest ? inches of the cyl inder wall consists of c removable 1*0 mesh sorsenj the bottom is solid. Projecting down through bhe oenter of the oylinder and extending nearly to the bottom is a motor-driven shaft carrying five evenly spaoed disks or rotors. These raters are 3 inches in diameter, l/*2 inch thick, and 2 inohea apart. The first rotor extends to within one inch of the bottem of tho chamber and the last to within 3 l/2 inches of the top. In operation, the mill la loaded about l/\ capacity with Ottawa sad, minus 20 plus 3 wash. The rotors are driven at 3U50 'AH*, or 2?dC ft./min, peripheral speed, and the grinding Is accomplished by the motion of the sand grains. EJngroixid slurry is fad in continuously at thj top of the mill uad discharged out through the screen at the insw the chamber. Tho grinding chamber Is so mounted that the lower third is oonta-ijisd in a closed re solving ohamber. The receiving chamber is fitted with a sloping bottom for good drainage and la discharged through a pipe and gate valve. Inasmuch as the aoreen area is fixed in this mill, the retention time in the mill, and henoe the amount of grinding, is controlled by regulating the die charge rate through the valve. The following site and oapaoity figures for the mill (2 inoh free-*) card) are pertinent1 n 0007-SWP-043715 0007-SWP Total Volun Sorting Vo lisas (rotors inserted) Apparent Volume of Sand Charge Solid Volume of Sand Vo Ions of Slurry Experimental Work: The particular ln-procea# naterial with whioh this work la concerned la " quanCh-bom" lithopoue, or oaloinar diaohurge produot. The sample submitted, ADEL 3613, was takes from regular produotion. This naterial la relatively coarse; such of the aggregate being in exoess of 2*0 ns ah. All of the grinding trials were run at a 30% solids concentration. As a basis for comparison, a portion of the staple was ground in a labora tory pebble Bill. gapaoity of Mill Voluae Pebbles (apparent) Vo Iv s h Slurry Total Voluna 1.00 gal, 0.50 0.29 0.60 Weight Slurry Weight Uthopone (dry) lh32 U29 The progress of the milling was folleeed by selecting nail oplea at perlodio Intervals and eheokiag for grind and rssldas. Time 1/2 hr. Sanaa Grind* 2 lA 0 325 Mesh Residua 6.1* 1 3 1/fl 0.80 2 1 1/2 3 3 U U 1/2 U 5 S 3A 6 1/8 6 1/2 0.17 0,03 less Than 0.01 less Than 0.01 teas than 0.01 '"Run directly on will slurry. 2 lA indicates dirt to 0 grind. 0 -2 0007"SWP--043716 0007-SWP At the completion or the run, the lurry was do-not#rod tad drlod at 110C. for further evaluation. Ia operating tho Hoohbsrg Mill, the discharge valve oa the reoeiver woo oloaod and sufficient water oddod to tho milling ohsmber to bring tho lat o 1 just above the charge of sand. The rotors were then started, feeding begun, and the discharge valve opened juet sufficiently to maintain the working level in the mill. For several reasons, it was desirable to uae a feed of 30% aolids concentration on all runs. Several preliminary triala were made which, while indicative, ware not too satisfactory because of the non-uniformity of the feed rate and solids oonoeatretion. This problem (which would not be encountered in pleat operation) was due to the rapidity with which the very coarse solids settled out of suspension, together with the pfcyeioal arrangement for foeding the mill. With the exoeption of the lest run, one galloa (U900 grama) of 30% slurry was used ia all the trials. The method of feeding the 111 was to add the wet 11thopone "sends" sad water separately ia small 1noremeats and in the proper proportions, as nearly as could be estimated. Sines the mill was loaded with water at the start of the run, the first discharge waa nsoessarily very dilute; hence about half of the feed was run through before retaining a sample of the product. After certain testa on the wot slurry, a portion waa de watered and dried at 11QC. for special texture teats. Ru b Wo . Ii The llthopone solids were reduced to 60 concentration to obtain a "pourable" sluny, vfaioh was then fad to the mill with additional water as required. There waa no discharge of llthopone from the mill and after a abort period of time, the feed had to bn discontinued bscause the level in the milling chamber did mot reaede. The rotors were continued until it waa obvious that the discharge soreen was bloated end would not be relieved by additional grinding. Run No. 2 * In this run, 0.2% tetresodli pyrophosphate (llthopone basis) was added as a dispersing agent. The llthopone solids ware added as a wet sludge containing 30? moisture, and the additional water carrying the dispersing agent added separately as before. This time there did not appear to be any hold-up In the llthopone discharge, although the solids concentration of the retained sample was only 23% llthopone. It was noted that there was considerable discoloration, lmdloattlng abrasion, during the early part of the rue. Bun Bo. 31 Another attempt was made to run without a dispersing agent. It waa felt that In the first r the eolids concentration was too high in the milling chamber, thus blocking the soreen. 3- - 0007-SWP-043717 0007-SWP-i * Uora care was taken to add sufficient water with the feed. There waa a good discharge of lithopone during moat of the run, but the mill appeared to block up Just at its completion. Discharge oeased and water could not be flushed through until a heavy charge of dispersing agent waa added. The faot that a dispersing agent relieved the blook strongly indloates that thsre la a tendency for the lithopone solids to bridge aoross the aoreen as a "cake" under oertaln conditions. Run No. Us This run waa basioally a repetition of the aeoond run, using pyrophosphate to produce a dispersed system. An attempt waa made to increase the feed rate with only indifferent suooeas beoause of the nature of the feed. While there was a oantinuous disaherge of slurry, the yield of lithopone appeared to be low. Flushing out of the mill further Indioatad that a considerable build-np had ooourrsd. Run Wo. 5* The behavior of the first four runs indloated a marked tendency for lithopone to build up in the mill and gradually block the discharge aoreen. However, it was felt that this may have been due to poor feed techniques, which resulted In variable and, at tinea, axoesalve solids content end low through-put rates. In order to oorreot the situation, a quantity of the quenoh-bax materiel waa given a very light pebble milling; 1$ minutes at 3solids. This slurry, than raduoad to 30% solids, was still relatively ooarae with a grind of 0, but could be readily kept In suspension by oooaslonal stirring. In this run, no dispersing agent waa used and -the nature of the feed enabled a uniform charge to the mill at about twioe the rate used In the previous trials. Imnsdlately following the slurry oharge, flushing water was rim tbrout the mill to wash out the bulk of the lithopone retained in the milling and raoalTing chambers. Aooardingly, the effluent was oolleotad as three separate portions; the dilute pre run effluent, the product effluent, and the wash effluent, as outlined below. Feed! Lithopone Slurry (Lithopone, dry Flushing Water Tima to Charge Slurry: 6390 gas. (1.3 gala.) 1900 gms.) 260 gas. (0.75 gals.) 9 nln. Rate 8.7 gal./hr. Dieoharge: 1. Prorun Kffluaat Solids oono. Lithopone yield Grind Ut55 gms. (0.35 gal.) lit. 0% 210 gms. 7 H. -u- 0007--SWP-043718 0007-SWP' .2 Product Effluent Solids oono. Lithopon# yield Grind 3. Wash Effluent Solids oono. Lithopone yield Grind 5055 p*a< 25.0 % 1265 gms, 6 Vk H. k (1.06 gel.) 32 l)i gms. 8.6 % 276 gms. 7H There did not appear to be any inclination for the aill to oholoo op in this run. While there waa a shortage of 150 gms. of Uthopone in the combined effluent*, this oan be at leant partially aooouated for by the tendency of the Uthopone to aettle out in the receiving ohember of the mill. After evaluation of the aeparate fraction* of effluent, they mere oombined and a portion of the composite de-watered and dried, later examina tion (aee reeulta below) indicated that a olaaeifloatlon far removal of overalae waa naoeasary. Consequently, a e*xg)le of the oonpoaite a lurry waa dlaperaed with 0.251 tetraaodium pyrophosphate and elutriated througi a single ohamber of aa inverted oone-type toil elutrlator. The olaaslfied slurry waa then floooulated with a small amount of alia, de"watered, and dried at 110C. Run Permolith UQM, Standard Quench Boor, Unprocessed Effluent Slurry Grind Realdue ---- 22 u 0 Pry Plcant Hoover Muller Texture 100 UOu Rev, 5 1 iA 0 5 1/2 h V'2 3 Ball Milled, 6 l/2 hours 6 1/2 l.t. 0.01 6 6 lA 6 lA Run VI No Produot Run #2, (diap.agent) Run #3 6 3A U 0 0.05? 1.05 u iA 3 1/2 2 lA 1 U 1/2 3 1/2 2 3A 5 1/8 5 iA Run ifh., (disp.agent) jA 0.099 0 3^ k 1/2 3 lA 5 iA Run *5, oonpoaite 6 VU U 0.20 n/i 2 3 3A 6 5 lA Run V5* classified 7* l.t. 0.01 6 6 lA MW -5- 0007-SWP--043719 All tuples from the rune la ths Hochberg mill showed a definite gray dlsoolaration, indloatlog abrasion in tbs ad 11. The product of Run #$ showed ths least dlsooloration. An analysis of this product showed that It had ploted up 0,,08f Fe; almost certainly from abrasion of the still by ths sand. Dlsouaslon and Conclusions- Thar* appears to b# no question that the Boohberg Mill Is capable of grinding quenoh-box llthopone to satlsfaotoiy fineness. It is also apparent that such a prooass would require a olaaatfloatlon system In oonjunction with It, just as la used with a ball-milling oircuit. It has not been definitely established whether the Boohberg unit eill produce a llthopone of lag!roved texture end dispersion oharaoterletics. The products from all the runs exhibited considerable odor de gradation beoauae of sill abrasion. The stiff of the Dispersion laboratory feels that this abrasion oould probably be oorreoted by replacing the present olid steel rotors with a hard alley. On the other hand, it aust be reoognized that the Boohberg mill has been primarily Intended for dispersion of pigments in oil media. This sssentially provides a lubricant that minimicss ths abrasive aotion of the send, whereas watsr slurries have little lubrloating effect. Banos, non-metal* suoh as osramios, glass coatings, rubber, or plastlos might provide a better solution to this problem, The important advantages of the Boohberg mill appear to be the saall site of equipment required and the low power ooneumption. If we use Run Bo. 5 as a basis end assume a direct else faotor, a 35 ton per day llthopone unit would require a will having the following apprcoclasts dlsmnslona2 fright 6 lA ft. Dieneter I 1/2 ft. Capacity II l/2 ou.ft. (65 gals.) Sand Charge 725 lbs. Rotor Speed 700 RPK. (2700 ft./min.) This, of oourse, refers only to the grinding chamber and does not include the reoelver and auxiliary equipment. The conclusions drawn here ere only tentative. Additional work must be done to establish optimum conditions and longer runs should be made to obtain definite evaluations, both as to the app Host ion of the Boohberg process to the grinding of quenoh-box llthopone end to the quality of the pigment produced. F. C. Varduln, H. E. Dingle :hb 00 < Technical frillng Hat Auxilisries Mailing list C. B. Adams, Ulnars.1 Products laboratory -6- 0007-SWP-043720