MinBaS-dagen 2007
Transcription
MinBaS-dagen 2007
MinBaS II Mineral•Ballast• Sten Område 2 Rapport nr 2.2.5:1 MinBaS II område nr 2 Produktutveckling Delområde nr 2 Utveckling av industrimineralbaserade produkter Projekt/Delprojektnamn nr 2.2.5. Coating och malning av industrimineral med Hicom-teknik Slutrapport Malning och coating med Hicom-teknik Eric Forssberg, MISEC AB Stockholm i april 2011 Sammanfattning Vid besök hos Hicom- hos Ludovici Australia Pty, Pinkenba, QLD, Australien i oktober 2009 diskuterades torrmalning och coating av industrimineral. Ett projekt med två försöksmaterial genomfördes. Som försöksmaterial användes kalksten med deltagande av Nordkalk AB och Omya AB. Försöken genomfördes hos Ludovici i deras försöksanläggning med en Hicom 25 kW utrustad med vindsikt Comex ACX 200. Försök gjordes med tillsats av stearat som coating kemikalie. Försöken gjordes andra halvåret 2010. Materialprover har tillställts de deltagande företagen för analysering och utvärdering som ännu ej är färdig och som kommer att redovisas senare. För malning och coating ner till 3 à 4 micron fås i en Hicom om 110 kW en kapacitet av något ton per timme. Summary Coating and grinding of industrial minerals was discussed with Hicom at Ludovici Australia Pty, Pinkenba, QLD, Australia in October 2010. In this project limestone from Nordkalk AB and Omya AB was used for tests with coating and grinding during the second half of 2010. Samples have been sent to the participating companies for evaluation. The results from the evaluation are not yet available and they will be reported later outside the MinBaS framework. A capacity of about one ton per hour is obtained in coating and grinding to 3 à 4 micron in a Hicom of 110 kW. Innehållsförteckning - MinBaS proj 2 2 5 Sammanfattning Summary Rapport Bilaga 1. Besök Hicom den 6.10.09 Bilaga 2. Projektförslag. Coating och malning av industrimineral med Hicomteknik, 16.11.09 Bilaga 3. Hicom pilot plant description. 23.05.10 Bilaga 4. Confidential report H-2010. MIS.01. Hicom pilot plant dry grinding trials on Calcium Carbonate for Misec. Nordkalk PArfill 7 results. 16 September 2010 Bilaga 5. . Confidential report H-2010. MIS.02. Hicom pilot plant dry grinding trials on Calcium carbonate for Misec AB. Omyacarb 10 results. 25 January 2011. MinBaS Projekt 2.2.5. Coating och malning av industrimineral med Hicom-teknik. 1. Inledning. Hicom-tekniken har utvecklats under lång tid. Från början var fokus på våtmalning oh ett omfattande utvecklingsarbete genomfördes i Australien. Bland kända tillämpningar kan nämnas frimalning av diamanter vid off-shore utvinning. Jag fick första gången kännedom om Hicom tekniken år 1985 och besökte senare MD Research utanför Sydney, NSW. I oktober 2009 besökte jag Ludowici Australia, Pty i Pinkenbaa utanför Brisbane, QLD. Reserapporten finns som bilaga #1. Teknologin hade flyttats och inriktningen var nu på torrmalning och en kombination med coating för ytbehandling av fyllmedel för termoplast. På grundval av erfarenheterna från besöket och efter kontakter med företagen utarbetades ett projektförslag för MinBaS område 2. Detta projektförslag, bilaga # 2 godkändes av styrgruppen och ett slutligt avtal tecknades den 11.2.10. Två av MinBaS medlemsföretag visade intresse för att deltaga i försöken hos Ludowci i Brisbane. Detta var Nordkalk och Omya. Försöksmaterial, Parfill 7 skickades från Nordkalk till Brisbane. För Omya anskaffades försöksmaterial, Omyacarb 10 lokalt i Australien. Efter undertecknande av sekretessförbindelser beslöts att försöken skulle genomföras under vecka 31 , 2-6 augusti 2010. Per korrespondens hade erforderlig tid för försöken diskuterats och en vecka bedömdes som tillräckligt för två material. Malningsförsök skulle genomföras med och utan coating. Försöksanläggningen för Hicom hos Ludowici är påkostad och beskrivs i bilaga # 3. I princip består anläggningen av en Hicom kvarn storlek 25 kW och en vindsikt typ COMEX ACX 200. I övrigt finns utrustning för pneumatisk transport, dammavskiljning, provtagning och en Insitec partikelstorleksanalysator. För matning av stearinsyra finns utrustning för smältning och pumpning. Styrsystem och datainsamlingssystem kompletterar utrustningen. 2. Försökens genomförande och resultat. Det stod klart på ett tidigt stadium att försöken inte skulle kunna genomföras under vecka 31 2010. Praktiskta problem uppträdde med materialhantering och matning av stearinsyra. Den ledning som skulle föra smält stearinsyra till kvarnen var inte tillräckligt isolerad varvid materialet stelnade och blockerade ledningen. Ett litet antal försök med Parfill 7 hanns med under vecka 31 och resten av försöken genomfördes under hösten 2010. Jag fick tillfälle att besöka Brisbane ytterligare en gång under perioden 6-10 september 2010 för deltagande i XXV International Mineral Processing Congress, IMPC. Jag besökte då Ludowici en gång för att diskutera försöken inom MinBaS med Dr Steve Marshall och ytterligare en gång tillsammans med Dr Andreas Fredriksson från LKAB , på den tiden representerande Minelco. Andreas Fredriksson hade tidigare visat intresse för att deltaga i MinBaS försök men av olika anledningar hade detta ej blivit av. En rapport över försöken med Parfill 7 erhölls i slutet av september 2010, bilaga # 4. En rapport över försöken med Omyacarb 10, bilaga # 5 erhölls i slutet av januari 2011. Försöksresultaten har kommenterats i bilagorna # 4 och 5. Försöksresultaten visar att det är svårt att mala utan malhjälpmedel och att det är möjligt att komma ner till till 97 % mindre än 3 à 4 micron. För en fullstor anläggning skulle kapaciteten för en Hicomkvarn om 110 kW bli något ton per timme. Det rekommenderas att två Hicom kvarnar kombineras med en vindsikt. 3. Fortsatt arbete. Ett stort antal prover från malning med såväl Omyacarb 10 som Parfill 7 har skickats till Omya respektive Nordkalk för utvärdering som fyllmedel för termoplast. Några resultat från dessa utvärderingar föreligger ej ännu. En separat rapport kommer att presenteras senare. MinBas har betalat Ludowici cirka 45 000 kronor för försöken. Ludowicis egeninsats uppgår till cirka 390 000 kronor. Åkersberga den 7.2.11. Eric Forssberg Misec AB Bilaga 1 Besök Hicom den 6.10.09, Ludowici Australia Pty, Ltd.,Pinkenba, QLd (Brisbane) Kontakt:,Dr Steve Marshall, manager Hicom technologies, Hicom är sedan kort tid en del av Ludowici. Ludowici tillverkar diverse utrustning för mineralberedning som vibrationssiktar och avvattningscentrifuger. Andra intressanta områden är slitbeläggningar av kalcinerad bauxit med resin och keramiska plattor som klistras. För slitbeläggningar i rörledningar rullas slitmaterial och resin inne i röret. Ludowici gör också polyuretan detaljer för t ex siktar. I Brisbane sker montering och målning. Maskinbearbetning sker huvudsakligen genom lego eller t ex i Indien. Försöksanläggningen för Hicom har flyttats från Sydney till Brisbane i slutet av 2008. Steve Marshall var den enda som kom med. Han anser att man nu har en mer kommersiell verksamhet jämfört med då R&D finansierades av Charles Warman. Det ultimata syftet för Charles Warman var att skapa en utrutning med hög energitäthet som kunde användas under jord för frontnära malning. Tidigare låg fokus på våtmalning t ex för diamanter i marine deposits. Där gällde det att mala ner snäckskal som spred röntgenstrålning på ungefär samma sätt som diamanter och följaktligen förhindrade XRF sorting. En annan fördel med Hicom var att den genom de små dimensionerna kunde placeras ombord på fartyg. Nu är fokus på torrmalning av Industrial minerals. En typisk anläggning består av 2 stycken Hicom om 110 kW, vilket är maxstorleken och en vindsikt. Vindsiktarna kan vara dels Comex , dels Hosokawa. Pilotanläggningen i Brisbane är uppställd med en Comex vindsikt. Man vill leverera hela anläggningar med Hicom, transportutrustning steel work, styrsystem och vindsikt. Pilotanläggningen har för övrigt en Insitec partikelanalysator on line. Tidigare användes rubber lining i Hicom men denna höll inte länge i våtmalning förmodligen på grund av de höga krafterna och den höga temperaturen. Kylning av varmt gods på grund av den höga energiintensiteten är fortfarande ett problem. Steve Marshall visade hur man genom att ta upp ett hål i manteln kunde kyla effektivt. En annan möjlighet att kyla materialet är att tillföra vatten men det är ej så praktiskt. Typiska temperaturer kan vara 90 grader C. Nu användes steel lining bestående av white iron, (gjutjärn) och det går bra även för abrasiva material som SiC. En steel lining kan räcka ett år jämfört med gummi kanske en månad. Steve Marshall anser att man nu kommit över olika mekaniska problem som tidigare förekom. För att abrasion inte skall vara något problem krävs att ingående inte är för grovt. Ett ingående om cirka 50 mikron går bra. Vore det 1 mm skulle det blir slitageproblem. En målsättning enligt Steve Marshall nu är att marknadsföra Hicom som ett system för malning och coating av fyllmedel för plast. Med två Hicom och en klasserare torde man kunna producera 2* 750 kg coatad filler, t ex CaCO3 per timme för termoplast. Energiförbrukningen blir lägre än för den nu använda tekniken med våtmalning, torkning och coating. Investeringskostnaden för en sådan anläggning blir ungefär MAUD 2 komplett. En Hicom svarar för AUD 650 000. Däremot måste sägas att Hicom bara för malning inte är särskilt energieffektiv . Coating med steric acid. Denna finns i en behållare som värms så att stearinsyran smälter och sedan användes en pump för att spraya kemikalien. Ungefär 10 Hicom anläggningar är i drift. Exempel på material är: Zirkon Kiselkarbid Talk CaCO3 Silika Mica Baryt Fly ash Kaolin Diamantmalm För t ex Zirkon är det möjligt att uppnå D97 2,4 mikron och för CaCO3 D97 = 3.5 mikron. För torrmalning utan coatingsyfte måste oftast grinding aids i form av tex EDTA tillsättas, kemikalier väljs efter vilket mineral som skall malas. Det finns sedan rätt länge en Hicom hos Sintef i Trondheim. För ett MinBas projekt är det mer ändamålsenligt att göra försöken i Brisbane. Som malmedia kan material ner till 1 mm användas. Normalt är dock 2,5 mm. Vanligen användes yttriumstabiliserad zirkoniumoxid eller stål. Aluminiumoxid blir för sprött och slås sönder snabbt vid den höga impacten. Media kostar storleksordningen USD 40 per kg. Detta kan verka högt men det går inte åt mer än 170 kg media för hela chargen i en 110 kW maskin. Styrning av malfinlek sker genom: Uppehållstid Öppen utmatningsyta Mediastorlek Fyller man Hicom med mer media blir det snarare fråga om skrubbning än om malning. Vad som verkligen sker inne i Hicom vet man inte så mycket om. Det finns DEM modeller och PBM . CSIRO har gjort CFD simuleringar som visar kulornas rörelser. Vid t ex malning av mica och kaolin fås förmodligen en viss delaminering men det är osäkert. För kaolin fås en bättre liberation och därmed ökat utbyte. Andra material som skulle kunna vara intressanta för ett MinBaS projekt vore magnetit. För försök med pilotanläggning får man räkna med 1 à 2 ton material och upp till fyra dagars arbete. Kostnaden är AUD 2000 per dag men då ingår även rapport. Steve Marshall skall skicka en hel del material på CD: Presentation Technical data Particle size distribution Movies Pictures Steve Marshall skall göra en round the world trip I februari/mars 2010 och besöker då gärna intresserade företag. File name ”Hicom6.10.09” Bilaga 2 HICOM Projektförslag 16.11.09 Coating och malning av industrimineral med Hicom-teknik. 1. Inledning Hicomtekniken utvecklades på 1980-talet. Målsättningen var att ta fram teknik för malning med hög energiintensitet. Hicom karakteriseras av att malningen sker i en behållare fylld med malkroppar och att denna är upphäng och utför en nuterande rörelse. www.hicom-mill.com . Utvecklingsarbetet bedrevs i stor skala i Sydney, NSWoch finansierades av Charles Warman. (Warman pumps). Ett litet antal Hicom-anläggningar såldes framför allt för våtmalning av marina diamantförande material. Hicom teknologin har 2008 övertagits av Ludowici Australia Pty. Ltd med anläggningar i Brisbane, Australien. En ny försöksanläggning har satts upp och focus har ändrats från våtmalning till torr malning och behandling. En mycket intressant applikation är coating och malning av industrimineral. Ytterligare information framgår av Eric Forssbergs rapport från besök den 6.10.09. Ett projekt föreslås omfattande coating och malning av ett à två utvalda industrimineral vid Hicoms anläggning i Brisbane. Proverna skickas tillbaka till de deltagande företagen för utvärdering och en sammanfattande rapport utarbetas. 2. Målsättning. Målsättningen med det föreslagna projektet är att utvärdera och bedöma Hicomteknikens potential för malning och coating av filler. 3. Projektets genomförande. Projektet genomföres av Eric Forssberg, Misec AB. Projektet omfattar följande moment: 1. Val av försöksmaterial i samråd med deltagande företag. 2. 500 à 1000 kg försöksmaterial, mindre än 50 micron skickas till Hicom i Brisbane 3. Försök med coating och malning vid Hicom i Brisbane. Partikelstorleksfördelning bestämmes med befintlig Insitec-utrustning. Försöksparamterar är uppehållstid, avskiljningsgräns för vindsikt, typ COMEX, mediastorlek, öppen utmatningsyta, koncentration av coatingkemikalie. Energiförbrukningen bestäms. 4. Prover tas ut och skickas för undersökning hos deltagande företag. 5. Sammanställning av försöksresultat och värdering av tekniken dels med avseende på malning, dels för coating och produktutveckling av filler. 4. Kostnader för projektets genomförande. Projektet beräknas kunna genomföras inom en kostnadsram av kronor 305000 Enligt nedanstående specifikation. 1. 2. 3. 4. 5. 6. Uttag av prover, analysering och frakt till Brisbane, naturainsats 50000 Kostnad för försök vid Hicom AUD 10000, kontant 60000 Rese- och uppehållskostnader, kontant 45000 Analysering av prover vid deltagande företag, naturainsats 50000 Arbetskostnad för Eric Forssberg, kontant 50000 Arbetskostnad för Eric Forssberg, naturainsats 50000 Summa projektkostnad 305000 Kontant Naturainsats 5. Tidplan Projektet beräknas kunna genomföras under tiden 1.1.10 – 30.9.10. Hicom projförslag 16.11.09 155000 150000 Bilaga 3 CONFIDENTIAL Hicom pilot plant Description Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 1 of 10 CONFIDENTIAL Contents Hicom 25 Dry Pilot Plant: Description and Operating Procedures .......................................................... 3 Typical Test Procedure .................................................................................................................... 4 Grinding circuit behavior and sampling .......................................................................................... 6 Data Analysis Procedures ........................................................................................................................ 8 Test conditions .................................................................................................................................... 8 Feed and product rate ......................................................................................................................... 8 Circulating load ratio estimation ....................................................................................................... 10 Author: Dr. Steve Marshall Report Date: 23rd May 2010 Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 2 of 10 CONFIDENTIAL Hicom 25 Dry Pilot Plant: Description and Operating Procedures Figure 1 Photograph showing the Hicom 25 dry pilot plant The Hicom 25 dry pilot plant is shown in the above picturAe (Figure 1) Figure 1and schematically in Figure 2 below. The plant consists of a Hicom 25 kW mill with variable speed drive, operating in closed circuit with a Comex ACX200 high efficiency air classifier. The entire plant is controlled and monitored using a Siemens S7-300 PLC and Siemens WinCC SCADA package operating on a touchpanel PC mounted in the main control cabinet. A 75 mm screw feeder is used to transport material to the mill from a feed bin. Solids feed rate to the mill is calculated from loss-in-weight measurement from a load cell on the feed hopper. The calculated rate can be used in closed loop with the screw feeder VSD to provide feed rate control. The Hicom 25 mill motor is controlled by a Siemens VSD in the main control cabinet. The mill is generally operated at discrete speeds of 760 and 960 RPM corresponding to maximum chamber acceleration of 30 and 50 G respectively. The mill drive lubrication system is monitored and controlled by the central Siemens PLC. The grinding system operates under vacuum in order to avoid dust emission. Material is drawn through the mill and pneumatically conveyed to the classifier. The air flow required for effective pneumatic transport through the mill is much less than that required for effective classification. Therefore, additional air is drawn into the system through the primary air valve indicated on Figure A1.1. The setting of this valve and the secondary air valve also control the differential pressure across the mill – that is the mill vacuum. Oversize particles, rejected by the classifier rotor, fall by gravity down the oversize chute for regrinding in the mill. The classifier is operated by a VSD which allows the rotor speed to be set to achieve a precise product top cut size. Compressed air is used to seal both the classifier rotor and the Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 3 of 10 CONFIDENTIAL rotor bearings. The classifier oversize return is sealed by a 150 mm double-butterfly valve air lock system as indicated on the diagram. The secondary air flow to the classifier is manually adjusted by a butterfly valve, and monitored by an orifice-plate flow meter. Air and fine product are pneumatically transported to a Torit-DCE DLM V20/12B Dalamatic dust collector where the product is collected in a drum or bulker bag. The dust collector is sealed by a 200 mm double-butterfly valve air lock system. An Insitec on-line particle size analyser is installed on the classifier fine-product line. This enables instant feedback on classifier performance and provides the means for meeting precise particle size specifications by automatic adjustment of classifier rotor speed. Two blowers operated in parallel are used to generate the system air flow. A Rietschle SAP1500 (System Blower 2) is run at full speed, and a GAST R93150A (System Blower 1) is operated by a VSD to provide trim control on system air flowrate in closed-loop feedback with an orifice-plate flow meter downstream of the dust collector. The total system air capability is roughly 1600 m3/hr at 20 kPa using both blowers. Instrumentation is incorporated for monitoring critical process and mill control parameters, most of which are recorded on the SCADA system. The mill power draw is determined from direct reading of the Mill VSD. A microwave mass-flow indicator installed on the classifier feed (mill discharge) line provides feedback as to whether the plant is at steady state. The grinding chamber nominal volume is 10.7 L and its 40 mm discharge ports are positioned at the circle of maximum diameter. Grates are placed over the discharge ports to retain the media inside the grinding chamber. The grate slot width is generally selected at least one-half the diameter of the smallest media particle used. Typical Test Procedure After every chamber change-out, or after an extended shutdown, the mill is operated for twenty minutes with an empty chamber to establish the no-load power. The required charge of media is added to the mill before commencing each test. The solids feed rate to the mill is selected, and the system and secondary air flows set to maintain appropriate classifier conditions. The classifier rotor speed is then adjusted to give the desired cut size based on Insitec particle size readings. Product and recycle samples are taken once relatively steady-state plant operation is obtained, as indicated by the mill discharge mass flow indicator. This is generally 20 to 25 minutes after starting a run. Critical mill control and process parameters are monitored during each run and recorded on a standard log sheet every time a sample is taken. The recirculating load rate is estimated after taking a physical sample of the mill discharge after a crash stop of the plant. The particle size distributions of the classifier feed, fine product and coarse reject streams can be used to back-calculate the recirculating load ratio. The rate of product discharge from the dust collector is calculated from gain-in-weight measurement of the product bulk bag, which is positioned on electronic weigh-scales. Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 4 of 10 CONFIDENTIAL F T F IC PI IN SITEC FI PI D UST C OL LEC TOR 2 0 0 NB M VSD IA 15 0 N B PI COM MEX ACX 200 CLASSIF IER FI FT PI PI M V S D JT JI SY ST E M BL OW E R 1 LOAD C ELL FI FT FEED H OPPER SE C ON DA R Y A IR V ALV E PI W VSD M 1 0 0 NB F IC F IN E PR OD U C T C OL LEC T I ON JT V S D 1 0 0 NB JI FI M TS TI PI PT H ICOM 25 MIL L PE BB LE T R AP Figure 2 Hicom Report PE-0816.P-1 (Revision 1) PR IM A RY A IR V ALV E Schematic diagram of the Hicom 25 dry pilot plant 23-May-2010 Page 5 of 10 CONFIDENTIAL This rate is compared with the feed rate to assess whether the circuit is at steady state. Generally, the feed and measured product rates must be within 20% of one another, otherwise the data is from the run is not considered for analysis. The exception to this rule is when the material is very fine or sticky and there is significant holdup of material in the dust collector. Under such conditions, accurate determination of product rate is not possible over a short time period, and we rely on microwave sensor readings of the circulating load to determine if the plant is at steady state. The mill net power draw for calculation of specific mill grinding energy is determined as the difference between the measured gross power and the no-load power. Grinding circuit behavior and sampling Typical circuit responses for dry pilot plant operation and the test protocol followed are best illustrated with reference to Figure 3 below, which shows a characteristic SCADA trend obtained during a pilot plant trial. Figure 3 Hicom 25 pilot plant SCADA Trend screen Between 5:54 pm and 6:10 pm, the mill power draw (red trace) was around 11 kW, the circulating load (black trace) was below 10% and the mill exit temperature (light blue trace) was around 72oC. Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 6 of 10 CONFIDENTIAL The feed rate (oscillating blue trace) was increased slightly at around 6:10 pm. This resulted in an increase in circulating load, a decrease in mill power and a decrease in mill temperature due to the increased rate of heat removal from the mill from the higher solids throughput. Despite the increased circulating load, the circuit is nevertheless stable as the circulating load is not increasing above 15-20% on average. This indicated level of circulating load was considered the maximum stable level for plant operation with ATH. Experience showed that further increases in feed rate resulted in accelerating increase in circulating load rate due to the fact that the rate of fresh feed to the mill started to exceed the rate of fine particle production. The objective in pilot plant trials was to adjust conditions such as discharge port open area, mill vacuum, media size and quantity and other factors to try and maximize the mill feed rate before an excessive circulating load rate was reached. In the example shown in Figure 3, at around 6:36 pm, the plant was stopped (crash stop) by stopping the mill, air blowers, the classifier and by shutting the classifier return air lock valves. This way, a ‘snap shot’ was taken of the circuit from which samples could be taken for analysis. We sampled the recycle stream, the residual powder on the internal walls of the mill body (equivalent to classifier feed) and also the fine product collected in the product filter. These samples were used to estimate recirculating load ratio, as outlined in Appendix B. For some runs, the mill contents were also removed and the powder and grinding media separated by screening. This way it was possible to determine the holdup level of powder in the mill and also to assess media wear. Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 7 of 10 CONFIDENTIAL Data Analysis Procedures Test conditions All of the data logged on the SCADA system is collated into an Excel spreadsheet. Where necessary, a simple first order filter can be applied to smooth the data for more accurate estimation of parameter values at the time of sample collection or crash stop. Feed and product rate For most test runs, estimation of feed and product rate is done by calculating the numerical derivative of the recorded change in weight of the feed hopper and the product weigh scales respectively. First-order filtering before and after numerical differentiation is used to reduce the affect of inherent ‘noise’ in the data. Generally, the feed rate data is considered more reliable as hold up of material in the product filter meant that the change of measured product weight with time is usually not a smooth progression. An algorithm was introduced into the PLC program to calculate the feed rate in real time. However, because of the long lag times necessary to achieve a smooth output, and a periodic variation in screw feeder output, use of this calculated rate to control the screw feeder can cause oscillation in the controlled feed rate. It is noted that these oscillations do not significantly affect process operation as they are usually dampened by the relatively high circulating load in the grinding and classification circuit. Typical rate calculation results are illustrated in Figure 4 below. Figure 5 shows the corresponding process parameters of mill air temperature (discharge temperature), mill power and circulating load corresponding to the same time period of the data in Figure 3 and Figure 4. In this example, it can be seen that a relatively small increase in average feed rate from around 58 kg/h to around 62 kg/h resulted in a significant increase in circuit load and it was concluded that further increase was not possible beyond around 62 kg/h for this particular mill and plant configuration. Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 8 of 10 CONFIDENTIAL Calculated Feed rate (filtered) Feed rate (PLC output) Feed Hopper Weight (raw) Feed Hopper Weight (filtered) 100 620.0 90 600.0 80 70 580.0 50 560.0 WT (kg) RATE (kg/h) 60 40 540.0 30 20 520.0 10 0 500.0 19/03/2010 16:00 19/03/2010 17:00 Figure 4 19/03/2010 18:00 Hicom 25 pilot plant feed rate estimation example Air Temp Mill Power Circulating Load 80.0 70.0 60.0 50.0 40.0 30.0 20.0 10.0 0.0 19/03/2010 16:00 Figure 5 19/03/2010 17:00 19/03/2010 18:00 Process parameters corresponding to the time periods shown in Figure 3 and Figure 4 Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 9 of 10 CONFIDENTIAL Circulating load ratio estimation The circulating load ratio, hence coarse recycle rate, can be estimated from the particle size distribution of samples of classifier feed, fine product and coarse reject. The Excel solver function is used to minimize the sum of squares of the difference between measured particles size distribution and the corresponding particle size distribution calculated using an assumed ratio and the other two distributions. Generally, the measured classifier feed is considered the least accurate of the collected samples and this is then taken as the basis for the estimation procedure. In the example shown in Figure 6 below, it can be seen the calculated and measured classifier feed distribution closely match, which gives a high level of confidence in the ratio of 6.6 calculated for this particular test run. Calculation of the ratio using the coarse return and the fine product was also done to verify accuracy of the primary estimate. In most cases, variation in calculated values was less than 10%. The coarse recycle rate was then obtained by multiplying the steady state feed rate by the estimated recirculating load ratio. For those trial runs where no crash-stop samples were collected, the ratio may be estimated from the recirculating load level indicated on the microwave sensor output. Such estimates are considered accurate only within 20%. Measured classif ier f eed Measured coarse reject Calculated Classif ier Feed Measured f ine product 100 90 80 % Undersize 70 60 50 40 30 20 10 0 0.1 1 10 100 Size (µm) Figure 6Results from estimation of recirculation load ratio (RLR) using sum of squares error (SSE) minimization on adjustment of the calculated classifier feed particle size distribution Hicom_Pilot_Plant_Description[2] 23-May-2010 Page 10 of 10 Bilaga 4 CONFIDENTIAL Confidential Report H-2010.MIS.01 Hicom pilot plant dry grinding trials on Calcium Carbonate for MISEC: Nordkalk Parfill 7 results H-2010.MIS.01 R0 16-September-2010 Page 1 of 28 CONFIDENTIAL Contents Executive Summary for MISEC ............................................................................................................ 4 1 Introduction ................................................................................................................................ 5 2 Objectives ................................................................................................................................... 5 3 Conclusions & Recommendations ............................................................................................... 5 4 Equipment and procedures ......................................................................................................... 7 4.1 Hicom 25 pilot plant ............................................................................................................ 7 4.1.1 5 Sample / run labelling .................................................................................................. 7 4.2 Particle Size Measurement ................................................................................................ 7 4.3 Data analysis ....................................................................................................................... 7 Test results & discussion ............................................................................................................. 8 5.1 Feed material particle size distribution ................................................................................ 8 5.2 Pilot plant results................................................................................................................. 8 5.2.1 Product size 3-4 µm (P97) - Table 2 ............................................................................ 12 5.2.2 Product size 5-6 µm (P97) - Table 3 ............................................................................ 14 5.2.3 Product size 8-9 µm (P97) - Table 4 ............................................................................ 15 5.2.4 Product size versus specific grinding energy ............................................................... 15 5.3 Scale-up and Hicom 110 production capacity ..................................................................... 17 5.4 Comments on production plant design .............................................................................. 17 Appendix A – Hicom 25 Dry Pilot Plant: Generic Description and Operating Procedures .................... 19 Generic Description of the plant.................................................................................................... 19 Stearic acid dosing system ............................................................................................................ 21 Typical test procedure................................................................................................................... 23 Grinding circuit behaviour and sampling ....................................................................................... 23 Appendix B – Data Analysis Procedures............................................................................................. 25 Test conditions.............................................................................................................................. 25 Feed and product rate................................................................................................................... 25 Circulating load ratio estimation ................................................................................................... 25 Figures Figure 1 Nordkalk Parfill 7 feed size distribution compared with customer standard ....................... 8 Figure 2 Example of changing product size with change in classifier solids loading......................... 13 H-2010.MIS.01 R0 16-September-2010 Page 2 of 28 CONFIDENTIAL Figure 3 Product size distributions from the finest uncoated (Run 2) and coated (Run 3) product samples .............................................................................................................. 13 Figure 4 Example of product size control by automatic regulation of classifier speed..................... 14 Figure 5 PSD for intermediate coated product (Run 6) ................................................................... 15 Figure 6 PSD for coarse coated product (Run 9) ............................................................................. 16 Figure 7 Product size as a function of specific grinding energy – all data ........................................ 16 Figure 8 Projected Hicom 110 kW production rate as a function of product size ............................ 18 Figure 9 Photograph showing the Hicom 25 dry pilot plant ........................................................... 19 Figure 10 Schematic diagram of the Hicom 25 dry pilot plant .......................................................... 20 Figure 11 Hicom pilot plant stearic acid dosing system – reservoir and gear pump ........................ 22 Figure 12 Hicom pilot plant stearic acid dosing system – controls and dosing line .......................... 22 Figure 13 Hicom 25 pilot plant SCADA Trend screen ........................................................................ 24 Figure 14 Hicom 25 pilot plant feed rate estimation example.......................................................... 26 Figure 15 Process parameters corresponding to the time periods shown in Figure 13 and Figure 14 ......................................................................................................................... 26 Figure 16 Results from estimation of recirculation load ratio (RLR) using sum of squares error (SSE) minimization on adjustment of the calculated classifier feed particle size distribution...................................................................................................................... 27 Tables Table 1 Preferred Hicom mill grinding conditions for Nordkalk Parfill 7 ............................................ 5 Table 2 Summary of results for production of 3-4 µm material ........................................................ 9 Table 3 Summary of results for production of 5-6 µm material ...................................................... 10 Table 4 Summary of results for production of 8-9 µm material ...................................................... 11 Author: Dr. Steve Marshall Report Date: 18th September 2010 Revision No: 0 Comments: Initial release for review by customer H-2010.MIS.01 R0 16-September-2010 Page 3 of 28 CONFIDENTIAL Executive Summary for MISEC A series of trials was undertaken on Nordkalk Parfill 7 in the Hicom pilot plant to demonstrate the concept of simultaneous grinding of calcium carbonate and coating with stearic acid in the one process. Stable plant operation was achieved for manufacture of a range of coated product sizes and provided a high degree of confidence in scale-up of the concept. Reliable data on product size as a function of specific grinding energy, and projected Hicom 110 kW mill production capacity as a function of product size was obtained and is presented in this report. It is recommended that Nordkalk undertake their own particle size analysis and evaluation of other powder properties on selected bulk samples generated during this test work. H-2010.MIS.01 R0 16-September-2010 Page 4 of 28 CONFIDENTIAL 1 Introduction Hicom was approached by Prof. Eric Forssberg, principal of MISEC with a view to understanding more about current developments on the Hicom mill. During the course of discussions held in our Brisbane facility, it was explained that Hicom had recently developed a method for simultaneous grinding calcium carbonate and coating with stearic acid. Following this initial meeting, Prof. Forssberg garnered interest from Nordkalk and OMYA SE in undertaking test work in the Hicom pilot plant on their specific materials. This was done under the auspices and sponsorship of the MinBas group to evaluate the technical and economic case for using new technology in Scandinavian mineral process plants. It was agreed that the present Hicom test work would be undertaken for MISEC who would be acting on behalf of MinBas. This report is therefore directed to MISEC. The first material received for testing was one metric ton of Nordkalk Parfill 7 calcium carbonate from Finland. As there were no target size requirements or particle properties specified, the first series of tests was undertaken as a generic proof-of-concept exercise to demonstrate the capabilities of the Hicom process. The purpose of this report is to present results from this first series of trials on the Nordkalk material. The participation (and patience) of Prof. Forssberg during the initial stages of testing is gratefully acknowledged. 2 Objectives Specific objectives of the test work were as follows: 1. Determine suitable conditions for processing Parfill 7 in the Hicom Mill. 2. Estimate mill grinding energy and corresponding production capacity for a Hicom 110 kW mill over a range of coated product sizes. 3. Provide test samples for evaluation by Nordkalk. 3 Conclusions & Recommendations 1. Table 1 below outlines the mill grinding conditions established as being suitable for this application Table 1 Preferred Hicom mill grinding conditions for Nordkalk Parfill 7 Feed Mill Mill speed, rpm Mill filling, vol % Media Mass, kg Media type Media SG, kg/L Media size, mm Liners H-2010.MIS.01 R0 Parfill 7 D97=74 µm Hicom 25 Pilot Plant Hicom 110 Production Mill 760 600 50 60 19.0 175 Ce-TPZ (Zirconox, India) Ce-TPZ (Zirconox, India) 6.1 6.0 1.2-1.4 mm 1.4-1.8 mm 440C Stainless Steel 15/3 Cr/Mo Cast Iron 16-September-2010 Page 5 of 28 CONFIDENTIAL 2. Mill grinding energy and production capacity estimates are provided in sections 5.2.4 (p. 15) and 5.3 (p. 17) of this report. 3. Bulk product samples (5-15 kg) were collected for all test runs. It is suggested that Nordkalk evaluate properties of selected samples from the best runs from each of the three product size groups evaluated. At this stage evaluation of product samples from Runs 2, 3, 6 and 9 would be recommended. H-2010.MIS.01 R0 16-September-2010 Page 6 of 28 CONFIDENTIAL 4 Equipment and procedures 4.1 Hicom 25 pilot plant The Hicom 25 dry pilot plant employed for this test work is described in detail in Appendix A. The grinding media was ‘Zirconox’ Ce-TPZ ceramic media (Jyoti, India). Further details of the operating conditions are provided in Section 5. 4.1.1 Sample / run labelling Each test run sample is given a number, as detailed in the table below: Sample Number – 1st part Sample Number – 2nd Part (example) Description Pilot Plant Tests on Nordkalk Parfill 7 – 1st series NOR.P.A.001 -F Feed material designation -1AP Run/Sample 1A Product (Classifier Fines) -1AD Run/Sample 1A Mill Discharge (Classifier Feed) -1AR Run/Sample 1A Recycle (Classifier Coarse Reject) This labelling convention relates primarily to spreadsheet data and physical samples where provided. In this report, run numbers are given without the first part prefix. Generally, ‘A’ and ‘B’ samples refer to duplicate samples taken at the same run condition. In one case here – Run 5 – the results for A and B samples taken five minutes apart are included to demonstrate consistency of the data. 4.2 Particle Size Measurement Feed and product sizing were measured by laser diffraction on Hicom’s Malvern 2000 Mastersizer (with Hydro 2000MU) under the following conditions: Mineral Type CaCO3 Particle Refractive Index (Mie) 1.530 Particle Absorption Index (Mie) 0.1 Dispersant Distilled Water Dispersant RI 1.33 Pump speed 2000 Dispersion method (non-coated) Dry sample into 700 ml distilled water in beaker with 15 ml 0.5% w/v Calgon T. 30s Ultrasonic Irradiation at Level 12 prior to measurement Dispersion method (coated) Dry sample in test tube with 3 drops Nonidet P40, 15 ml 0.5% w/v Calgon T, shake for 30s, soak for 1 hr. Froth killed with IPA, suspension agitated with pipette and pipetted into 700 ml distilled water in beaker. 30s Ultrasonic Irradiation at Level 12 prior to measurement. 4.3 Data analysis Details of the procedures used for analysis of logged data are given in Appendix B. H-2010.MIS.01 R0 16-September-2010 Page 7 of 28 CONFIDENTIAL 5 Test results & discussion 5.1 Feed material particle size distribution The feed particle size distribution (PSD) measured on our Malvern laser size was close to the supplied customer specification, as seen in Figure 1, although the top size may have been slightly coarser than standard. Parfill 7 (Hicom measurement) Parfill 7 (Customer specification) 100 90 80 % Undersize 70 60 50 40 30 20 10 0 0.1 1 10 100 1000 Size (µm) Figure 1 Nordkalk Parfill 7 feed size distribution compared with customer standard Please note that there is often a wide discrepancy between Malvern (wet) sizing and Insitec (dry, online) sizing data on the same product material. For the sake of consistency, unless noted otherwise, all particle sizes mentioned in this report refer to the Malvern (wet) sizing data. It is also important to recognise that virtually every size analysis method is likely to produce a different result on the same sample. Therefore, the customer needs to analyse physical samples from these pilot plant trials in order to correlate the data and information presented with their own particular knowledge base. 5.2 Pilot plant results Results from all tests are shown in Table 2, Table 3 and Table 4 below. The tabulated data is grouped by product size and discussed below in terms of these groupings. H-2010.MIS.01 R0 16-September-2010 Page 8 of 28 CONFIDENTIAL Table 2 Summary of results for production of 3-4 µm material Run Number System Performance Mill GE based on production rate, kWh/t Feed F97, µm Feed F80, µm Feed F50, µm Malvern (wet) product sizing data Insitec online (dry) product sizing data Recirculating load Ratio Production rate, kg/h Gross Power Draw, kW Net Mill Power Draw, kW Recirculating load, kg/h ACX 200 Classifier Parameters Classifier speed, rpm System air flow, m3/h Secondary air flow, m3/h % Secondary Air ACX200 Classifier Mass Balance FEED, kg/h PRODUCT, kg/h RECYCLE, kg/h System Configuration Mill model Mill speed, rpm Discharge ports Discharge slot width, mm Liner material Media Media size, mm Media S.G. Mill Differential Pressure, mmWG Mill Filling, J% Additive Additive rate vs fresh feed (%w/w) Classifier Efficiency Total Fines Mass Recovery %Passing P97 in Classifier Feed Classifier Efficiency @ P 97 Solids/Air Ratio to Classifier, kg/m3 H110 Plant Parameters Feed rate, kg/h Recycle rate, kg/h Nominal Recirculating load Ratio Classifier feed rate, kg/h H-2010.MIS.01 R0 P97, P90, P80, P50, P97, P90, P80, P50, µm µm µm µm µm µm µm µm 01A 02A 03A 12A 3/08/2010 12:20 150 73.8 51.8 17.5 3.07 2.52 2.15 1.55 3.48 2.54 1.91 0.96 30.0 29 6.65 4.35 870 3/08/2010 16:40 154 73.8 51.8 17.5 2.88 2.38 2.05 1.48 3.40 2.48 1.87 0.95 18.0 29 6.77 4.47 522 6/08/2010 11:25 169 73.8 51.8 17.5 3.42 2.84 2.44 1.77 4.23 3.16 2.44 1.19 15.0 24 6.34 4.04 360 13/09/2010 16:40 150 73.8 51.8 17.5 3.46 2.85 2.44 1.75 4.09 3.09 2.40 1.18 18.0 25 6.06 3.76 450 5283 800 265 33% 5283 800 267 33% 5283 800 274 34% 5285 800 271 34% 899 29 870 551 29 522 384 24 360 475 25 450 Hicom 25 760 Hicom 25 760 Hicom 25 760 Hicom 27 760 2/6 2/6 2/6 1.2 0.9 0.9 1/6*0.6; 1/6*0.9; 1/2*0.4 0.4, 0.6, 0.9 Steel Ce-TPZ 2.4-2.8 6.0 93 52% DEG 0.87 Steel Ce-TPZ 1.4 6.0 125 52% DEG 0.87 Steel Ce-TPZ 1.4 6.0 126 52% Stearic Acid 1.37 Steel Ce-TPZ 1.4 6.0 137 52% Stearic Acid 1.11 3.2% 35.8 8.7% 1.12 5.3% 35.9 14.2% 0.69 6.3% 41.3 14.7% 0.48 5.3% 41.9 12.2% 0.59 600 7400 12 8000 585 7415 13 8000 535 7465 14 8000 600 7400 12 8000 16-September-2010 Page 9 of 28 CONFIDENTIAL Table 3 Summary of results for production of 5-6 µm material Run Number System Performance Mill GE based on production rate, kWh/t Feed F97, µm Feed F80, µm Feed F50, µm Malvern (wet) product sizing data Insitec online (dry) product sizing data Recirculating load Ratio Production rate, kg/h Gross Power Draw, kW Net Mill Power Draw, kW Recirculating load, kg/h ACX 200 Classifier Parameters Classifier speed, rpm System air flow, m3/h Secondary air flow, m3/h % Secondary Air ACX200 Classifier Mass Balance FEED, kg/h PRODUCT, kg/h RECYCLE, kg/h System Configuration Mill model Mill speed, rpm Discharge ports Discharge slot width, mm Liner material Media Media size, mm Media S.G. Mill Differential Pressure, mmWG Mill Filling, J% Additive Additive rate vs fresh feed (%w/w) Classifier Efficiency Total Fines Mass Recovery %Passing P97 in Classifier Feed Classifier Efficiency @ P 97 Solids/Air Ratio to Classifier, kg/m3 H110 Plant Parameters Feed rate, kg/h Recycle rate, kg/h Nominal Recirculating load Ratio Classifier feed rate, kg/h H-2010.MIS.01 R0 P97, P90, P80, P50, P97, P90, P80, P50, µm µm µm µm µm µm µm µm 04A 05A 05B 06A 11A 6/08/2010 17:27 131 73.8 51.8 17.5 5.16 4.13 3.44 2.30 6.21 4.87 4.01 2.50 8.0 28 5.98 3.68 224 12/08/2010 15:25 138 73.8 51.8 17.5 4.79 3.87 3.26 2.21 6.05 4.53 3.61 1.98 9.0 29 6.31 4.01 261 12/08/2010 15:30 138 73.8 51.8 17.5 4.85 3.92 3.30 2.26 6.01 4.51 3.61 2.00 9.0 29 6.30 4.00 261 18/08/2010 14:05 113 73.8 51.8 17.5 4.97 4.00 3.36 2.28 6.25 4.78 3.83 2.22 7.6 31 5.81 3.51 236 2/09/2010 18:50 124 73.8 51.8 17.5 5.64 4.49 3.72 2.48 5.97 4.56 3.68 2.09 21.0 37 6.88 4.58 777 3740 800 277 35% 3682 801 278 35% 3682 800 278 35% 3758 797 277 35% 3627 800 285 36% 252 28 224 290 29 261 290 29 261 267 31 236 814 37 777 Hicom 25 760 Hicom 25 760 Hicom 25 760 Hicom 25 760 Hicom 26 760 2/6 1/6*0.6; 1/6*0.9 1/6*0.6; 1/6*0.9 1/6*0.6; 1/6*0.9 0.9 0.6, 0.9 0.6, 0.9 0.6, 0.9 1/6*0.6; 1/6*0.9; 1/2*0.4 0.4, 0.6, 0.9 Steel Ce-TPZ 1.4 6.0 133 52% Stearic Acid 1.27 Steel Ce-TPZ 1.4 6.0 155 52% Stearic Acid 1.23 Steel Ce-TPZ 1.4 6.0 155 52% Stearic Acid 1.23 Steel Ce-TPZ 1.4 6.0 158 52% Stearic Acid 1.15 Steel Ce-TPZ 1.4 6.0 121 52% Stearic Acid 0.96 11.1% 49.8 21.6% 0.32 10.0% 45.6 21.3% 0.36 10.0% 96.6 10.0% 0.36 11.6% 44.3 25.4% 0.33 4.5% 49.6 8.9% 1.02 760 6080 8 6840 725 6525 9 7250 725 6525 9 7250 885 6726 8 7611 730 7270 10 8000 16-September-2010 Page 10 of 28 CONFIDENTIAL Table 4 Summary of results for production of 8-9 µm material Run Number System Performance Mill GE based on production rate, kWh/t Feed F97, µm Feed F80, µm Feed F50, µm Malvern (wet) product sizing data Insitec online (dry) product sizing data Recirculating load Ratio Production rate, kg/h Gross Power Draw, kW Net Mill Power Draw, kW Recirculating load, kg/h ACX 200 Classifier Parameters Classifier speed, rpm System air flow, m3/h Secondary air flow, m3/h % Secondary Air ACX200 Classifier Mass Balance FEED, kg/h PRODUCT, kg/h RECYCLE, kg/h System Configuration Mill model Mill speed, rpm Discharge ports Discharge slot width, mm Liner material Media Media size, mm Media S.G. Mill Differential Pressure, mmWG Mill Filling, J% Additive Additive rate vs fresh feed (%w/w) Classifier Efficiency Total Fines Mass Recovery %Passing P97 in Classifier Feed Classifier Efficiency @ P 97 Solids/Air Ratio to Classifier, kg/m3 H110 Plant Parameters Feed rate, kg/h Recycle rate, kg/h Nominal Recirculating load Ratio Classifier feed rate, kg/h H-2010.MIS.01 R0 P97, P90, P80, P50, P97, P90, P80, P50, µm µm µm µm µm µm µm µm 07A 08A 09A 10A 31/08/2010 16:10 80 73.8 51.8 17.5 7.95 6.19 5.02 3.11 7.99 6.11 4.98 3.01 9.0 47 6.05 3.75 423 31/08/2010 18:00 76 73.8 51.8 17.5 9.25 6.98 5.57 3.40 7.95 6.12 5.02 3.09 11.2 53 6.35 4.05 594 2/09/2010 15:49 73 73.8 51.8 17.5 8.56 6.58 5.27 3.17 8.04 6.12 4.98 2.98 4.2 49 5.90 3.60 206 2/09/2010 17:25 77 73.8 51.8 17.5 8.53 6.61 5.32 3.24 8.47 6.35 5.09 3.05 11.0 56 6.59 4.29 616 2364 798 283 35% 2392 799 281 35% 2365 799 277 35% 2394 798 285 36% 470 47 423 647 53 594 255 49 206 672 56 616 Hicom 25 760 Hicom 25 760 Hicom 25 760 Hicom 25 760 1/6*0.6; 1/6*0.9; 1/2*0.4 0.4, 0.6, 0.9 1/6*0.6; 1/6*0.9; 1/2*0.4 0.4, 0.6, 0.9 1/6*0.6; 1/6*0.9; 1/2*0.4 0.4, 0.6, 0.9 1/6*0.6; 1/6*0.9; 1/2*0.4 0.4, 0.6, 0.9 Steel Ce-TPZ 1.4 6.0 150 52% Stearic Acid 0.76 Steel Ce-TPZ 1.4 6.0 132 52% Stearic Acid 0.72 Steel Ce-TPZ 1.4 6.0 152 52% Stearic Acid 0.99 Steel Ce-TPZ 1.4 6.0 125 52% Stearic Acid 0.87 10.0% 50.3 19.3% 0.59 8.2% 59.5 13.4% 0.81 19.2% 53.2 35.1% 0.32 8.3% 53.3 15.2% 0.84 1125 6875 6 8000 1180 6820 6 8000 1360 5712 4 7072 1175 6825 6 8000 16-September-2010 Page 11 of 28 CONFIDENTIAL 5.2.1 Product size 3-4 µm (P97) - Table 2 This series of test runs was conducted with the classifier rotor speed fixed at 5300 RPM (nominal). While the ACX200 classifier is capable of higher speed (hence finer cut size), the speed used was a conservative value that can be applied for scale up to the larger classifier sizes required for a production plant. The system air rate is obviously an important influence on classifier cut size also. Again, we adopted a conservative approach of using a relatively high system air rate of 800 m3/h to ensure reliable material transport in the grinding circuit. This air rate was used for all trials on Parfill 7. In short, the product sizes obtained during these pilot plant trials can be readily achieved in a full scale production plant using Hicom 110 kW mills with a commercially available classifier. 5.2.1.1 DEG only runs Runs 1 and 2 were conducted with grinding aid only (diethylene glycol – DEG) to demonstrate the system capability without stearic acid coating. This was of relevance as it is well known that in ball mills for example, the grinding energy is greatly increased and hence production capacity is decreased when attempting to grind and coat in the one machine. While the grinding energy in both of these runs was similar, Run 2 conducted using 1.4 mm media had a much lower circulating load compared to Run 1 conducted using 2.4-2.8 mm media. In addition, the product size for Run 2 was slightly lower. From this comparison we concluded that operation using the finer media was more efficient (as expected) and all subsequent runs were conducted using the 1.4 mm media. 5.2.1.2 Stearic acid coating runs In going to relatively high levels of stearic acid dosing in Runs 3 and 12, we see that the grinding energy was similar to that obtained with DEG at the same classifier speed. However, the coated product size is slightly higher. The higher product size can be attributed to more effective dispersion of material in the classifier separation zone. It is a known phenomenon of calcium carbonate air classification that as the circulating load increases, the particle top cut decreases even though the classifier rotor speed and system air rate remain unchanged. This phenomenon probably occurs because of a ‘filtering’ effect of high solids loading in the swirling air in the separation zone just outside the classifier rotor. The effect is quite clearly seen in Figure 2 which reproduces a chart from the Insitec online particle size analyser. The red trace shows laser light transmission level which is inversely proportional to the amount of material in the sampling pipe; higher transmission means lower solids loading. The steady increase in product particle size (black traces) with increase in transmission (decrease in solids loading) can clearly be seen in the chart. H-2010.MIS.01 R0 16-September-2010 Page 12 of 28 CONFIDENTIAL Figure 2 Example of changing product size with change in classifier solids loading With stearic acid coating, the particles are more dispersed than with DEG alone, which is likely to reduce the solids-loading filtering effect observed with non-coated material. This may partially explain the coarser top cut with coated material at similar circulating loads, classifier speed and system air rate, compared with non-coated material. 5.2.1.3 Product size distributions The product size distributions shown in Figure 3 for the finest products made illustrate the difference in classifier performance on coated and uncoated materials. The marked difference in distribution shape as reported by the two measurement methods is also apparent. NOR.P.A.001-2AP Insitec (2A) NOR.P.A.001-3AP Insitec (3A) 100 90 80 % Undersize 70 60 50 40 30 20 10 0 0.1 1 10 Size (µm) Figure 3 H-2010.MIS.01 R0 Product size distributions from the finest uncoated (Run 2) and coated (Run 3) product samples 16-September-2010 Page 13 of 28 CONFIDENTIAL 5.2.2 Product size 5-6 µm (P97) - Table 3 For this series of tests, the Insitec size controller was set to a top cut (D97) of 6 µm nominal. The classifier speed was allowed to vary under automatic control to maintain this cut size. An example of such control can be seen in Figure 4. D97 (Insitec) D97 Set Point 4000 7 3900 6.8 3800 6.6 3700 6.4 3600 6.2 3500 6 3400 5.8 3300 5.6 3200 5.4 3100 5.2 3000 12/08 14:00 Figure 4 12/08 14:30 12/08 15:00 12/08 15:30 12/08 16:00 Size (µm) Classifier Rotor Speed (RPM) Classifier Speed 5 12/08 16:30 Example of product size control by automatic regulation of classifier speed The product size distribution from Run 6 is shown in Figure 5. In general, the Malvern-measured product size was somewhat lower and more variable than the Insitec-reported size, which is due to the different measurement method and also possibly from variability in product sampling. The data from Runs 4-6 is fairly consistent in terms of product rate. The lowest grinding energy and smallest product size was obtained in Run 6. In Run 11, the discharge open area on the grinding chamber was increased and the process was ‘pushed’ at a high circulating load. While this resulted in a significantly higher production rate, the specific grinding energy was more or less the same as for Run 6. This result demonstrates one way that production rate can be increased in the Hicom process. H-2010.MIS.01 R0 16-September-2010 Page 14 of 28 CONFIDENTIAL NOR.P.A.001-6AP Insitec (P) 100 90 80 % Undersize 70 60 50 40 30 20 10 0 0.1 1 10 100 Size (µm) Figure 5 5.2.3 PSD for intermediate coated product (Run 6) Product size 8-9 µm (P97) - Table 4 For this series of tests, the product size controller was set to a D97 cut size (Insitec) of 8 µm. The particle size distribution for Run 9 product is shown in Figure 6. The data from Runs 7-10 showed a high degree of consistency in terms of specific grinding energy, but with variation in production rate and power draw. This consistency indicates that the process was probably quite well optimised for this product size under the range of conditions tested. The best result was obtained with Run 9, which had the lowest grinding energy at a relatively low circulating load rate. 5.2.4 Product size versus specific grinding energy Figure 7 shows all of the P97 versus grinding energy test data. For the stearic acid coating runs, a line drawn through the minimum grinding energy values represents the best performance obtained in the pilot plant. The DEG only data points are only slightly below this line. This clearly shows that there was only a small reduction in process energy efficiency with simultaneous grinding and coating as compared to grinding only using a typical glycol grinding aid. This result is highly significant as it markedly differentiates the Hicom process from any other size reduction method currently available for grinding and coating calcium carbonate. H-2010.MIS.01 R0 16-September-2010 Page 15 of 28 CONFIDENTIAL NOR.P.A.001-9AP Insitec (P) 100 90 80 % Undersize 70 60 50 40 30 20 10 0 0.1 1 10 100 Size (µm) Figure 6 PSD for coarse coated product (Run 9) DEG Only Stearic acid coated P97 Malvern (µm) 10 MINIMUM GRINDING ENERGY LINE 1 10 100 1000 Mill Specific Grinding Energy (kW.h/t) Figure 7 H-2010.MIS.01 R0 Product size as a function of specific grinding energy – all data 16-September-2010 Page 16 of 28 CONFIDENTIAL 5.3 Scale-up and Hicom 110 production capacity Experience has shown that full scale production capacity can usually be estimated from pilot plant test results on the basis of mill specific grinding energy. This is because the grinding environment in the Hicom 25 test mill is virtually identical to that in a Hicom 110 kW mill, provided the circulating load is not too high. The Hicom 110/60 mill has a nominal net power draw capability of 100 kW. Therefore estimates of the corresponding capacity for a single Hicom 110/60 mill are obtained as follows: Hicom 110 Mill Capacity (tph) = 100 (kW) / Pilot Plant Mill Grinding Energy (kWh/t) In a number of the present test runs, the circulating load was relatively high due to the process being ‘pushed’ as much as possible to maximise production rate. However, in almost all such cases, a small drop in fresh feed rate – no more than 10% – was sufficient to bring the circulating load down to a low and stable level. Experience has also shown that the total mill throughput (that is the circulating load, equal to fresh feed plus recycle) should not exceed about 8000 kg/h in practice. Therefore, for those runs where the projected full-scale circulating load calculated directly from the pilot plant recycle ratio exceeded 8000 kg/h, the classifier feed rate was capped at this value in the results tables shown above. The projected Hicom mill capacity was also reduced by 10% for these runs. In other words, a value of 90 kW was used in the above formula rather than the full 100 kW. The projected Hicom 110 kW mill capacity as a function of product size shown in Figure 8 below was determined on the basis just described. The maximum capacity line shown corresponds to the minimum energy line shown in Figure 7. We have a high level of confidence that these production capacities would be achieved in practice. 5.4 Comments on production plant design Overall, stable plant operation was obtained over the full range of conditions reported here. Similar stable performance can be expected in a full scale production plant using Hicom 110 kW mills. It is recognised that production capacity for a single Hicom 110 kW mill on the finest product may not be economic. Therefore, we would propose a production plant concept using two Hicom 110 kW mill operating in parallel but with a single classifier, system air blower and product collection filter. This way, a doubling in mill capacity can be achieved with more or less the same capital outlay for construction of the balance of the plant. Details on a plant design utilising this two-mill concept are available on request. H-2010.MIS.01 R0 16-September-2010 Page 17 of 28 CONFIDENTIAL DEG only Stearic Acid Coating 2000 Production Rate in H110 mill (kg/h) 1800 1600 MAXIMUM CAPACITY LINE 1400 1200 1000 800 600 400 200 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 P97 Malvern (µm) Figure 8 H-2010.MIS.01 R0 Projected Hicom 110 kW production rate as a function of product size 16-September-2010 Page 18 of 28 CONFIDENTIAL Appendix A – Hicom 25 Dry Pilot Plant: Generic Description and Operating Procedures IMPORTANT NOTE: The data presented in Appendices A and B is generic and may not correspond to actual data obtained during the present test program. Generic Description of the plant The Hicom 25 dry pilot plant is shown in the picture below (Figure 9) and schematically in Figure 10. The plant consists of a Hicom 25 kW mill with variable speed drive, operating in closed circuit with a Comex ACX200 high efficiency air classifier. The entire plant is controlled and monitored using a Siemens S7-300 PLC and Siemens WinCC SCADA package operating on a touch-panel PC mounted in the main control cabinet. Figure 9 Photograph showing the Hicom 25 dry pilot plant A 75 mm screw feeder is used to transport material to the mill from a feed bin. Solids feed rate to the mill is calculated from loss-in-weight measurement from a load cell on the feed hopper. The calculated rate can be used in closed loop with the screw feeder VSD to provide feed rate control. The Hicom 25 mill motor is controlled by a Siemens VSD in the main control cabinet. The mill is generally operated at discrete speeds of 760 and 960 RPM corresponding to maximum chamber acceleration of 30 and 50 G respectively. The mill drive lubrication system is monitored and controlled by the central Siemens PLC. H-2010.MIS.01 R0 16-September-2010 Page 19 of 28 CONFIDENTIAL FT FIC PI FI VSD M IA PI DUST COLLECTOR 200 NB INSITEC 15 0 N B PI COM MEX ACX 200 CLASSIF IER FI FT PI PI M VSD JT JI SYSTEM BLOWER 1 LOAD CELL FI FT FEED HOPPER SECONDARY AIR VALVE PI W FINE PRODUCT COLLECTION VSD M 100 NB FIC 100 NB FI JI JT VSD M TS TI PI PT HICOM 25 MILL PEBBLE TRAP Figure 10 H-2010.MIS.01 R0 18-September-2010 PRIMARY AIR VALVE Schematic diagram of the Hicom 25 dry pilot plant Page 20 of 28 CONFIDENTIAL The grinding circuit operates under vacuum in order to avoid dust emission. Material is drawn through the mill and pneumatically conveyed to the classifier. The air flow required for effective pneumatic transport through the mill is much less than that required for effective classification. Therefore, additional air is drawn into the system through the primary air valve indicated on Figure 10. The setting of this valve and the secondary air valve also control the differential pressure across the mill – that is the mill vacuum. Oversize particles, rejected by the classifier rotor, fall by gravity down the oversize chute for regrinding in the mill. The classifier is operated by a VSD which allows the rotor speed to be set to achieve a precise product top cut size. Compressed air is used to seal both the classifier rotor and the rotor bearings. The classifier oversize return is sealed by a 150 mm double-butterfly valve air lock system as indicated on the diagram. The secondary air flow to the classifier is manually adjusted by a butterfly valve, and monitored by an orifice-plate flow meter. Air and fine product are pneumatically transported to a Torit-DCE DLM V20/12B Dalamatic dust collector where the product is collected in a drum or bulker bag. The dust collector is sealed by a 200 mm double-butterfly valve air lock system. An Insitec on-line particle size analyser is installed on the classifier fine-product line. This enables instant feedback on classifier performance and provides the means for meeting precise particle size specifications by automatic adjustment of classifier rotor speed. Two blowers operated in parallel are used to generate the system air flow. A Rietschle SAP1500 (System Blower 2) is run at full speed, and a GAST R93150A (System Blower 1) is operated by a VSD to provide trim control on system air flowrate in closed-loop feedback with an orifice-plate flow meter downstream of the dust collector. The total system air capability is roughly 1600 m3/hr at 20 kPa using both blowers. Instrumentation is incorporated for monitoring critical process and mill control parameters, most of which are recorded on the SCADA system. The mill power draw is determined from direct reading of the Mill VSD. A microwave mass-flow indicator installed on the classifier feed (mill discharge) line provides feedback as to whether the plant is at steady state. The grinding chamber nominal volume is 10.7 L and its 40 mm discharge ports are positioned at the circle of maximum diameter. Grates are placed over the discharge ports to retain the media inside the grinding chamber. The grate slot width is generally selected at least one-half the diameter of the smallest media particle used. Stearic acid dosing system The stearic acid dosing system for particle coating is shown in Figure 11 and Figure 12 below. Stearic acid flakes (Symex #4989, Symex Holdings, Melbourne) are melted in the heated reservoir shown, which is maintained at 70-80oC. The heated liquid stearic acid is then dosed directly (drip-wise) into the feed tube of the Hicom mill through a heat-traced stainless steel tube using a Zenith gear pump with DC speed control, which is also heat-traced. The gear pump enables precise, controlled and reproducible dosing over a linear dosing rate calibration range of 4-20 g/min. H-2010.MIS.01 R0 18-September-2010 Page 21 of 28 CONFIDENTIAL As there is also fresh feed rate control on the plant, the stearic acid dosing can be manually ratioed to that as required. Figure 11 Hicom pilot plant stearic acid dosing system – reservoir and gear pump Figure 12 Hicom pilot plant stearic acid dosing system – controls and dosing line H-2010.MIS.01 R0 18-September-2010 Page 22 of 28 CONFIDENTIAL Typical test procedure After every chamber change-out, or after an extended shutdown, the mill is operated for twenty minutes with an empty chamber to establish the no-load power. The required charge of media is added to the mill before commencing each test series. The solids feed rate to the mill is selected, and the system and secondary air flows set to maintain appropriate classifier conditions. The classifier rotor speed is then adjusted to give the desired cut size based on Insitec particle size readings. Product and recycle samples are taken once relatively steady-state plant operation is obtained, as indicated by the mill discharge mass flow indicator. This is generally 30 to 45 minutes after starting a run. Critical mill control and process parameters are monitored during each run and recorded on a standard log sheet every time a sample is taken. The recirculating load rate is estimated after taking a physical sample of the mill discharge after a crash stop of the plant. The particle size distributions of the classifier feed, fine product and coarse reject streams can be used to back-calculate the recirculating load ratio. The rate of product discharge from the dust collector is calculated from gain-in-weight measurement of the product bulk bag, which is positioned on electronic weigh-scales. This rate is compared with the feed rate to assess whether the circuit is at steady state. Generally, the feed and measured product rates must be within 20% of one another, otherwise the data is from the run is not considered for analysis. The exception to this rule is when the material is very fine or sticky and there is significant holdup of material in the dust collector. Under such conditions, accurate determination of product rate is not possible over a short time period, and we rely on microwave sensor readings of the circulating load to determine if the plant is at steady state. The mill net power draw for calculation of specific mill grinding energy is determined as the difference between the measured gross power and the no-load power. Grinding circuit behaviour and sampling Typical circuit responses for dry pilot plant operation and the test protocol followed are best illustrated with reference to Figure 13 below, which shows a characteristic SCADA trend obtained during a pilot plant trial. In the example shown in Figure 13 , between 5:54 pm and 6:10 pm, the mill power draw (red trace) was around 11 kW, the circulating load (black trace) was below 10% and the mill exit temperature (light blue trace) was around 72oC. The feed rate (oscillating blue trace) was increased slightly at around 6:10 pm. This resulted in an increase in circulating load, a decrease in mill power and a decrease in mill temperature due to the increased rate of heat removal from the mill from the higher solids throughput. Despite the increased circulating load, the circuit is nevertheless stable as the circulating load is not increasing above 15-20% on average. This indicated level of circulating load was considered the maximum stable level for plant operation in this particular case. Experience showed that further increases in feed rate resulted in accelerating increase in circulating load rate due to the fact that the rate of fresh feed to the mill started to exceed the rate of fine particle production. H-2010.MIS.01 R0 18-September-2010 Page 23 of 28 CONFIDENTIAL Figure 13 Hicom 25 pilot plant SCADA Trend screen The objective in pilot plant trials was to adjust conditions such as discharge port open area, mill vacuum, media size and quantity and other factors to try and maximize the mill feed rate before an excessive circulating load rate was reached. In the example shown in Figure 13, at around 6:36 pm, the plant was stopped (crash stop) by stopping the mill, air blowers, the classifier and by shutting the classifier return air lock valves. This way, a ‘snap shot’ was taken of the circuit from which samples could be taken for analysis. We sampled the recycle stream, the residual powder on the internal walls of the mill body (equivalent to classifier feed) and also the fine product collected in the product filter. These samples were used to estimate recirculating load ratio, as outlined in Appendix B. For some runs, the mill contents may also be removed and the powder and grinding media separated by screening. This way it is possible to determine the holdup level of powder in the mill and also to assess media wear. H-2010.MIS.01 R0 18-September-2010 Page 24 of 28 CONFIDENTIAL Appendix B – Data Analysis Procedures IMPORTANT NOTE: The data presented in Appendices A and B is generic and may not correspond to actual data obtained during the present test program. Test conditions All of the data logged on the SCADA system was collated into Excel spreadsheets. Where necessary, a simple first order filter was applied to smooth the data for more accurate estimation of parameter values at the time of sample collection or crash stop. The resulting values are shown in the test condition tables in the body of this report. Feed and product rate For most test runs, estimation of feed and product rate was done by calculating the numerical derivative of the recorded change in weight of the feed hopper and the product weigh scales respectively. First-order filtering before and after numerical differentiation was used to reduce the affect of inherent ‘noise’ in the data. Typical rate calculation results are illustrated in Figure 14 below. Figure 15 shows the corresponding process parameters of mill air temperature (discharge temperature), mill power and circulating load corresponding to the same time period of the data in Figure 13 and Figure 14. It can be seen that a relatively small increase in average feed rate from around 58 kg/h to around 62 kg/h resulted in a significant increase in circuit load and it was concluded that further increase was not possible beyond around 62 kg/h for this particular mill and plant configuration. Circulating load ratio estimation The circulating load ratio, hence coarse recycle rate, was estimated from the particle size distribution of samples of classifier feed, fine product and coarse reject. The Excel solver function was used to minimize the sum of squares of the difference between measured particles size distribution and the corresponding particle size distribution calculated using an assumed ratio and the other two distributions. Generally, the measured classifier feed was considered the least accurate of the collected samples and this was usually taken as the basis for the estimation procedure. In the example shown in Figure 16 below, it can be seen the calculated and measured classifier feed distribution closely match, which gives a high level of confidence in the ratio of 6.6 calculated for this particular test run. Calculation of the ratio using the coarse return and the fine product was also done to verify accuracy of the primary estimate. In most cases, variation in calculated values was less than 10%. The coarse recycle rate was then obtained by multiplying the steady state feed rate by the estimated recirculating load ratio. For those trial runs where no crash-stop samples were collected, the ratio was estimated from the recirculating load level indicated on the microwave sensor output. These estimates were considered accurate only within 20%. H-2010.MIS.01 R0 18-September-2010 Page 25 of 28 CONFIDENTIAL Calculated Feed rate (filtered) Feed rate (PLC output) Feed Hopper Weight (raw) Feed Hopper Weight (filtered) 100 620.0 90 600.0 80 70 580.0 50 560.0 WT (kg) RATE (kg/h) 60 40 540.0 30 20 520.0 10 0 500.0 19/03/2010 16:00 Figure 14 19/03/2010 17:00 19/03/2010 18:00 Hicom 25 pilot plant feed rate estimation example Air Temp Mill Power Circulating Load 80.0 70.0 60.0 50.0 40.0 30.0 20.0 10.0 0.0 19/03/2010 16:00 Figure 15 19/03/2010 17:00 19/03/2010 18:00 Process parameters corresponding to the time periods shown in Figure 13 and Figure 14 H-2010.MIS.01 R0 18-September-2010 Page 26 of 28 CONFIDENTIAL Measured classifier f eed Measured coarse reject Calculated Classifier Feed Measured f ine product 100 90 80 % Undersize 70 60 50 40 30 20 10 0 0.1 1 10 100 Size (µm) Figure 16 Results from estimation of recirculation load ratio (RLR) using sum of squares error (SSE) minimization on adjustment of the calculated classifier feed particle size distribution H-2010.MIS.01 R0 18-September-2010 Page 27 of 28 CONFIDENTIAL DISCLAIMER 1. In conducting equipment testing, careful regard is given to the customer’s requirements. However, operating conditions and materials used in testing cannot be guaranteed to replicate all operating materials or conditions in actual industrial use. 2. The results shown in this test report may differ with different materials or in different environmental or operating conditions. Hicom is not liable to you or any other person in relation to any failure to duplicate the results in this test report. 3. Hicom warrants only that: • It has taken reasonable care in the conduct of tests and the preparation of this report; and • The test results in this report reflect the test results achieved. 4. Hicom does not make, and will not be liable for any other representations or warranties, expressed or implied. 5. This report is provided subject to confidentiality, only for the information of the party to whom it is addressed and solely for the purpose of that party assessing Hicom’s equipment. Hicom accepts no responsibility for any reliance placed on this report by any other party. H-2010.MIS.01 R0 18-September-2010 Page 28 of 28 Bilaga 5 Hicom Technologies Pty Ltd Head Office: 67 Randle Road, Pinkenba QLD 4008 Australia Tel: +61 7 3121 2900 Fax: +61 7 3121 2901 Confidential Report H‐2011.MIS.02 Hicom pilot plant dry grinding trials on Calcium Carbonate for Misec AB: OMYACARB 10 results CONFIDENTIAL Contents 1 Introduction ..................................................................................................................................... 3 2 Test results & discussion ................................................................................................................. 3 2.1 Feed material particle size distribution ................................................................................... 3 2.2 Pilot plant results ..................................................................................................................... 3 2.3 Product size versus specific grinding energy ........................................................................... 7 2.3.1 2.4 Comparison with Nordkalk data ...................................................................................... 7 Hicom 110 production capacity............................................................................................... 8 Figures Figure 1 OMYACARB 10 feed size distribution compared with Nordkalk Parfill 7 .............................. 3 Figure 2 Product size as a function of specific grinding energy – all data ........................................... 7 Figure 3 P97 versus grinding energy: present data compared with Nordkalk results ......................... 8 Figure 4 Projected Hicom 110 kW production rate as a function of product size .............................. 9 Tables Table 1 OMYACARB‐10 trials – summary of test conditions and results (1) ....................................... 4 Table 2 OMYACARB‐10 trials – summary of test conditions and results (2) ....................................... 5 Table 3 OMYACARB‐10 trials – summary of test conditions and results (3) ....................................... 6 Author: Dr. Steve Marshall Report Date: 25th January 2011 Revision No: 0 Comments: Initial release for review by customer H‐2011.MIS.02 R0.docx 25‐January‐2011 Page 2 of 10 CONFIDENTIAL 1 Introduction This report presents results from a second series of trials on simultaneous grinding and coating of calcium carbonate undertaken for Misec AB. The test material was a typical limestone sourced from OMYA Australia, chosen with the aim of providing OMYA‐SE with samples of coated product for evaluation in Sweden. Details of the background to this test program and also of the Hicom pilot plant and data analysis procedures are provided in the first report to Misec AB (Hicom No. H‐2010.MIS.01 R1). The focus here is on summarizing the results and comparing them with those obtained from testing of Nordkalk feed material. 2 Test results & discussion 2.1 Feed material particle size distribution Figure 1 shows that the OMYACARB‐10 feed material was slightly finer than the Parfill 7 used for the first series of trials, but otherwise typical of a ball‐milled product. OMYACARB-10 NORDKALK PARFILL 7 100 90 80 % Undersize 70 60 50 40 30 20 10 0 0.1 1 10 100 Particle Size (µm) Figure 1 OMYACARB 10 feed size distribution compared with Nordkalk Parfill 7 2.2 Pilot plant results Test conditions and results from all pilot plant runs are shown in Table 1, Table 2 and Table 3 below. H‐2011.MIS.02 R0.docx 25‐January‐2011 Page 3 of 10 CONFIDENTIAL Table 1 OMYACARB‐10 trials – summary of test conditions and results (1) Run Number System Performance Mill GE based on production rate, kWh/t Feed F97, µm Feed F80, µm Feed F50, µm Malvern (wet) product sizing data Insitec online (dry) product sizing data Recirculating load Ratio Production rate, kg/h Gross Power Draw, kW Net Mill Power Draw, kW Recirculating load, kg/h ACX 200 Classifier Parameters Classifier speed, rpm System air flow, m3/h Secondary air flow, m3/h % Secondary Air ACX200 Classifier Mass Balance FEED, kg/h PRODUCT, kg/h RECYCLE, kg/h System Configuration Mill speed, rpm Liner material Media Media size, mm Media S.G. Mill Differential Pressure, mmWG Mill Filling, J% Additive Additive rate vs fresh feed (%w/w) Classifier Efficiency Total Fines Mass Recovery %Passing P97 in Classifier Feed Classifier Efficiency @ P97 Solids/Air Ratio to Classifier, kg/m3 H110 Plant Parameters Feed rate, kg/h Recycle rate, kg/h Nominal Recirculating load Ratio Classifier feed rate, kg/h H‐2011.MIS.02 R0.docx P97, P90, P80, P50, P97, P90, P80, P50, µm µm µm µm µm µm µm µm 01A 02A 03A 04A 05A 05B 06A 06B 07A 07B 18/11/2010 16:30 164 43.0 30.7 11.1 2.81 2.31 1.99 1.44 3.07 2.24 1.66 0.89 3.5 25 6.45 4.15 89 18/11/2010 17:45 168 43.0 30.7 11.1 2.60 2.16 1.87 1.36 3.10 2.27 1.69 0.89 7.7 26 6.68 4.38 201 27/11/2010 8:53 181 43.0 30.7 11.1 2.66 2.20 1.89 1.35 3.15 2.29 1.71 0.90 6.8 27 7.25 4.95 187 27/11/2010 11:25 193 43.0 30.7 11.1 3.28 2.72 2.35 1.70 4.20 3.16 2.45 1.20 9.8 20 6.14 3.84 194 29/11/2010 14:58 185 43.0 30.7 11.1 3.33 2.76 2.37 1.71 4.08 3.04 2.33 1.14 6.5 20 6.02 3.72 131 29/11/2010 15:30 186 43.0 30.7 11.1 3.34 2.77 2.39 1.73 4.11 3.06 2.35 1.15 9.1 21 6.18 3.88 190 29/11/2010 16:18 192 43.0 30.7 11.1 3.46 2.84 2.42 1.72 4.10 3.06 2.35 1.15 13.5 22 6.44 4.14 290 29/11/2010 16:53 180 43.0 30.7 11.1 3.60 2.95 2.51 1.78 4.10 3.07 2.36 1.16 8.8 22 6.25 3.95 193 29/11/2010 17:30 199 43.0 30.7 11.1 3.32 2.75 2.37 1.72 4.03 3.02 2.31 1.14 18.2 23 6.80 4.50 411 29/11/2010 17:55 188 43.0 30.7 11.1 3.32 2.75 2.37 1.72 4.21 3.08 2.34 1.14 18.2 23 6.63 4.33 421 5283 799 247 31% 5283 800 250 31% 5283 800 267 33% 5285 801 262 33% 5285 799 248 31% 5285 799 250 31% 5285 800 254 32% 5285 800 252 32% 5285 799 256 32% 5284 799 259 32% 114 25 89 227 26 201 215 27 187 214 20 194 151 20 131 211 21 190 311 22 290 215 22 193 434 23 411 444 23 421 760 Steel Ce-TPZ 1.4 6.0 175 52% DEG 1.00 760 Steel Ce-TPZ 1.4 6.0 170 52% DEG 0.97 760 Steel Ce-TPZ 1.4 6.0 147 52% DEG 1.38 760 Steel Ce-TPZ 1.4 6.0 195 52% Stearic Acid 0.87 760 Steel Ce-TPZ 1.4 6.0 181 52% Stearic Acid 1.12 760 Steel Ce-TPZ 1.4 6.0 177 52% Stearic Acid 1.08 760 Steel Ce-TPZ 1.4 6.0 167 52% Stearic Acid 1.29 760 Steel Ce-TPZ 1.4 6.0 169 52% Stearic Acid 1.26 760 Steel Ce-TPZ 1.4 6.0 159 52% Stearic Acid 1.34 760 Steel Ce-TPZ 1.4 6.0 145 52% Stearic Acid 1.32 22.2% 49.5 43.5% 0.14 11.5% 41.2 27.1% 0.28 12.8% 42.7 29.0% 0.27 9.3% 47.8 18.9% 0.27 13.3% 45.5 28.3% 0.19 9.9% 43.9 21.8% 0.26 6.9% 42.7 15.7% 0.39 10.2% 46.4 21.3% 0.27 5.2% 41.4 12.2% 0.54 5.2% 42.1 12.0% 0.56 610 2136 4 2746 595 4577 8 5172 555 3791 7 4346 520 5074 10 5594 540 3518 7 4058 540 4923 9 5463 520 7003 13 7523 555 4890 9 5445 455 7545 17 8000 480 7520 16 8000 25‐January‐2011 Page 4 of 10 CONFIDENTIAL Table 2 OMYACARB‐10 trials – summary of test conditions and results (2) Run Number System Performance Mill GE based on production rate, kWh/t Feed F97, µm Feed F80, µm Feed F50, µm Malvern (wet) product sizing data Insitec online (dry) product sizing data Recirculating load Ratio Production rate, kg/h Gross Power Draw, kW Net Mill Power Draw, kW Recirculating load, kg/h ACX 200 Classifier Parameters Classifier speed, rpm System air flow, m3/h Secondary air flow, m3/h % Secondary Air ACX200 Classifier Mass Balance FEED, kg/h PRODUCT, kg/h RECYCLE, kg/h System Configuration Mill speed, rpm Liner material Media Media size, mm Media S.G. Mill Differential Pressure, mmWG Mill Filling, J% Additive Additive rate vs fresh feed (%w/w) Classifier Efficiency Total Fines Mass Recovery %Passing P97 in Classifier Feed Classifier Efficiency @ P97 Solids/Air Ratio to Classifier, kg/m3 H110 Plant Parameters Feed rate, kg/h Recycle rate, kg/h Nominal Recirculating load Ratio Classifier feed rate, kg/h H‐2011.MIS.02 R0.docx P97, P90, P80, P50, P97, P90, P80, P50, µm µm µm µm µm µm µm µm 08A 09A 10A 10B 11A 11B 12A 13A 14A 15A 1/12/2010 9:20 194 43.0 30.7 11.1 3.25 2.70 2.32 1.68 4.07 3.03 2.32 1.13 15.3 23 6.70 4.40 348 1/12/2010 10:16 189 43.0 30.7 11.1 3.28 2.72 2.34 1.70 4.13 3.08 2.36 1.15 16.7 23 6.73 4.43 392 1/12/2010 11:30 178 43.0 30.7 11.1 3.21 2.66 2.28 1.65 4.02 3.00 2.29 1.12 18.0 26 6.85 4.55 461 1/12/2010 12:00 191 43.0 30.7 11.1 3.21 2.66 2.29 1.65 3.97 2.96 2.26 1.11 20.2 26 7.21 4.91 520 1/12/2010 15:45 146 43.0 30.7 11.1 4.14 3.35 2.83 1.94 5.98 4.04 3.01 1.44 11.5 30 6.62 4.32 339 1/12/2010 16:08 146 43.0 30.7 11.1 4.17 3.38 2.85 1.98 5.99 4.04 3.01 1.44 12.4 30 6.64 4.34 370 1/12/2010 16:57 148 43.0 30.7 11.1 4.25 3.44 2.90 2.01 6.00 4.06 3.03 1.45 15.8 32 7.02 4.72 503 1/12/2010 17:45 145 43.0 30.7 11.1 4.24 3.43 2.89 1.99 5.98 4.05 3.02 1.45 15.6 34 7.20 4.90 526 2/12/2010 10:40 139 43.0 30.7 11.1 4.30 3.47 2.92 2.00 5.95 4.12 3.10 1.52 13.1 34 7.02 4.72 443 2/12/2010 12:47 141 43.0 30.7 11.1 4.46 3.61 3.05 2.11 6.13 4.20 3.15 1.53 16.3 42 8.22 5.92 682 5284 801 260 32% 5284 799 262 33% 5284 799 271 34% 5283 800 279 35% 4256 801 260 32% 4245 800 260 33% 4189 801 264 33% 4119 800 267 33% 3995 801 260 32% 3851 801 269 34% 370 23 348 415 23 392 486 26 461 545 26 520 369 30 339 399 30 370 535 32 503 559 34 526 477 34 443 724 42 682 760 Steel Ce-TPZ 1.4 6.0 160 52% Stearic Acid 1.34 760 Steel Ce-TPZ 1.4 6.0 154 52% Stearic Acid 1.02 760 Steel Ce-TPZ 1.4 6.0 168 52% Stearic Acid 1.29 760 Steel Ce-TPZ 1.4 6.0 157 52% Stearic Acid 1.28 760 Steel Ce-TPZ 1.4 6.0 163 52% Stearic Acid 1.03 760 Steel Ce-TPZ 1.4 6.0 160 52% Stearic Acid 1.02 760 Steel Ce-TPZ 1.4 6.0 155 52% Stearic Acid 1.04 760 Steel Ce-TPZ 1.4 6.0 156 52% Stearic Acid 1.06 760 Steel Ce-TPZ 1.4 6.0 168 52% Stearic Acid 1.05 760 Steel Ce-TPZ 1.4 6.0 161 52% Stearic Acid 1.04 6.1% 41.5 14.3% 0.46 5.6% 43.2 12.7% 0.52 5.3% 41.5 12.3% 0.61 4.7% 41.6 11.0% 0.68 8.0% 45.6 17.1% 0.46 7.4% 45.6 15.8% 0.50 6.0% 45.5 12.7% 0.67 6.0% 45.3 12.9% 0.70 7.1% 44.4 15.5% 0.59 5.8% 46.0 12.2% 0.90 465 7535 16 8000 475 7525 16 8000 505 7495 15 8000 475 7525 16 8000 615 7385 12 8000 615 7385 12 8000 610 7390 12 8000 620 7380 12 8000 650 7350 11 8000 640 7360 12 8000 25‐January‐2011 Page 5 of 10 CONFIDENTIAL Table 3 OMYACARB‐10 trials – summary of test conditions and results (3) Run Number System Performance Mill GE based on production rate, kWh/t Feed F97, µm Feed F80, µm Feed F50, µm Malvern (wet) product sizing data Insitec online (dry) product sizing data Recirculating load Ratio Production rate, kg/h Gross Power Draw, kW Net Mill Power Draw, kW Recirculating load, kg/h ACX 200 Classifier Parameters Classifier speed, rpm System air flow, m3/h Secondary air flow, m3/h % Secondary Air ACX200 Classifier Mass Balance FEED, kg/h PRODUCT, kg/h RECYCLE, kg/h System Configuration Mill speed, rpm Liner material Media Media size, mm Media S.G. Mill Differential Pressure, mmWG Mill Filling, J% Additive Additive rate vs fresh feed (%w/w) Classifier Efficiency Total Fines Mass Recovery %Passing P97 in Classifier Feed Classifier Efficiency @ P97 Solids/Air Ratio to Classifier, kg/m3 H110 Plant Parameters Feed rate, kg/h Recycle rate, kg/h Nominal Recirculating load Ratio Classifier feed rate, kg/h H‐2011.MIS.02 R0.docx P97, P90, P80, P50, P97, P90, P80, P50, µm µm µm µm µm µm µm µm 16A 16B 17A 17B 18A 18B 19A 20A 2/12/2010 14:05 86 43.0 30.7 11.1 6.75 5.20 4.22 2.66 8.12 5.78 4.47 2.50 7.9 59 7.41 5.11 471 2/12/2010 14:40 84 43.0 30.7 11.1 6.66 5.11 4.15 2.63 7.94 5.65 4.37 2.42 7.7 60 7.33 5.03 461 2/12/2010 15:25 85 43.0 30.7 11.1 7.01 5.41 4.40 2.78 8.03 5.63 4.33 2.36 8.1 69 8.23 5.93 559 2/12/2010 15:40 86 43.0 30.7 11.1 6.94 5.37 4.36 2.76 7.96 5.63 4.35 2.38 8.5 70 8.37 6.07 599 2/12/2010 16:26 63 43.0 30.7 11.1 10.10 7.30 5.72 3.36 10.60 7.25 5.51 3.01 6.2 79 7.27 4.97 492 2/12/2010 16:45 63 43.0 30.7 11.1 10.48 7.52 5.90 3.50 10.70 7.29 5.52 3.00 6.0 79 7.30 5.00 479 3/12/2010 11:15 67 43.0 30.7 11.1 9.75 7.41 5.90 3.53 10.60 7.28 5.54 3.00 5.1 77 7.49 5.19 394 3/12/2010 12:04 74 43.0 30.7 11.1 8.88 6.76 5.40 3.28 9.56 6.62 5.03 2.73 6.1 79 8.12 5.82 481 2668 800 272 34% 2675 799 270 34% 2670 800 273 34% 2640 799 272 34% 2225 801 268 33% 2241 800 267 33% 2190 799 266 33% 2387 800 269 34% 530 59 471 520 60 461 628 69 559 669 70 599 570 79 492 558 79 479 471 77 394 560 79 481 760 Steel Ce-TPZ 1.4 6.0 171 52% Stearic Acid 1.08 760 Steel Ce-TPZ 1.4 6.0 173 52% Stearic Acid 1.08 760 Steel Ce-TPZ 1.4 6.0 172 52% Stearic Acid 1.04 760 Steel Ce-TPZ 1.4 6.0 171 52% Stearic Acid 1.03 760 Steel Ce-TPZ 1.4 6.0 172 52% Stearic Acid 1.05 760 Steel Ce-TPZ 1.4 6.0 173 52% Stearic Acid 1.04 760 Steel Ce-TPZ 1.4 6.0 181 52% Stearic Acid 0.84 760 Steel Ce-TPZ 1.4 6.0 179 52% Stearic Acid 0.82 11.2% 49.5 21.9% 0.66 11.4% 48.7 22.8% 0.65 11.0% 52.4 20.4% 0.78 10.5% 51.7 19.7% 0.84 13.8% 65.0 20.6% 0.71 14.2% 66.1 20.8% 0.70 16.4% 62.4 25.5% 0.59 14.1% 61.9 22.1% 0.70 1045 6955 7 8000 1065 6935 7 8000 1055 6945 7 8000 1045 6955 7 8000 1425 6575 5 8000 1425 6575 5 8000 1335 6665 5 8000 1225 6775 6 8000 25‐January‐2011 Page 6 of 10 CONFIDENTIAL Differences between Malvern and Insitec (dry, on‐line) particles size analyses were similar to those reported previously. Only Malvern data is discussed here. It can be seen a reasonably wide range of product sizes was canvassed in this test series. In addition, different coating levels for stearic acid were evaluated to provide samples for evaluation. In general, there was little evidence that variations in coating level between 0.8% and 1.3% had any effect on plant performance or production capacity. 2.3 Product size versus specific grinding energy All of the P97 versus grinding energy test data is shown in Figure 2. Most of the data lies on the same straight line indicating the plant was operated at close to optimum conditions for most of the trials. This was not unexpected as the process was pre‐optimised on the Nordkalk Parfill 7 material. Coated Grinding Aid Only (DEG) P97 - Malvern Sizing (µm) 10 1 10 100 1000 Specific Grinding Energy (kWh/t) Figure 2 Product size as a function of specific grinding energy – all data The reduction in grinding energy obtained when using grinding aid only is also similar to that observed with the Nordkalk test series. Indeed, general experience with calcium carbonate processing in the Hicom mill is that grinding energy is increased by 20‐30% when simultaneous grinding and coating, as compared to optimized processing with grinding aid only. 2.3.1 Comparison with Nordkalk data The comparison shown Figure 2Figure 3 indicates the OMYACARB‐10 and Nordkalk Parfill materials exhibit very similar grindability in the Hicom mill. It might be argued that the Nordkalk material was H‐2011.MIS.02 R0.docx 25‐January‐2011 Page 7 of 10 CONFIDENTIAL slightly more refractory at the fine end of the spectrum studied – say below five µm – but the differences are fairly marginal. OMYACARB-10 DATA NORDKALK DATA P97 - Malvern Sizing (µm) 10 1 50 500 Specific Grinding Energy (kWh/t) Figure 3 P97 versus grinding energy: present data compared with Nordkalk results 2.4 Hicom 110 production capacity The production rate estimates shown in Figure 4 are consistent with those previously reported for the Nordkalk trials. Given the consistency of the present data set, and the similarity in grindability between the respective test materials, the straight line correlation shown Figure 4 is probably the more reliable predictor of expected Hicom 110 kW mill performance on simultaneous grinding and coating of a ‘typical’ calcium carbonate. The ca. 25% difference in mill productivity between coated and grinding aid only operation is also evident in Figure 4, reflecting the differences in specific grinding energy mentioned earlier. Finally, it is hoped the data presented here and in the previous report, together with samples of coated materials provided to respective parties, will provide sufficient information for economic assessment of the use of Hicom mills in this application. H‐2011.MIS.02 R0.docx 25‐January‐2011 Page 8 of 10 CONFIDENTIAL Coated Grinding Aid only 1600 Estimated H110 Mill Capacity (kg/h) 1400 1200 1000 800 600 400 200 0 0 2 4 6 8 10 12 P97 - Malvern Sizing (µm) Figure 4 Estimated Hicom 110 kW mill production rate as a function of product size H‐2011.MIS.02 R0.docx 25‐January‐2011 Page 9 of 10 CONFIDENTIAL DISCLAIMER 1. In conducting equipment testing, careful regard is given to the customer’s requirements. However, operating conditions and materials used in testing cannot be guaranteed to replicate all operating materials or conditions in actual industrial use. 2. The results shown in this test report may differ with different materials or in different environmental or operating conditions. Hicom is not liable to you or any other person in relation to any failure to duplicate the results in this test report. 3. Hicom warrants only that: • It has taken reasonable care in the conduct of tests and the preparation of this report; and • The test results in this report reflect the test results achieved. 4. Hicom does not make, and will not be liable for any other representations or warranties, expressed or implied. 5. This report is provided subject to confidentiality, only for the information of the party to whom it is addressed and solely for the purpose of that party assessing Hicom’s equipment. Hicom accepts no responsibility for any reliance placed on this report by any other party. H‐2011.MIS.02 R0.docx 25‐January‐2011 Page 10 of 10