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By H. S. Choi, I. Iwasaki

The effect of temperature as a parameter in ore flotation has not been systematically studied, although for some ores it has been known for many years that selectivity and grade of concentrates can be improved by conditioning or flotation at moderately or substantially elevated temperatures. In 1934 Coghill and Clemmer' stated that "elevated temperature seems to make hard water more tolerable" in soap flotation, and a cursory examination of the literature indicates that some earlier investigators were aware of beneficial results obtained by floating above room or mill-water temperatures. Tartaron,2 Mitchell et aL.,3 and particularly Hamilton et al.' have shown that high pulp temperatures give high recovery and selectivity in soap flotation of fluorite from a variety of gangue minerals. As a result of the work of these and of other investigators, high-temperature flotation has been successfully applied to industrial flotation of fluorite. Falconer" stated: "The use of high temperature conditioning (above 35°C and preferably above 60°C) in connection with the soap flotation of nonsulphide ores, as covered in B. Kalinowski's French Patent No. 847,-215, Dec. 7, 1938, is claimed to provide more intense activation, better separation of values from gangue, and reduction in quantity of reagents." The various investigations quoted above clearly demonstrate the improvements to be realized by increasing the temperature at which fluorite is floated, and it is surprising that little or no information has been published on systematic investigation of the same method as applied to other ores. The present article describes comparative results obtained at room temperature and at elevated temperatures by otherwise conventional flotation of iron ores, by single-mineral flotation in the Hallimond tube, and by contact-angle measurements. It is not the purpose of this article to evaluate the commercial feasibility of high-temperature flotation of iron ores, although preliminary calculations show that the cost should not be excessive and that the gains to be realized may well outweigh the extra cost of heating the pulp. LABORATORY FLOTATION TESTS Experimental: All flotation tests reported in this article that use a laboratory Fagergren cell were made on ore A (either containing the primary slimes or deslimed at 20µ as specified) following the preparatory procedures described elsewhere- or this particular ore. Ore A contained hematite, goethite (limonite), quartz, chert, and minor quantities of magnetite. Confirmatory tests made on other ores show that the same general principles apply to ores of similar mineralogy and structure. Conditioning was performed by adding the collector, as a soap, to the vigorously stirred and heated pulp. Conditioning time was 5 min, the pulp contained 60 pct solids, and the equivalent of 0.5 Ib of fatty acid was added per ton of original (unde-slimed) ore. The pH of the pulps ranged from 6.8 to 7.1 (25°C measurement) during conditioning. The pH was adjusted in the flotation cell by addition of either NaOH or H2SO4, the values reported being those of the pulp cooled to 25°C. During conditioning and flotation the pulp temperatures were controlled within l° to 2° by immersion of Variac-controlled Calrod elements in the conditioning beaker and in the cell, and by the use of water, heated to the appropriate temperature, for transferring pulp, adjusting pulp volume, and washing. Selectivity indexes have been calculated on the same basis as those reported in the article by Cooke, Iwasaki, and Choi." Results: Table I gives the results obtained by floating deslimed ore A with pure oleic acid at 25" and 50°C, and Fig. 1 shows the selectivity indexes plotted against pH of flotation. Inspection of Table I

Jan 1, 1961

By Brahm Prakash, R. Schuhmann

Chemical conditions for flotation and nonflotation of cassiterite and fluorite with oleic acid as collector and with alizarin dyes as modifying agents were studied by means of small-scale, vacuum-flotation tests. Artificial cassiterite was prepared fot these tests by high-temperature methods, especially by crystallization from borax melts. FLOTATION test work on Bolivian tin ores some years ago led to the development of several workable schemes of selective soap flotation, but left unanswered many questions of soap-flotation chemistry.' Accordingly, the study of the activation and soap flotation of quartz just reported? was undertaken as a start toward the elucidation of some of the unanswered questions. The experimental work on quartz flotation consisted primarily of small-scale, vacuum-flotation tests in which activator and collector additions and pH were varied between wide limits. In the work to be described in this paper, the soap flotation of cassiterite and fluorite was studied by the vacuum-flotation technique developed in the previous study of quartz. Using oleic acid as collector, conditions for floating cassiterite and fluorite in the absence of modifying agents were first determined. Then the effects of barium, calcium, and alizarin dyes on the flotation of cassiterite, fluorite, and quartz were studied. Alizarin dyes were chosen for study because of the promise they have shown as selective modifying agents in the flotation of non-sulphide minerals.12,1 Also, they form a family of reagents in which there should be a systematic correlation of chemical properties with composition. As a preliminary to the study of cassiterite flotation, an investigation of the preparation of synthetic cassiterite and X ray studies of natural and synthetic cassiterite were undertaken. Experimental Methods The flotation technique and most of the reagent preparations were described fully in the previous paper.' In addition, for the present work it was necessary to prepare satisfactory stocks of clean cassiterite and fluorite and to obtain samples of alizarin dyes. Cassiterite: High-grade cassiterite from the Netherlands East Indies was crushed, sized, and cleaned

Jan 1, 1951

By Brahm Prakash, R. Schuhmann

Chemical conditions for flotation and nonflotation of cassiterite and fluorite with oleic acid as collector and with alizarin dyes as modifying agents were studied by means of small-scale, vacuum-flotation tests. Artificial cassiterite was prepared fot these tests by high-temperature methods, especially by crystallization from borax melts. FLOTATION test work on Bolivian tin ores some years ago led to the development of several workable schemes of selective soap flotation, but left unanswered many questions of soap-flotation chemistry.' Accordingly, the study of the activation and soap flotation of quartz just reported? was undertaken as a start toward the elucidation of some of the unanswered questions. The experimental work on quartz flotation consisted primarily of small-scale, vacuum-flotation tests in which activator and collector additions and pH were varied between wide limits. In the work to be described in this paper, the soap flotation of cassiterite and fluorite was studied by the vacuum-flotation technique developed in the previous study of quartz. Using oleic acid as collector, conditions for floating cassiterite and fluorite in the absence of modifying agents were first determined. Then the effects of barium, calcium, and alizarin dyes on the flotation of cassiterite, fluorite, and quartz were studied. Alizarin dyes were chosen for study because of the promise they have shown as selective modifying agents in the flotation of non-sulphide minerals.12,1 Also, they form a family of reagents in which there should be a systematic correlation of chemical properties with composition. As a preliminary to the study of cassiterite flotation, an investigation of the preparation of synthetic cassiterite and X ray studies of natural and synthetic cassiterite were undertaken. Experimental Methods The flotation technique and most of the reagent preparations were described fully in the previous paper.' In addition, for the present work it was necessary to prepare satisfactory stocks of clean cassiterite and fluorite and to obtain samples of alizarin dyes. Cassiterite: High-grade cassiterite from the Netherlands East Indies was crushed, sized, and cleaned

Jan 1, 1951

By Brahm Prakash, R. Schuhmann

Maurice Rey—It may be interesting to note that depressing effects can also be obtained from cyclic compounds other than dyes. One such compound which is a dispersing agent for carbon, pigments and other compounds is known in France by the trade name "dispergine" and in the United States by the name of Lomar P W (Jacques Wolf & Co.) Dr. Rey admits that the compound is not very selective and is similar in its action to starch and dextrin.

Jan 1, 1951

By Brahm Prakash, R. Schuhmann

Maurice Rey—It may be interesting to note that depressing effects can also be obtained from cyclic compounds other than dyes. One such compound which is a dispersing agent for carbon, pigments and other compounds is known in France by the trade name "dispergine" and in the United States by the name of Lomar P W (Jacques Wolf & Co.) Dr. Rey admits that the compound is not very selective and is similar in its action to starch and dextrin.

Jan 1, 1951

By J. F. Myers, F. M. Lewis

The purpose of the mill tests reported herein, was to determine the relative power efficiency of fast and slow rod mill speeds on the ores of the Tennessee Copper Co. The tests were carried out at the Isabella Mill of the Tennessee Copper Co. under normal operating conditions. Every effort was made to keep the ore supply and other conditions constant, but it will be noted that some slight variation did occur. The open circuit 6 by 9 rod mill, and ore, used in these tests have been previously described.' Four motor drive pinions were available and the tests were performed in the following manner: each pinion was used to drive the mill for a period of one week. Constant sampling prevailed during the test run, and a composite sample for each speed test was made. Realizing that some slight liner wear took place during the four-week test-run, and that some slight variation of the ore may have taken place, a second and then a third series of four-week test-runs were made with the four different pinions. The screen analysis of each of the three-week run samples at the various speeds were composited and the results are shown in Table 2. The authors feel that the 22 weeks of operation consumed during these test-runs would represent fairly the effect of each mil1 speed. The data of line 37 show that within the error of sampling and plant operation, the tons of minus 65-mesh material generated per horsepower hour was the same at all four speeds. Obviously, rod and liner consumption could not be determined for each mill speed in so short a time. The rod load was maintained at a uniform level throughout the series of tests. The authors have operated rod mills at various speeds over the past several years, and it is their observation that rod consumption is directly proportional to the mill speed. Likewise, that the rod consumption per unit of work performed is a constant, providing that all other operating factors remain the same. It is a well known fact that the efficiency increases in a ball mill as the speed decreases. This is due to lateral segregation of the large and

Jan 1, 1950

By M. Takeda, H. Majima

Pyrite has been subjected to xanthate adsorption experiments in order to determine the nature of adsorption. The identification of adsorbed species by means of IR spectroscopy, as well as UV, shows that the dixanthogen adsorption is undoubtedly predominant on pyrite surface. The rest potential measured in a xanthate solution coincides with the redox potential of the xanthate-dixanthogen couple. Considering all the factors together, the adsorption mechanism of dixanthogen on pyrite has been proposed as This mechanism is consistent with the "passive" character of pyrite. From the measurement of the redox potential of the xanthate-dixanthogen couple in the homologous series, a rule similar to that for surface tensions proposed by Traube is also applicable. The polarization experiments were conducted on pyrite in a solution containing xanthate. In the anodic polarization, xanthate is observed to oxidize to dix- anthogen, which depresses oxygen evolution on py rite at higher potential levels. In spite of the importance of the presence of pyrite in the flotation of sulfide minerals, not many studies have been made on the xanthate-pyrite system in the absence of an activator or a depressant. In an early study by Gaudin and Wilkinson,' it was pointed out that no ferric xanthate was formed on a pyrite surface, while in another study Gaudin and his collaborators2 proved the formation of a very small amount of ferric xanthate. Afterwards, Gaudin et al.3 studied the pyrite-xanthate system with a radiometric technique and found indications of the presence of adsorbed dixanthogen on pyrite surfaces. Mamiya4 studied the flotation behavior of the pyrite-xanthate system and also suggested the possibility of dixanthogen. Recently, Fuerstenau and his coworkers at The Colorado School of Mines5 studied the role of dixanthogen in the xanthate flotation of pyrite and discussed the problem in terms of such properties as oxidation potential, zeta potential, flotation recovery, pH of solution, etc. However, the mechanism of dixanthogen adsorption at the pyrite-water interface is not yet understood. This paper is concerned with an electrochemical in-vestigation through which the mechanism of dixanthogen adsorption on pyrite is interpreted. EXPERIMENTAL MATERIALS AND TECHNIQUES Pure potassium xanthates were synthesized by an

Jan 1, 1969

By W. Mitchell, B. H. Bergstorm, C. L. Sollenberger

A unique compression testing machine was constructed to load individual 1/8 to I-in. spheres of glass, etc., at rates from 100 to 100,000 lb per min. During loading the applied load was continuously plotted us the deformation of the sphere-platen system. The load-deformation curve conforms to the theory of elasticity. The spheres were surrounded by steel retaining rings or by gelatin (to prevent secondary fracture). The product size modulus was determined from screen analyses. The data shows: 1) Energy input per unit mass is inversely proportional to the product size modulus (or directly proportional to the surface area per unit mass). 2) Increased loading rates slightly increase the energy input per unit mass required for fracture without affecting the preceding relationship. Theory and experiments show that much of the input strain energy is transformed into kinetic energy of fragments at fracture, this being a reason efficiencies based on "surface energies" are exceedingly small. This large kinetic energy component is usually dissipated as heat but may be partially reclaimed because impact of fragments against the surface of steel retaining rings causes additional comminution. There are currently several theories of crushing, all of which can be derived from the general energy equation of Gillilandl as was pointed out by Mitchellet al in 1954'and more recently by Rose and Sullivan. If the exponent of the equation dE-x-"dx is assigned values of 2,1, or 3/2, one obtains by intergration between suitable limits, the equations of Rittinger, kick,' and Bond,' respectively. Other investigators prefer to let the exponent be a variable parameter. To help resolve the controversy, the Allis-Chal-mers Research Laboratories set up a series of carefully controlled experiments in which the level of energy input required to induce the comminution of a single particle by slow compression loading was very accurately measured. The energy input requirement, in conjunction with the size analysis of the fragments produced at fracture, yielded an accurate energy-product size relationship for the conditions studied. APPARATUS The experimental apparatus was designed to apply a compressive load on opposite sides of an "ideal particle." Spherical shapes were chosen, because point contact loading is typical of the mechanics of conventional crushers. The bulk of the experimental data was obtained with glass spheres because glass is a fairly homogeneous, brittle material for which the properties follow definite statistical distributions. The spheres ranged from 1/8 to 1-in. diam. The compressive load was applied to the specimen at a uniform rate by a loading mechanism (Fig. 1) which acted through a system of levers. The uniform rates, ranging from 100 to 100,000 lb per min, were obtained by metering water into a bucket suspended at the end of the secondary level. Point contact was made with the sphere through tungsten-carbide platens. This latter material is extremely hard and has a high modulus of elasticity, thereby having a minimum of distortion when loaded. The actual load on the sphere was measured independently of the lever system by a load cell, Fig. 2, which was designed so that the voltage output of the load cell would be proportional to load. The deformation of the specimen was indirectly measured by a pair of transformers which were attached to opposite edges of the upper platen. The cores of the transformers, which were attached to the lower platen, moved relative to the transformer so that the voltage output was proportional to the deformation of the sphere-platen system. The load was plotted against the deformation on an X-Y recorder. The area under the curve, as shown on Fig. 3, was proportional to the energy input of the

Jan 1, 1961

By I. C. Edwards, G. E. Agar

INTRODUCTION Many research efforts over the past years have been devoted to the study of energy consumption in comminution and the characteristics of the broken material. The old "laws" have been superseded by more general methods of analysis1,2,3 but these methods have not received much attention outside the laboratory. The work to be described here was done in order to obtain scale-up information on wet rod milling of sylvinite. EXPERIMENTAL A 30 x 51 in. Denver rod mill with a scoop feeder was used for these tests. Ore was fed from a variable speed screw conveyor into the feed box along with saturated brine. The mill was filled to approximately 45% of its volume with 2400 lbs of a mixed rod charge. The minimum possible feed rate was 2.5 tph and the practical maximum for this mill was 8 tph. Individual tests were run by setting the solid feed rate, then adjusting the brine flow rate to give the desired pulp density. After steady state, as evidenced by constant discharge pulp density, had been reached, samples of the discharge were taken at 15-minute intervals. These samples were filtered, washed with alcohol, dried, then screened on Tyler screens using a Ro-tap shaker. The sylvinite feed was regular plant feed that had been scalped at 20 mesh and was tapped from the coarse ore bins. It had been previously passed through a roll crusher set at 3 inches and after scalping was essentially minus 1 in. plus 20 mesh. RESULTS The screen analysis of samples from each series of tests was plotted on double logarithmic scale paper to determine the reliability of the series. In some cases, a faulty sample or screening procedure dictated that the results of one test be discarded. The criterion is a simple one — if the slope of one plot was noticeably different from the others in the series, it was discarded. The only cases that caused difficulty were those in which the brine was not thoroughly displaced from the solids. When this occurred agglomerates were easily identified on the screens and the whole of the sample was retained on 3 or 4 screens. There were no border line cases. The number N given in Table 1 is the number of size analyses that were pooled to form the data shown in Fig. 1. While examining the reliability of the sizing and sampling by plotting the data, it became apparent that there was no significant difference between grinds made at 50 and 60% solids. For the analysis given here, these tests were regarded

Jan 1, 1967

By P. L. De Bruyn, R. J. Charles

THE transfer of kinetic energy of translation into other forms of energy by impact is a fundamental process in most crushing and grinding operations. During and after the impact process the original source energy may be accounted for in any of the following possible forms: 1) Kinetic energy of translation of both the impacted and impacting objects. 2) Kinetic energy of vibration of the components of the impact system. 3) Potential energy as strain energy of the components of the system or in the form of residual stresses. 4) Heat generated by internal friction during plastic deformation or during damping of elastic waves. 5) New surface energy of fractured materials. At any instant during the impact process only the strain energy of the components of the system can contribute directly to the brittle fracture process. If fracture is the desired result, as in comminution, it would seem advantageous to choose or arrange the conditions of impact so that a maximum amount of the original kinetic energy could be converted to strain energy at some moment during a single impact. The present work deals with determination of these desirable conditions for a simple case of impact and application of the principles involved to general cases of impact. Experimental Method: Longitudinal impact of a rod with a fixed end was chosen as the impact system for investigation. The rod was mounted horizontally and the fixed end was formed by butting one end of the rod against a rigidly mounted steel anvil. The rod, of pyrex glass, was 10 in. long by 1 in. diam with both ends rounded to a 6 in. radius. The rounded ends permitted reproducible impacts on the free end of the rod and assured a symmetrical fixed end. Pyrex was selected as the rod material because of the marked elastic properties of such glass and the similarity of fracture between pyrex and many materials encountered in crushing and grinding operations. The frequency of natural longitudinal oscillation of the rod was 10 kc, and thus simple electronic equipment could be used for observation of strain changes occurring in the rod at this frequency. As shown in Fig. 1, impacts on the free end of the rod were obtained either by a pendulum device or by a spring-loaded gun. Relatively heavy hammers (100 to 600 g) of mild steel were used in the pendu- lum impacts, while fairly light projectiles (20 to 80 g) were fired from the spring-loaded gun. One of the main objects of the experimental work was to obtain the strain-time history of the rod as a function of the mass and kinetic energy of the impacting hammers. For this purpose a technique involving wire resistance strain gages and a recording oscilloscope was employed. Five gages were applied at equidistant sections along the rod, and by means of a switching arrangement the strain-time history at any section, and for any impact, could be obtained in the form of an oscillograph with a time base. The equation relating strain and voltage change across a strain gage through which a constant current is flowing is as follows: e = ?v/iRF [1] ? = strain, ?v = voltage change, i = gage current, R = gage resistance, and F = gage factor (from manufacturer's data — SRA type, Baldwin Lima Corp.). With the above equation an oscillograph depicting voltage change vs time on a single trace can be converted directly to a strain-time diagram if a calibration of the vertical response on the oscilloscope screen for specific voltage inputs is available. In the present case the calibration was obtained by photographing precisely known audio frequency voltages on the same oscillograph as that on which a voltage-time trace from a strain gage had been made. Synchronization of the beginning of the single trace with the beginning of the impact was accomplished by permitting contact of the impacting objects to close an electrical circuit from which a voltage pulse, sufficient to initiate the trace, was obtained. The struck end of the rod was lightly silvered for purposes of electrical conduction so that it would form one of the electrical contacts. Markers every 100 micro-seconds on the traces served for a time base calibration. Determinations of the kinetic energies of translation prior to impact were made in the case of the pendulum hammers by measuring the height of fall of the hammer and in the case of the projectiles by measuring the exit velocity from the gun barrel by means of an electrical circuit employing light sources, slits, and phototubes.' During the experimental work it became evident that the time of contact between the impacting object and the rod was an important variable in the impact process. Measurements of the times of contact were made, therefore, for every impact for which a strain-time record was obtained. The time of contact was determined by permitting the impacting components, when in contact, to act as a closed switch and discharge a condenser at relatively constant voltage. The discharge was observed and photographed with a time base on the oscilloscope screen.

Jan 1, 1957

By J. Leja, A. Pomianowski

This paper deals with equimolar solutions of xanthate and alkyl trimethyl ammonium bromide adsorption on copper, nickel and sphalerite powders. After an exposition of the experimental methods used and the results obtained, a thorough discussion leads to the conclusion that some molecular association between xanthates and CnTAB's does take place in the bulk of the solution as well as at the air/liquid interface. A spectrophotometric study of xanthate solutions alone and their mixtures with equimolar amounts of alkyl trimethyl ammonium bromide (CnTAB) has established the additivity of ultraviolet spectra (190 to 400 mµ) for potassium ethyl xanthate (KEtX) and C12TAB. No obvious effect of C12TAB addition on the decomposition rate of KEtX was observed, the half life of which was established as 29±3 days at 22°C and pH ~ 6. In mixed solutions of longer xanthate homologues (e.g. hexyl and nonyl) and equimolar CnTAB, colloidal precipitates are gradually formed which contain primarily the corresponding xanthate molecules. The kinetics of collector abstraction by copper, nickel and sphalerite powders were studied in 10-5 to 10"3 M solutions of KEtX alone and in equimolar mixtures of KEtX and CI2TAB. Presence of C12TAB caused a two to three fold increase in the amounts of xanthate (equivalent to many monolayers) abstracted by copper and nickel powders (and in their rates of abstraction) but had no effect on the abstraction of xanthate by unactivated sphalerite (equivalent to less than a monolayer). The adsorption of C12TAB itself from the mixed solutions was very low, at most one monolayer only, and was not influenced by the nature of the solid powder used. A change in the rates of abstraction, observed with copper powder, was interpreted as a completion of a multilayer coating (completely enveloping the grains of powder) following which the rate of reaction between solution and substrate becomes controlled by diffusion through this coating. Work of Buckenham and Schulmanl on molecular associations between different collectors has shown unusual synergistic effects in flotation of individual minerals using mixtures of xanthates and alkyl trimethyl ammonium bromides. The objectives of the present work were: 1) to determine whether these molecular associations between the two types of collectors (indicated by strong surface tension lowering in Buckenham and Schulman's work) take place at the air/liquid interface only or in the bulk of solution as well 2) to establish whether different solids adsorb any species from the mixture of these amphipatic molecules preferentially or as molecular complexes 3) to establish whether there are any differences in the kinetics of adsorption. Metallic copper and sphalerite powder were chosen as adsorbents since they represent two extremes since copper readily adsorbs multilayers of xanthate (and is easily floated with ethyl xanthate) while unactivated sphalerite does not appreciably adsorb xanthate but is known to be readily floated by the amine type collectors. Metallic nickel was included because the infrared spectroscopic work2 on xanthate

Jan 1, 1964

By A. Sutulov

The segregation process, an alternative to benefi-ciation of oxidized and mixed sulfide-oxide copper ores, is studied here with particular emphasis placed on time, temperature, and coke and salt percentage factors. The results show that in a segregated charge, the copper assay of the coarsest fractions normally is of the same order as the copper assay of the tails obtained from grinding and flotation of the same charge. This observation suggests the possibility of limiting or even eliminating the grinding step from the flowsheet of a segregation plant. The segregation process, which offers an alternative to beneficiation of oxidized and mixed sulfide-oxide copper ores, was discovered in 1923 by Moulden and Taplin1,2 who were attempting to apply the Perkins process3'4 to a Chilean ore from the Sagasca mine. After a number of investigations and pilot plant tests,'-' the segregation process became a successful industrial operation.'r9 The process aroused considerable interest in Chile because of the existance of large reserves of oxidized copper minerals which could not be treated by conventional hydrometallurgical methods because of the high consumption and prohibitive cost of sulfuric acid. During the last two years, the Mineral Dressing Dept. of the Institute de Investigaciones Tecnology cas of University of concepci6n (Chile) has carried out a test program on 23 different ore samples representative of the national territory. These tests were carried out on a semi-continuous and batch scale with a rotary, automatically controlled and gas-fired furnace (supplied by Bartlett and Snow, Fig. 1). The results of these tests indicate that out of the 23 samples 20 can be successfully treated by this process with recoveries of copper ranging from 85 to 95%.10,11 The purpose of this paper is to treat some specific problems related to the segregation process. TIME AND TEMPERATURE FACTORS Time and temperature of calcination play an important role in the segregation process. When moderate salt and coke conditions were maintained (each of reagents was added in the quantity of 1 — % wt), systematic testing easily demonstrated the influence of these two factors on segregation and flotation recovery. The pertinent results are summarized in Fig. 2. To determine what specific changes the segregation process made on the ore, the samples, segregated at 700°C for different periods of time and under standard conditions, were granulometrically analysed and

Jan 1, 1963

By F. Petkovich, M. P. Sudbury

Development of a new method of treating flotation concentrates for the preparation of feed suitable for direct charging to blast furnaces or converters is described. The method takes advantage of the fact that pyrrhotite contained in the concentrates can be made to undergo exothermic reactions which, under properly controlled conditions, result information of oxidation products that serve to cement the concentrate particles together. Thus green concentrates either in the form of pellets or briquettes containing 5 to 8 pct moisture not only were hardened, but also completely dried autogenously by continuous countercu,vrent shaft treatment with air. The process was developed through pilot plant operations ranging from 35 1b per hr to 2.5 tph, culminating in products evaluation tests on a railway-car scale. Falconbridge Nickel Mines Ltd., Falconbridge, Ont., have practised sintering, on a travelling grate machine, for many years to prepare a pyr-rhotite-bearing Cu-Ni sulfide flotation concentrate for blast furnace smelting. In recent years the development of new mines, and the construction of concentration plants some 40 miles from the smelter has increased the quantity of concentrate shipped, and encouraged the search for a method of producing dry, hard pellets or briquettes suitable for direct charging to a blast furnace or converter, and capable of withstanding considerable handling. The cementing properties of pyrrhotite oxidation products were discovered during a search for a suitable agglomeration method for sulfide concentrates, and were exploited in a process subsequently developed for autogenously drying and hardening pellets and briquettes of pyrrhotite-bearing Cu-Ni sulfide flotation concentrate. EARLY TEST WORK The production of hard, dry pellets of concentrate filter cake was attempted in the drying plant of one of the new concentrators. While soft pellets were produced containing 5 pct moisture, attempts at further drying resulted in disintegration of the pellets and intolerable dusting. The plant therefore was controlled to produce a concentrate containing about 6 pct moisture. The partially dried concentrate, which was shipped to Falconbridge for sintering, tended to heat spontaneously in transit. An at- tempt to briquette the moist concentrate at Falconbridge, in a plant incorporating a muller, a 20-in. roll briquetting press, and a steam-heated travelling grate oven, was more successful, although the equipment corroded rapidly due to the acid nature of the concentrate after spontaneous heating had occurred. LABORATORY STUDIES OF SPONTANEOUS HEATING OF CONCENTRATE The spontaneous heating of partially dried concentrate was studied in the laboratory. Moist concen-

Jan 1, 1961

By Z. F. Oszter

This paper discusses the materials handling problems encountered in cement plants in the areas of raw and finished product grinding and cement storage. It illustrates by examples taken from actual installations, how optimum feed rate is maintained in grinding circuits with properly applied bin dischargers (vibrating hoppers, Mexican feed boxes and aerated bin bottoms) for materials with high moisture content and/or difficult handling characteristics. Initial operating problems with the equipment will be discussed and maintenance requirements will be indicated for comparison purposes. In a modern cement plant, properly functioning bins and feeders are as essential as process control, for no process control system, however sophisticated, can perform efficiently if raw materials do not flow into the plant processing facilities at the required time and rate. Most materials used in the manufacture of portland cement - such as silica sand, iron ore fines, crushed limestone, gypsum, clinker or cement itself-have difficult handling characteristics under specific conditions. High moisture content or even dampness due to condensation may create bin hang-ups, arching and ratholing, all of which result in improper functioning of the feeders or proportioning equipment. The occurrence of these problems in existing cement plants spurred a search for the corrective devices discussed in this article. The equipment investigated included bin dischargers in the form of vibrating hoppers for moist raw materials, Mexican feed boxes for clinker and aerated bin bottoms for cement. Operating experience with different types of bin dischargers showed that the actual performance of some did not come up to the expected level under prevailing operating conditions. The aim of this paper is to record the results of this experience and there- by aid designers and/or operators in selecting the most suitable equipment for their requirements. BIN DISCHARGERS (GENERAL) A discharger is a device that causes stored solids to flow out of a hopper without metering the rate of flow as a feeder does. The investigation discussed here encompasses the following types of bin dischargers used in a cement plant: (1) vibrating hoppers (horizontal motion), (2) whirlpool hoppers (horizontal and vertical motion), (3) aerated bin bottoms (air fluidization), and (4) Mexican feed boxes. Most of the bins used in the cement industry are of the plug flow type. Raw materials with difficult handling characteristics such as high moisture content may cause flow problems when fed through small openings (12 x 18 in.), even if two walls of the bin are vertical.' The most appropriate solution to these flow problems would be the installation of separate mass flow bins for the different materials such as silica sand, iron ore fines, crushed limestone and gypsum, with each bin correctly designed from test data obtained by measuring the flow properties of representative samples. However, limited storage capacity and plant space usually preclude this approach. Quantitative design of bins for flow based on measured flow properties of representative samples of the bulk solid to be handled is no longer an "engineering art," thanks to the basic research done on the flow of bulk solids in bins during the last decade.2, Where space limitations exist, however, or where improvements are being sought for equipment already installed, bin dischargers offer a satisfactory solution to flow problems. They can be applied effectively under flat-bottom bins or mounted to existing plug-flow bins with very little modification to these facilities. In both the foregoing cases, plug flow will be maintained, but the flow channel will be considerably increased so that it is larger than the discharger's bin-side diameter, and material flow can be sustained if the discharger is correctly selected. The main purpose of a bin discharger is to draw the bulk solids across the whole area of the bin outlet, to make the opening fully effective. As long as the bin-side opening of the discharger is large enough

Jan 1, 1969

By James J. Bean

HE task of measuring the specific gravity of the -*- operating medium in a heavy-media separation system has never presented a particularly difficult problem because the medium is fairly stable and the overflow of the separatory vessel, as well as its underflow, can be sampled easily and accurately and the specific gravity of the suspension determined easily by weighing a known volume. However, while this method is simple and accurate it does require the operator to take the sample by hand and to weigh it and there is considerable temptation to avoid the periodic sampling if everything seems to be going well, or if something is occupying the attention of the operator. Furthermore all operators do not sample in exactly the same manner and considerable practice is required for two operators to be able to "check" each other to the last few hundredths, particularly if the sample is cut underneath the drainage screen where location of the point of sampling and load on the screens tends to influence the determination. While none of the above presents much of a problem, we have all recognized that some mechanical method of continuous measurement and recording would be advantageous since the operator would merely have to glance at the meter to check the gravity and to have an indication of the trend of any changes. Also if the instrument were of the recording type, a permanent record would be available for the guidance of the superintendent. The Eagle-Picher Mining and Smelting Co. was the first heavy-media user to actually install such a recording meter. In 1946 they installed in their Central Mill at Cardin, Okla., a specific gravity recorder manufactured by the Bristol Co. of Water-bury, Conn. R. A. Barnes, of the Bristol Co., working with E. H. Crabtree, Jr. and Elmer Isern, of Eagle-Picher, made the application and worked out the problems of sampling and measuring. Their attempts to measure the specific gravity of the medium in the cone itself were not entirely successful and they resorted to an outside sample tube for actually making the determination. Because of the particular flowsheet used, it was possible to tap off from the medium return pipeline a stream of medium and divert it into the sampling tube, which was provided with a constant level overflow and a spigot underflow, and into which the bubbler tubes dipped. The Eagle-Picher installation was successful and its possibilities were recognized by the Mineral Dressing Laboratory of the American Cyanamid Co. It was decided to install a similar unit in the heavy-media pilot plant to investigate further its possibilities. Chief among these was the continuous record which it was felt would be proof of the steadiness of the gravity in a heavy-media cone, something which is not always appreciated by POtential users. Because the heavy-media pilot plant is required to operate at a wide range of specific gravities, it was realized that the unit would have to record all gravities from 1.25 to 3.50, and do it to the nearest 0.01. It would not be necessary to record all of this wide range on a single chart and the method selected was to have 4 bands, each band range overlapping the other a small amount and calibrated so that with standard charts one division would represent 0.01 sp gr. A shift from one band to another could be arranged without alteration of the instrument itself, being accomplished by a simple change in the bubble-tube lengths, as described later. Accordingly, a recording type instrument was purchased and installed. Because there were some advantages in doing so, the first installation attempted to measure the gravity of the cone proper by placing the bubble tubes in the cone. This was not at all satisfactory and the second scheme utilized a fixed vertical screen at the surface of the cone, and an external sample-tube arrangement. We were particularly anxious to make this work as we felt it would be advantageous to measure the top level of medium where the separation was actually being made, but we were doomed to disappointment because it was impossible to keep the screen clean of float. Since the top gravity of the cone is the most convenient place to sample for control, a launder about 2 in. wide was installed longitudinally beneath the

Jan 1, 1951

By James J. Bean

HE task of measuring the specific gravity of the -*- operating medium in a heavy-media separation system has never presented a particularly difficult problem because the medium is fairly stable and the overflow of the separatory vessel, as well as its underflow, can be sampled easily and accurately and the specific gravity of the suspension determined easily by weighing a known volume. However, while this method is simple and accurate it does require the operator to take the sample by hand and to weigh it and there is considerable temptation to avoid the periodic sampling if everything seems to be going well, or if something is occupying the attention of the operator. Furthermore all operators do not sample in exactly the same manner and considerable practice is required for two operators to be able to "check" each other to the last few hundredths, particularly if the sample is cut underneath the drainage screen where location of the point of sampling and load on the screens tends to influence the determination. While none of the above presents much of a problem, we have all recognized that some mechanical method of continuous measurement and recording would be advantageous since the operator would merely have to glance at the meter to check the gravity and to have an indication of the trend of any changes. Also if the instrument were of the recording type, a permanent record would be available for the guidance of the superintendent. The Eagle-Picher Mining and Smelting Co. was the first heavy-media user to actually install such a recording meter. In 1946 they installed in their Central Mill at Cardin, Okla., a specific gravity recorder manufactured by the Bristol Co. of Water-bury, Conn. R. A. Barnes, of the Bristol Co., working with E. H. Crabtree, Jr. and Elmer Isern, of Eagle-Picher, made the application and worked out the problems of sampling and measuring. Their attempts to measure the specific gravity of the medium in the cone itself were not entirely successful and they resorted to an outside sample tube for actually making the determination. Because of the particular flowsheet used, it was possible to tap off from the medium return pipeline a stream of medium and divert it into the sampling tube, which was provided with a constant level overflow and a spigot underflow, and into which the bubbler tubes dipped. The Eagle-Picher installation was successful and its possibilities were recognized by the Mineral Dressing Laboratory of the American Cyanamid Co. It was decided to install a similar unit in the heavy-media pilot plant to investigate further its possibilities. Chief among these was the continuous record which it was felt would be proof of the steadiness of the gravity in a heavy-media cone, something which is not always appreciated by POtential users. Because the heavy-media pilot plant is required to operate at a wide range of specific gravities, it was realized that the unit would have to record all gravities from 1.25 to 3.50, and do it to the nearest 0.01. It would not be necessary to record all of this wide range on a single chart and the method selected was to have 4 bands, each band range overlapping the other a small amount and calibrated so that with standard charts one division would represent 0.01 sp gr. A shift from one band to another could be arranged without alteration of the instrument itself, being accomplished by a simple change in the bubble-tube lengths, as described later. Accordingly, a recording type instrument was purchased and installed. Because there were some advantages in doing so, the first installation attempted to measure the gravity of the cone proper by placing the bubble tubes in the cone. This was not at all satisfactory and the second scheme utilized a fixed vertical screen at the surface of the cone, and an external sample-tube arrangement. We were particularly anxious to make this work as we felt it would be advantageous to measure the top level of medium where the separation was actually being made, but we were doomed to disappointment because it was impossible to keep the screen clean of float. Since the top gravity of the cone is the most convenient place to sample for control, a launder about 2 in. wide was installed longitudinally beneath the

Jan 1, 1951

By James J. Bean

F. M. Lewis—I believe that density recorders are a prerequisite to all well operated ore concentrators. Well designed density instruments are very accurate and give an excellent record of the steadiness of the operation. Controlling the density of a pulp with an instrument, as described by Mr. Bean, is new and the experiences in developing this controller at the American Cyanimid Co.'s Mineral Dressing Laboratory are very interesting and should be extremely helpful to others who are planning on designing or installing controlling density instruments. Instruments for recording the density of the classifier overflow or flotation feed are rather common in ore concentrators, but there are a number of profitable uses for these instruments that are not too well known. Density recorders with bubble tubes submerged to different depth in a classifier pool give an excellent record of the classifier operation. The loading and unloading of the machine, that is so easily masked in the density of the overflow, can be easily recorded if the instrument is installed at some depth in the classifier pool. On some occasions, two instruments with bubble tubes at different depths give a more candid picture of the irregularities in the classifier operation. When cleaner machines are operated in closed circuit with roughers, a record of the density of the cleaner tails will indicate the circulating load in the circuit and is very helpful in coordinating different operators, because quite often the circulating load will be increasing for some time before the analyses of the products will change. Density recorders are used to record the variations in the dilution of the underflow from thickening tanks and in at least one plant the instrument controls the underflow.

Jan 1, 1951

By James J. Bean

F. M. Lewis—I believe that density recorders are a prerequisite to all well operated ore concentrators. Well designed density instruments are very accurate and give an excellent record of the steadiness of the operation. Controlling the density of a pulp with an instrument, as described by Mr. Bean, is new and the experiences in developing this controller at the American Cyanimid Co.'s Mineral Dressing Laboratory are very interesting and should be extremely helpful to others who are planning on designing or installing controlling density instruments. Instruments for recording the density of the classifier overflow or flotation feed are rather common in ore concentrators, but there are a number of profitable uses for these instruments that are not too well known. Density recorders with bubble tubes submerged to different depth in a classifier pool give an excellent record of the classifier operation. The loading and unloading of the machine, that is so easily masked in the density of the overflow, can be easily recorded if the instrument is installed at some depth in the classifier pool. On some occasions, two instruments with bubble tubes at different depths give a more candid picture of the irregularities in the classifier operation. When cleaner machines are operated in closed circuit with roughers, a record of the density of the cleaner tails will indicate the circulating load in the circuit and is very helpful in coordinating different operators, because quite often the circulating load will be increasing for some time before the analyses of the products will change. Density recorders are used to record the variations in the dilution of the underflow from thickening tanks and in at least one plant the instrument controls the underflow.

Jan 1, 1951

By D. W. Frommer, M. M. Fine

Mineral dressing research showed that iron concentrates of commercial quality could be produced from the Pea Ridge deposit near Sullivan, Mo. Magnetic separation and flotation, on a laboratory scale, yielded concentrates ranging from 60.0 to 71.4 pet Fe at recoveries of 89.9 to 97.6 pct. Early in 1957 St. Joseph Lead Co. announced discovery of three new centers of iron ore deposition in east central Missouri.' The discovery resulted from exploratory drilling in the vicinity of a magnetic anomaly or high. A deep hole, drilled into the Pre-Cambrian porphyry to determine the cause of anomaly, penetrated a magnetite-rich deposit.' The magnetic surveys that revealed the anomalies were begun by the Missouri Geological Survey in 1929 and were continued into the 1930's.3 At that time an area in Crawford County known as the Bourbon magnetic high was located. A second anomaly, similar in size and intensity, was discovered about six miles to the northeast in Franklin County in the vicinity of Sullivan. This area was not studied in detail until the early 1940's. To determine the cause of the anomalies, the USBM drilled four holes at the Bourbon site in 1943-1944.4 The most productive hole penetrated four mineralized zones having a total thickness of 127.5 ft. These zones contained magnetite in rhyo-lite porphyry at depths between 1600 and 2000 ft. Additional iron ore below 2000 ft was considered a possibility at the time. Some years later, the USGS, Missouri Geological Survey, St. Joseph Lead Co., and others cooperated in sponsoring an aeromagnetic survey of the Bourbon-Sullivan area which resulted in discovery of a third high, about eight miles distant at Pea Ridge. This deposit, with an estimated reserve of 50 to 100 million tons of iron ore, is considered the main find, although other orebodies in the same general area are of definite interest.' When this discovery was announced, St. Joseph Lead also revealed plans to exploit the deposit jointly with Bethlehem Steel Co. A new corporation, Meramec Mining Co., was established, and 1962 was set as the target date for completing physical plant.2 Annual production goals of 2 million tons of beneficiated and pelletized iron ore were proposed. Preparation of the site for shaft sinking was begun in June 1957. Orebody and Character of Samples: Drilling to date has established the Pea Ridge orebody as a crescent-shaped pipe about 300 ft wide. Some drillholes were bottomed at 2800 ft in very good iron ore.6 he orebody is predominantly magnetite, although hematite and a mixture of hematite and magnetite occur in the upper areas and peripheral walls. Drillhole cores representing ore from different areas and depths of mineralization were grouped into composites for testing. These composites consisted of: 1) medium grade mixed hematite and magnetite, 2) high grade mixed hematite and magnetite, and 3) high grade magnetite. The medium grade ore came from three holes with depths of i350 to 1900 ft. The high grade mixed hematite and magnetite cores came from the 1790 to 2812-ft interval of one hole. Partial chemical analyses of the three samples, given in Table 1, reveal that all are excessively high in phosphorus and sulfur, and sample 1 is

Jan 1, 1960

By H. Kahata, I. Iwasaki, Y. Takahasi

A combined process of segregation roasting-flota-tion or magnetic separation was developed to recover nickel from lateritic iron ores and oxidized nickel ores. An ore was mixed with a halide, such as sodium or calcium chloride, and a solid reductant, and roasted, whereby the nickel content was segregated out as discrete metallic particles. Either by magnetic separation, or by flotation using a sulfhydryl collector together with a heavy metal salt as an activator, the metallic nickel could be concentrated, Effects of such variables as the types and amounts of the halide and solid reductant addition and of the roasting conditions were extensively investigated. The concentration results on several types of ores from Japan, the Philippines, and New Caledonia are presented. Laterite is a residual product of rock decay in tropical and subtropical regions, and consists mainly of hydrated oxides of iron and alumina. Those derived from serpentine sometimes become enriched in nickel, cobalt, and chromium contents. Oxidized nickel ores are of the similar origin, but their nickel as well as silica contents are higher due to gamierite-type silicates. Apparently, nickel enrichment is more pronounced in the transition region between the surface layer of iron laterite and the underlying serpentine. Iron laterites often contain over 50% iron, and their reserve is reported to exceed 22 billion tons, corresponding approximately to 20% of the world iron ore reserve.1 It is readily apparent, therefore, why the iron laterites have attracted much attention of the steel industry as a potential source of iron ores. Numerous attempts to remove nickel and chromium as byproducts, have been reported in literature.' Worldwide discoveries of high-grade iron ore deposits in recent years have inevitably lessened the interests in iron laterites. However, in view of the tremendous potential for their gross value and supplies of nickel, cobalt, chromium, and alumina along with iron, the problem remains as a challenge. Much of the chromium in laterites is present in the form of relatively coarse particles of chromite, and various classification methods have successfully been applied for its removal.2,3 The nickel, however, is intimately associated with limonite, and ordinary concentration techniques are totally ineffective. Much attention has, therefore, been given to hydro-metallurgical or pyrometallurgical means. Yet, all the known processes appear to have limitations either economically or for the use of products as iron raw materials due to a high residual content of nickel. Some attempts have been made to pre-roast laterites or oxidized nickel ores, particularly with sulfidizing agents, and to remove nickel either by magnetic separation,' or by flotation.4 It is apparent that any such concentration process would require grain growth of nickel during roasting for effective separation. Oxidized copper ores are reported to be concentrated by the segregation roasting-flotation process,5 in which the ores are roasted with a chloridizing agent and a carbonaceous reductant in order to promote the growth of metallic copper through repeated cycles of copper chloride volatilization and its reduction on the solid reductant surfaces. Examination of a vapor pressure-temperature diagram of various metal chlorides indicates that a separation of nickel from iron may be effected by a similar process. In fact, the segregation roasting of laterites was reported to increase the extraction of nickel by the ammonia leach process, as compared to the ordinary reduction roasting.6 In the present article some of the preliminary experimental results of the segregation roasting, followed by either flotation or magnetic separation, on laterites and oxidized nickel ores are reported. The effects of various parameters in the roasting as well as in the concentration steps are discussed. MATERIALS AND METHODS An oxidized nickel ore from Thio, New Caledonia, and three laterites from Homonhon, the Philippines, Wakasa and Miyagawa, Japan, were selected for the

Jan 1, 1967