WO2012051424A2 - Méthode de traitement de matériaux minéraux contenant de l'ilménite avec une teneur élevée en argile, et produits associés - Google Patents

Méthode de traitement de matériaux minéraux contenant de l'ilménite avec une teneur élevée en argile, et produits associés Download PDF

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WO2012051424A2
WO2012051424A2 PCT/US2011/056164 US2011056164W WO2012051424A2 WO 2012051424 A2 WO2012051424 A2 WO 2012051424A2 US 2011056164 W US2011056164 W US 2011056164W WO 2012051424 A2 WO2012051424 A2 WO 2012051424A2
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Prior art keywords
separation
feed
weight percent
settling velocity
ilmenite
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WO2012051424A9 (fr
WO2012051424A3 (fr
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Martin C. Kuhn
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CIC RESOURCES Inc
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CIC RESOURCES Inc
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/02—Settling tanks with single outlets for the separated liquid
    • B01D21/04—Settling tanks with single outlets for the separated liquid with moving scrapers
    • B01D21/06—Settling tanks with single outlets for the separated liquid with moving scrapers with rotating scrapers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/0087—Settling tanks provided with means for ensuring a special flow pattern, e.g. even inflow or outflow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00—General arrangement of separating plant, e.g. flow sheets
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D21/00—Separation of suspended solid particles from liquids by sedimentation
    • B01D21/0009—Settling tanks making use of electricity or magnetism
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2221/00—Applications of separation devices
    • B01D2221/04—Separation devices for treating liquids from earth drilling, mining
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D3/00—Differential sedimentation

Definitions

  • titanium-containing minerals are by mining of sedimentary sand deposits rich in heavy minerals, often including rutile, ilmenite and zircon.
  • the mineral sands may be dry-mined or wet-mined (e.g., dredged).
  • Processing may include gravity separation (e.g., in spiral concentrators) to separate heavy-mineral sand particles (e.g., rutile, ilmenite, zircon) from other sand particles (e.g., silica). Processing may also involve desliming, such as in a centrifuge, to remove clay fines.
  • other heavy minerals e.g., zircon
  • Electrostatic and magnetic properties may be used to separate different heavy minerals.
  • ilmenite has magnetic properties and is often recovered by magnetic separation from non-magnetic minerals (e.g., rutile and zircon).
  • Further ilmenite processing may include smelting to separate the titanium and iron components of the mineral and to concentrate titanium in slag. The slag may then be processed through a traditional chloride process for production of titanium dioxide pigment or opacifier products.
  • the initial feed may be the mineral material as mined, also referred to as "run of mine” material.
  • the initial feed of mineral material may include ilmenite in an amount of at least 7 weight percent, or at least 10 weight percent, or at least 13 weight percent, or at least 14 weight percent, or even at least 15 weight percent or more.
  • the initial feed may include ilmenite in an amount of up to 22 weight percent, or up to 20 weight percent, or up to 18 weight percent.
  • Ti0 2 content in the initial feed of mineral material may be mostly or entirely provided by the ilmenite. When all or substantially all of the Ti0 2 is provided by the ilmenite, then the ilmenite content will be approximately 1.9 times the Ti0 2 content.
  • the initial feed of the mineral material may comprise one or more components in addition to the ilmenite, magnetite and clay.
  • the initial feed in the mineral material may comprise silica, which may be in the form of coarse silica, in an amount up to 3 weight percent or up to 12 weight percent or more. When present, the silica may often be present in an amount of at least 0.5 weight percent.
  • the initial feed of the mineral material may include calcium in an amount of up to 0.25 weight percent, up to 0.1 weight percent or up to 0.05 weight percent. When present, the calcium may often be in an amount of at least 0.005 weight percent, at least 0.01 weight percent or at least 0.03 weight percent.
  • the initial feed of the mineral material may include manganese in an amount up to 0.25 weight percent or up to 0.1 weight percent.
  • the method may include processing directed to preparing the first particulate feed for preparing the first ilmenite concentrate.
  • the first particulate feed may be prepared as or to include the initial feed, e.g., run of mine material.
  • Preparing the first particulate feed may include processing initial feed of the mineral material to better prepare the first particulate feed for beneficial processing by settling velocity separation.
  • Preparing the first particulate feed may include removing one or more of the following from the initial feed: large particles (e.g., +28 mesh), plant material that may be mixed with the mineral material (e.g., from surface mining operations), or trash from mining operations or from storage or handling of the mined mineral material.
  • clay dispersant it is meant a reagent that promotes dispersion of the clay particles and/or stabilizes a dispersion of clay particles to inhibit aggregation.
  • clay dispersants include sodium hexametaphosphate and polyacrylates.
  • a polyacrylate dispersant is Colloid 211 from Kemira, which includes a sodium polyacrylate polymer.
  • the blunging may be performed in a single stage or in multiple stages in series. In one implementation, the blunging may include at least a first blunging stage and a second blunging stage, and optionally with intermediate size separation of particles between the first and second blunging stages. The first blunging stage may help to liberate from clay aggregates larger particles not optimal for further processing.
  • the settling velocity separation may include any process operation that is based on differences in settling velocities between different particles.
  • the settling velocity separation may include a differential settling separation.
  • differential settling separation refers to processing to settle coarse/heavy mineral particles through a dispersed pulp of fine particles in a process vessel (e.g., a tank), such as dispersed particles of clay and silica fines.
  • fines or “fine particles” it is meant generally particles of a size smaller than 10 microns. Dispersion of the clay may be aided by clay dispersant reagent.
  • larger ilmenite particles may tend to preferentially settle due to both a larger particle size and higher density than the dispersed fines.
  • Coarse silica particles may tend to preferentially settle primarily due to a larger particle size than the dispersed fines.
  • differential settling separation a majority of the clay from feed to the differential settling separation may be recovered in overflow and a majority of ilmenite from the feed to the differential settling separation may be recovered in the underflow.
  • a majority of coarse silica from the feed to differential settling separation may be recovered in the underflow.
  • Underflow of differential settling separation may be concentrated in, and overflow of differential settling separation may be depleted in, ilmenite and possibly also coarse in silica relative to feed to the differential settling separation.
  • a majority of clay from feed to differential settling separation may be recovered in overflow.
  • Feed to a differential settling separation process tank may be at an elevation above an elevation of underflow removal and may be at, above or below an elevation of overflow removal.
  • Residence time in a differential settling process tank may be at least 0.5 hour, and may be less than 2 hours.
  • Differential settling may be at a pH of at least pH 6, and may be at a pH of up to pH 9.
  • Differential settling separation may be performed in a thickener, which may be a high rate thickener such as available from WesTech Engineering, Inc., and which may be modified to provide for upward flow within the thickener tank.
  • the settling velocity separation may include elutriation processing.
  • elutriation there is an upward flow of the liquid medium in a process vessel (e.g., a tank), that is sufficiently large to overcome the settling velocity of certain coarse particle constituents in feed to be separated from other particles during the elutriation processing.
  • the elutriation may have an upward flow that is sufficient to overcome the settling velocity of at least some coarse silica particles, and preferably a majority of coarse silica, for separation of coarse silica particles from heavy mineral (e.g., ilmenite-containing) particles, and especially from coarse heavy mineral particles.
  • heavy mineral e.g., ilmenite-containing
  • faster- settling particles may be removed from the process vessel at a lower elevation of the process vessel and slower-settling particles may be removed from a higher elevation of the process vessel.
  • the elevation of the process vessel from which the slower-settling particles are removed may be above the level at which feed of mineral material to be separated is introduced into the process vessel, and the elevation of the process vessel from which the faster-settling particles are removed may be below the elevation at which such feed is introduced into the process vessel.
  • Solids content in the liquid medium during elutriation may often be in a range of from 2 to 25 percent solids by weight.
  • Overflow of elutriation may be concentrated in, and underflow of elutriation may be depleted in, clay and also preferably in coarse silica relative to feed to the elutriation.
  • Residence time in elutriation process tank may be at least 0.5 hours, and may be less than 2 hours.
  • Elutriation may be at a pH of at least pH 6, and may be at a pH of up to pH 9.
  • settling velocity separation includes maintaining an upward fiow of fluid in a process tank (e.g., a differential settling process tank or an elutriation process tank) between elevations where overflow and underflow are removed from the tank.
  • a main target component for removal in overflow is dispersed fines (e.g., differential settling to remove dispersed clay and/or silica fines)
  • the velocity of the upward flow may be no larger than 10 centimeters per minute, no larger than 8 centimeters per minute or no longer than 6 centimeters per minute, and may often be at least 2
  • centimeters per minute at least 3 centimeters per minute or at least 4 centimeters per minute.
  • the velocity of the upward fiow may be at least 3 centimeters per minute, at least 4 centimeters per minute or at least 5 centimeters per minute and may often be no larger than 10 centimeters per minute or no larger than 15 centimeters per minute.
  • Maintaining an upward fiow may include introducing upward flowing streams, or jets, of liquid (e.g., process water) into a process tank (e.g., differential settling process tank or elutriation process tank) at an elevation that is lower than an elevation of mineral material feed to the tank.
  • a process tank e.g., differential settling process tank or elutriation process tank
  • Such upward flowing streams may be introduced into the tank adjacent the bottom (e.g., in upwardly flowing streams introduced via fluid ports through the bottom wall of the tank).
  • the settling velocity separation may include at least two different differential settling velocity separation steps implementing different settling velocity separation operations.
  • the different settling velocity separation operations may include a differential settling separation and an elutriation.
  • a first settling velocity separation step a first portion of the clay may be removed, followed by a second settling velocity separation step to remove a second portion of the clay.
  • Feed to the second settling velocity separation step may include all or a portion of a larger-particle-size fraction of mineral material recovered with underflow from the first settling velocity separation step.
  • the settling velocity separation includes a first settling velocity separation step including differential settling separation and a second settling velocity separation step including elutriation.
  • the settling velocity separation a majority of the clay is removed from the first particulate feed.
  • the settling velocity separation may comprise removing at least 85 weight percent, or at least 90 weight percent or even at least 95 weight percent of the clay from the first particulate feed.
  • Any settling velocity separation operation within the settling velocity separation may be performed in one or in multiple stages in series. In a preferred implementation, each settling velocity separation step is performed in a single stage operation. In one
  • the settling velocity separation includes a first step comprising a single stage of differential settling separation followed by a second step comprising a single stage of elutriation.
  • Each stage may include multiple process vessels in parallel. Any settling velocity separation processing may proceed in a single process train or in multiple parallel process trains.
  • the settling velocity separation may include a first settling velocity separation step and a second settling velocity separation step, and with a size separation intermediate between the first settling velocity separation step and the second settling velocity separation step.
  • a larger particle-size fraction from the size separation may be processed separately from the second particulate feed during the preparation of the second ilmenite concentrate.
  • the size separation may be accomplished by a screen of an appropriate mesh size. In one implementation a 65 mesh screen may be used for the size separation. The screen may be a vibrating screen.
  • the second ilmenite concentrate may comprise all or a portion of magnetic ilmenite- containing and/or magnetite-containing particles recovered by magnetic separation.
  • the second ilmenite concentration is enriched in ilmenite relative to each of the initial feed, the first particulate feed and the second particulate feed.
  • the second ilmenite concentrate being "enriched" in a component it is meant that the second ilmenite concentrate has a higher content, or concentration, of that component relative to each of the initial feed, the first particulate feed or second particulate feed, as the case may be.
  • the second ilmenite concentrate is lower than in the initial feed, first particulate feed or second particulate feed, as the case may be.
  • the second ilmenite concentrate may also be enriched in magnetite relative to one or more of the initial feed, the first particulate feed and the second particulate feed.
  • the second ilmenite concentrate may include ilmenite in an amount of at least 57 weight percent, at least 60 weight percent, at least 65 weight percent, or at least 67 weight percent.
  • the second ilmenite concentrate may include Ti0 2 (including the Ti0 2 content of the ilmenite) in an amount of at least 30 weight percent, at least 33 weight percent or even at least 35 weight percent.
  • the second ilmenite concentrate may include the clay in an amount of not greater than 5 weight percent, not greater than 4 weight percent, not greater than 3 weight percent or not greater than 2 weight percent.
  • the clay may be present in the second ilmenite concentrate in an amount of at least 0.2 weight percent, or at least 0.5 weight percent or at least 1 weight percent.
  • the second ilmenite concentrate may include magnetite in an amount of at least 10 weight percent, at least 15 weight percent or at least 20 weight percent.
  • the second ilmenite concentrate may include ilmenite and magnetite in a combined amount of at least 80 weight percent or at least 90 weight percent.
  • the second ilmenite concentrate may comprise iron oxides (e.g., magnetite, hematite, etc.), other than contained in the ilmenite, in an amount of at least 15 weight percent, at least 20 weight percent or at least 25 weight percent.
  • the second ilmenite concentrate may include silica in an amount up to 5 weight percent, up to 3 weight percent or up to 2 weight percent. When present, the silica may often be in an amount of at least 0.4 weight percent.
  • the second ilmenite concentrate may include calcium in an amount of up to 0.08 weight percent, up to 0.06 weight percent, up to 0.03 weight percent or up to 0.02 weight percent. When present, the calcium may often be in an amount of at least .01 weight percent.
  • the second ilmenite concentrate may include magnesium in an amount of up to 1.0 weight percent, up to 0.8 weight percent or up to 0.7 weight percent. When present, the magnesium may often be in an amount of at least 0.1 weight percent.
  • the second ilmenite concentrate may include manganese in an amount of up to 0.8 weight percent or up to 0.6 weight percent. When present, the manganese may be in an amount of at least 0.1 weight percent or at least 0.2 weight percent.
  • the second ilmenite concentrate may include thorium and/or uranium in a combined amount of up to 100 parts per million by weight, up to 60 parts per million by weight, up to 40 parts per million by weight or up to 30 parts per million by weight.
  • the second ilmenite concentrate may have a weight average particle size of larger than 50 microns, or larger than 100 microns, or larger than 120 microns.
  • the second ilmenite concentrate may be an ilmenite concentrate product of the second aspect of the invention discussed below.
  • the recovery of ilmenite in the second ilmenite concentrate may be at least 64 percent at least 68 percent, at least 70 percent, at least 72 percent, at least 74 percent or at least 76 percent or more relative to ilmenite in the initial feed or relative to ilmenite in the first particulate feed.
  • Weight recovery in the second ilmenite concentrate may be no greater than 25 weight percent, or no greater than 20 weight percent, or no greater than 18 weight percent, or even no greater than 15 weight percent or less of the weight of the initial feed or of the weight of the first particulate feed.
  • the method of the first aspect of the invention may comprise smelting at least a portion of the second ilmenite concentrate to produce a slag containing titanium dioxide, for example by electric arc smelting.
  • This slag may be a slag product according to the third aspect of the invention discussed below.
  • the method of the first aspect of the invention may comprise making bricks comprising at least a portion of clay separated from the mineral material during the settling velocity separation.
  • a second aspect of the invention is provided by a particulate ilmenite concentrate product prepared from mined ilmenite-containing mineral material.
  • the slag product may comprises magnesium oxides (e.g., MgO) in an amount of not greater than 1 weight percent, or not greater than 0.8 weight percent, or not greater than 0.7 weight percent.
  • MgO magnesium oxides
  • the slag product may comprise manganese oxides (e.g., MnO) in an amount of not greater than 1 weight percent, or not greater than 0.7 weight percent, or not greater than 0.5 weight percent.
  • MnO manganese oxides
  • the slag product may comprise chromium oxides (e.g., Cr 2 0 3 ) in an amount of not greater than 0.05 weight percent, or not greater than 0.03 weight percent.
  • chromium oxides e.g., Cr 2 0 3
  • the amount of the titanium dioxide in the slag product may be in a range having a lower limit of any of the weight percentages identified above for titanium dioxide in the slag product and an upper limit of 95 weight percent or 98 weight percent.
  • the slag product may comprise a combined amount of the thorium oxides and uranium oxides in a range having an upper limit of any of the combined amounts identified above in parts per million by weight for thorium oxides and uranium oxides in the slag product and a lower limit of 1 part per million by or 10 parts per million by weight.
  • the titanium-containing slag may be a titanium-containing slag product according to the third aspect of the invention.
  • a fifth aspect of the invention is provided by a method for preparing a titanium dioxide pigment product. The method comprises chloride treatment of a titanium-containing slag product, wherein the slag product is according to the third aspect of the invention.
  • Figure 1 is a process diagram of an embodiment of a method of the invention.
  • Figure 2 is a process diagram of an embodiment of a method of the invention.
  • Figure 4 is a process diagram of an embodiment of a method the invention.
  • Figure 5 is a process diagram of an embodiment of a method of the invention.
  • Figure 6 is a process diagram of an embodiment of a method of the invention.
  • Figure 7 is a schematic of an embodiment of a process tank for differential settling separation.
  • Figure 8 is a top view of a rake shown in the process tank of Figure 7.
  • Figure 11 is a process diagram of one more particular implementation of the more general embodiment shown in Figure 10.
  • Figure 12 is a process diagram of one particular implementation for tails processing, which may be used in combination with the processing shown in Figure 11.
  • Figure 13 illustrates one design for blugner vessel for use in a blunging operation of a method of the invention.
  • Figure 1 shows a generalized process block diagram relating to the method of the first aspect of the invention.
  • an initial feed 102 of particulate, ilmenite- containing mineral material is subjected to a process sequence 104 for preparing first particulate feed.
  • Resulting first particulate feed 106 is subjected to a process sequence 108 for preparing first ilmenite concentrate.
  • clay 110 is removed from the first particulate feed to prepare first ilmenite concentrate that is enriched in ilmenite relative to the first particulate feed 106 and in relation to the initial feed 102.
  • the separated clay 110 (which may be in one or multiple process streams) includes a majority of clay originally in the initial feed 102.
  • a second particulate feed 112 which contains at least a portion of the first ilmenite concentrate (and may be comprised entirely of the first ilmenite concentrate), is subjected to a process sequence 114 for preparing second ilmenite concentrate.
  • additional clay 118 is removed from the second particulate feed and a second ilmenite concentrate 116 is prepared.
  • the separated clay 118 (which may be in one or multiple process streams) may include a majority of the clay from the second particulate feed.
  • the term "at least a portion of a substance or composition means all of that substance or composition or a part of the substance or composition that is less than all of the substance or composition.
  • the initial feed 102 is processed through the process sequence 104, which includes blunging 130 at least a portion of the initial feed 102.
  • the blunging 130 may be performed in the presence of a clay dispersant added before or during the blunging 130.
  • the first particulate feed 106 is subjected to the process sequence 108, which includes subjecting at least a portion of the first particulate feed 106 to settling velocity separation 132.
  • a majority of the clay from the initial feed 102 (e.g., the clay 110) is separated in one or more overflow streams from process vessels of the settling velocity separation 132, and the first ilmenite concentrate is recovered from one or more underflow streams from such process vessels.
  • the second particulate feed 112 is processed through the process sequence 114, which includes magnetic separation 134 of a majority of the ilmenite from the second particulate feed 112.
  • magnetic particles e.g., containing ilmenite
  • the magnetic particles separated during the magnetic separation 134 may include magnetic materials besides ilmenite.
  • Such clay dispersant may be added before or during the first blunging stage 140 and/or before or during the second blunging stage 142.
  • a larger-particle-size fraction is removed from the mineral material, for example by screening.
  • the size separation 144 may, for example, may be a separation at 28 mesh, for example using a 28 mesh screen.
  • the larger-particle-size fraction that is removed is not subjected to the second blunging stage 142.
  • the first particulate feed 106 is subjected to the process sequence 108, including the settling velocity separation 132.
  • the settling velocity separation 132 includes a first settling velocity separation step 146 followed by a second settling velocity separation step 148.
  • the first velocity separation step 146 and second velocity separation step 148 represent different unit operations, with each including implementation of a different separation operation based generally on particle settling velocity in aqueous liquid medium.
  • the first settling velocity separation could involve differential settling separation and the second settling velocity separation could involve elutriation.
  • Each of the first settling velocity separation step 146 and the second settling velocity separation step 148 may include only a single stage or may include multiple stages in series.
  • the second particulate feed 112 which comprises at least a portion of first ilmenite concentrate prepared during the process sequence 108, is subjected to the process sequence 114, including the magnetic separation 134.
  • the magnetic separation 134 includes low-intensity magnetic separation 150 followed by high- intensity magnetic separation 152.
  • the low-intensity magnetic separation 150 removes magnetic particles, such as magnetic ilmenite-containing and/or magnetite-containing particles, from the second particulate feed 112.
  • the high-intensity magnetic separation 152 removes additional magnetic particles from at least a portion of reject material from the low- intensity magnetic separation 150 (i.e., material not magnetically removed during the low- intensity magnetic separation 150).
  • Additional magnetic particles removed during the high- intensity magnetic separation 152 may, for example, contain ilmenite and/or magnetite.
  • the second ilmenite concentrate 116 may include all or some of the magnetic particles removed during both the low-intensity magnetic separation 150 and the high-intensity magnetic separation 152, or during either one of them.
  • the low-intensity magnetic separation 150 involves subjecting material to a lower-intensity magnetic field (e.g., as accomplished with a permanent magnet) and the high-intensity magnetic separation 152 involves subjecting material to a higher-intensity magnetic field (e.g., 0.2 to 1 Tesla).
  • Figure 4 shows a process block diagram of one possible more particular
  • the process sequence 104 is the same as shown in and described with respect to Figure 3.
  • the settling velocity separation 132 of the process sequence 108 includes intermediate size separation 160 between the first settling velocity separation step 146 and the second settling velocity separation step 148.
  • Oversize particulate material 162 from the size separation 160 includes a larger-particle-size fraction separated from the mineral material being processed in the process sequence 108.
  • the size separation 160 may be accomplished, for example, using a screen with appropriate mesh size.
  • the screen may, for example, be a 65 mesh screen for separating out a +65 mesh fraction.
  • the screen may be a vibrating screen.
  • the magnetic separation 134 includes a separate parallel magnetic separation sequence including low- intensity magnetic separation 166 and the high-intensity magnetic separation 168, similar to the low-intensity magnetic separation 150 and the high-intensity magnetic separation 152, except processing a feed of the oversize particulate material 162.
  • magnetic particles such as for example magnetic ilmenite - containing and/or magnetite-containing particles, are magnetically removed from the oversize particulate material 162.
  • At least a portion of the reject material from the low-intensity magnetic separation 166 is processed in the high-intensity magnetic separation 168 to magnetically remove additional magnetic particles, such as additional magnetic ilmenite- containing and/or magnetite-containing particles.
  • the second ilmenite concentrate 116 may include all or a portion of the magnetic particles removed in all of any of the low-intensity magnetic separation 150, the high-intensity separation 152, the low-intensity magnetic separation 166 and the high-intensity magnetic separation 168.
  • the embodiment of the magnetic separation 134 shown in Figure 4 may advantageously permit more optimized design and implementation of the second settling velocity separation step 148 and more optimized design of magnetic separation 134 to more effectively handle the larger-particle- size material of the oversize particulate material 162 and the smaller-particle-size material of the second particulate feed 112.
  • the first settling velocity separation step 146 includes differential settling separation with two differential settling separation stages 172, 174 and with a scrub operation 176 (e.g., attrition scrubbing) intermediate between the first differential settling separation stage 172 and the second differential settling separation stage 174.
  • the first differential settling separation stage 172 is arranged as a rougher stage and the second differential settling separation stage 174 is arranged as a cleaner stage.
  • the intermediate scrub 176 prepares underflow 178 from the first differential settling separation stage 172 for feed to the second differential settling separation stage 174.
  • Underflow 180 from the second differential settling separation stage 174 is fed to the size separation 160.
  • the process sequence 114 is generally the same as shown in and described with respect to Figure 4, including the magnetic separation 134 with separate parallel magnetic separation processing for the second particulate feed 112 and the oversize particulate material 162.
  • the recovered magnetically-separated material is combined to prepare the second ilmenite concentrate 116.
  • the separated clay 118 stream includes reject material from the magnetic separation 134, and the separated clay 118 stream is sent to the tails thickening 182 and centrifuge 184 for preparation of the dewatered clay tails 186.
  • the second ilmenite concentrate 116 is processed through a filter 198 followed by drying 200 to prepare a dry ilmenite concentrate product 202.
  • the dry ilmenite concentrate product 202 may be bagged or otherwise packaged or containerized for easy handling and transportation.
  • Figure 5 also shows flows of process water from a process water feed 204 to various process operations and shows recycle water streams 206 and 208 from the tails thickening 182 and centrifuge 184, respectfully.
  • the tails thickening may include a pH adjustment to promote flocculation of clay.
  • flocculation and settling of clay may be performed at a basic pH to produce high-clarity liquid.
  • the pH for the tails thickening may be at a pH of at least pH 7.5 or at least pH 8.0, and may be at a pH of up to pH 11, up to pH 10.5 or up to pH 10.0.
  • flocculation and settling of clay is performed at an acidic pH, such as with the addition of sulfuric acid as a pH adjustment reagent.
  • the second ilmenite concentrate 116 is processed through the filter 198 followed by the drying 200 to prepare the dry ilmenite concentrate product 202, generally as shown in and described with respect to Figure 5.
  • the dry ilmenite concentrate product 202 may be bagged or otherwise packaged or containerized for easy handling and transportation.
  • Figure 6 also shows flows of process water from the process water feed 204 to various process operations and the shows the recycle water streams 206 and 208 from the tails thickening 182 and centrifuge 184, respectfully, generally as shown in and described with respect to Figure 5.
  • the implementation shown in Figure 6 is advantageous in that it includes very simple and streamlined processing relative to the processing implementation of Figure 5. Important to implementing the implementation shown in Figure 6 is careful design for efficient operation of the single differential settling separation stage 172 and the single elutriation stage 192.
  • Figure 7 shows generally features of a process tank 230, such as may be used for differential settling separation, for example in the differential settling separation stages 172, 174 of the first settling separation step 146 as shown in Figures 5 and 6.
  • the process tank 230 includes an overflow trough 232, a rake 234 and a rotatable shaft 236 to drive rotation of the rake 234.
  • a feed 238 of mineral material to be processed e.g., first particulate feed 106 of Figures 1-6
  • the Overflow 240 spills over into the overflow trough 232 for collection.
  • liquid 248 e.g., process water
  • the upwardly flowing streams of liquid 248 may, for example, be introduced through fluid ports through the bottom of the process tank 230.
  • Figure 9 shows generally features of a process tank 250, such as may be used for elutriation, for example in the elutriation stages 192, 194 as shown in Figures 5 and 6.
  • the process tank 250 includes an overflow trough 252, an agitator 254 and a rotatable shaft 256 to drive rotation of the agitator 254.
  • a feed 258 of mineral material to be processed e.g., from underflow from prior a differential settling separation operation, such as one or more of the differential settling separation stages 172, 174 shown in Figures 5 and 6) is introduced at a mid elevation into of the fluid containment volume of the process tank 250.
  • Overflow 260 spills over into the overflow trough 252 for collection.
  • the feed 258 may include in particular ilmenite, coarse silica and clay particles to be separated.
  • the overflow 260 is enriched in clay, and may also preferably enriched in coarse silica, and depleted in ilmenite relative to the feed 258.
  • the underflow 262 is collected from the bottom of the process tank 250.
  • the underflow 262 is enriched in ilmenite and depleted in clay, and also preferably is depleted in coarse silica, relative to the feed 258.
  • liquid 268 e.g., process water
  • the upwardly flowing streams of liquid 268 may, for example, be introduced through fluid ports through the bottom of the process tank 250.
  • a result is that during settling separation operation, there is an upward flow of fluid through the fluid containment volume of the process tank 250 generally in a direction from an elevation of removal of the underflow 262 (the bottom of the process tank 250 in this implementation) toward the elevation of removal of the overflow 260 (the top of the process tank 250 in this implementation).
  • This generally upward flow of fluid in the process tank 250 is represented by the arrows 269.
  • the velocity of the upward flow 269 will generally be higher above than below the elevation of the process tank 250 where the feed 258 is introduced.
  • the agitator 254 is rotated by the shaft to agitate the contents of process tank 250.
  • the agitator includes a flat circular plate 270 and multiple blades 272. Rotation of the agitator 254 causes liquid to be expelled from the peripheral edge of the plate 270 generally toward the side wall of the tank.
  • a high-shear zone of flow 274 develops in a high-velocity region between the peripheral edge of the agitator 254 and the side wall of the process tank 250.
  • the upwardly flowing streams of liquid 268 are directed toward the rotating agitator and the development of the high-shear zone of flow 274 helps to make a clean separation especially between ilmenite particles and coarse silica particles.
  • a rake may be used at the bottom of the process tank 250 to rake particles concentrating at the bottom of the tank for collection through a central port, similar to the rake 234 shown in and described previously with respect to Figures 7 and 8.
  • Figure 10 shows a process diagram for another particular implementation alternative of the more general implementation shown in and described with respect to Figure 2.
  • the initial feed 102 is processed through the process sequence 104, which includes the blunging 130 of at least a portion of the initial feed 102.
  • the resulting first particulate feed 106 is subjected to the process sequence 108, which includes subjecting at least a portion of the first particulate feed 106 to the settling velocity separation 132.
  • the settling velocity separation 132 includes the first settling velocity separation step 146 and the second settling velocity separation step 148, for example as described with respect to Figure 3.
  • the treated material from the first settling velocity separation step 146 is subjected to scrubbing 280.
  • the scrubbing 280 mineral material being processed is treated to further disaggregate and dispose particles for more effective separation during the second settling velocity separation step 148.
  • the scrubbing 280 may, for example, be an attrition scrubbing operation in which the mineral material being processed is subjected to high shear conditions to further disaggregate and disperse material prior to introduction to the second settling velocity separation step 148.
  • Processed mineral material from the second settling velocity separation step 148 is then processed through scrubbing 282.
  • the scrubbing 282 may be as described for the scrubbing 280, and preferably includes attrition scrubbing in which the processed mineral material is subjected to high shear environment to further disaggregate and disperse material to prepare the second particulate feed 112.
  • the magnetic separation 134 includes the low-intensity magnetic separation 150 and the high-intensity magnetic separation 152, for example as described with respect to Figure 3.
  • Processed material from the blunging vessel 304 is transmitted via a hose pump 314 to a multi-stage screen 316 to prepare a large particle fraction 318, a middle particle fraction 320 and a small particle fraction 322.
  • the large particle fraction 318 and middle particle fraction 320 may contain significant iron oxide (e.g., magnetite) and some ilmenite and may be further processed for iron oxide and ilmenite recovery as desired.
  • the small particle fraction 322 is held and conditioned in three conditioning vessels 324, 326 and 328 arranged in series.
  • conditioning vessels 324, 326 and 328 additional clay dispersant reagent 310 and pH adjustment reagent 312 are added. Also added to the first conditioning vessel 324 is additional recycled process water 308.
  • the material being processed is agitated and conditioned to assist in dispersing clay for effective processing.
  • Material from the last conditioning vessel 328 is transmitted through a hose pump 330 to a single-stage screen 332 to remove an over-size particle fraction 334.
  • An under-size particle fraction 336 is then subjected to the processing sequence 108.
  • Overflow 342 enriched in clay is removed from the top of the hydrosizer vessel 340 and underflow 344 enriched in ilmenite is removed from the bottom of the hydrosizer vessel 340.
  • the underflow 344 is transferred via a hose pump 346 to an attrition scrubbing vessel 348 where the material being processed is subjected to attrition scrubbing to further disaggregate and disperse particulates.
  • the attrition scrubbing vessel 348 may be a two-stage vessel, as shown in Figure 11, with two chambers each fitted with a dual impeller attrition mixer 350.
  • Process water 308 is introduced into a bottom portion of the elutriation vessel 354.
  • Overflow 358 enriched in silica and clay is removed from the top of the elutriation vessel 354 and an underflow 360 enriched in ilmenite is removed from the bottom of the elutriation vessel 354.
  • the underflow 360 is transferred to an attrition scrubbing vessel 362 via a hose pump 364.
  • the attrition scrubbing vessel 362 may be designed in a similar manner to the attrition scrubbing vessel 348 previously discussed.
  • the material being processed is subjected to further attrition scrubbing to further disaggregate and disperse particulates. Material exiting the attrition scrubbing vessel 362 is transferred via a bowl pump 364 for processing through the process sequence 114.
  • material from the scrubbing vessel 362 is fed to a series of three low-intensity magnetic separators 366, 368 and 370 arranged in series.
  • Final magnetic concentrate 372 from low-intensity magnetic separation is transferred via a bowl pump 374 for collection as an ilmenite concentrate (second ilmenite concentrate) in a filter 376.
  • Reject material 378, 380 and 382 from the low-intensity magnetic separators 366, 368 and 370 is transferred via a bowl pump 384 to a thickener vessel 386. Overflow 388 is removed from the top of the thickener vessel 386 and underflow 390 is removed from the bottom of the thickener vessel 386.
  • the underflow 390 is transferred via a hose pump 392 as feed to a series of three high-intensity magnetic separators 394, 396 and 398.
  • the underflow 390 may be diluted with fresh water 400 prior to introduction into the first high-intensity magnetic separator 394.
  • a final magnetic concentrate 402 from the last high-intensity magnetic separator 398 is transferred via a bowl pump 404 for collection as ilmenite concentrate (second ilmenite concentrate) in a filter 406.
  • Reject material 408, 410 and 412 from the high-intensity magnetic separators 394, 396 and 398 may be transferred via a bowl pump 414 as a combined reject stream 416 for tails processing.
  • recycle process water 308 may be added at various locations as needed to maintain appropriate slurry densities. It is preferred that fresh water 400 be used for water additions as needed for the magnetic separations.
  • FIG. 12 shows a process diagram showing one example of particular implementation for tails processing that may be used, for example, in combination with the processing shown in Figure 11.
  • overflow 342 from the hydrosizer vessel 340 ( Figure 11) is fed to an overflow vessel 420.
  • Material from the overflow vessel 420 is transferred via an air-operated pump 422 to a flocculation vessel 424.
  • Flocculant reagent 425 is added to the flocculation vessel 424 to promote flocculation of clay particles.
  • Material from the flocculation vessel 424 is transferred to a tailings thickener vessel 426.
  • Underflow 428 from the tailings thickener vessel 426 is transferred via a hose pump 430 to a tailing storage pond (not shown).
  • the underflow 428 is concentrated in flocculated clay settling in the tailings thickener vessel 426.
  • Overflow 432 from the tailings thickener vessel 426 is transferred to a pH adjustment vessel 434 where pH is adjusted by addition of a pH adjustment reagent 436 to promote effective flocculation and setting of clay. If operating at an acidic pH, the pH may be lowered through addition of an acidic pH adjustment reagent 436 (e.g., sulfuric acid). If operating at a basic pH, a basic pH adjustment reagent 436 (e.g., sodium hydroxide) may be used.
  • an acidic pH adjustment reagent 436 e.g., sulfuric acid
  • a basic pH adjustment reagent 436 e.g., sodium hydroxide
  • Material from the pH adjustment vessel tank 434 is transferred to a flocculation vessel 438, to which additional flocculant reagent 425 is added to further promote clay flocculation in the flocculation vessel 438.
  • additional flocculant reagent 425 is added to further promote clay flocculation in the flocculation vessel 438.
  • the overflow 388 is also introduced into the flocculation vessel 438 for treatment in the flocculation vessel 438.
  • Overflow from the tailings thickener vessel 456 is transferred to an overflow tank 460. Material from the flocculation vessel 438 is also transferred to the overflow tank 460. Additional flocculation reagent 425 is added to the overflow tank 460 and a treated stream 462 is withdrawn from the overflow vessel 460 for transfer to a recycle water pond (not shown).
  • the clay dispersant reagent 310 is Colloid 211 (Kemira).
  • the pH adjustment reagent 312 is sodium hydroxide to raise the pH in the conditioning vessels 324, 326 and 328.
  • the pH of material exiting the final conditioning vessel 328 is at about pH 7.25.
  • the single-stage screen 332 may be such that the over-size fraction 334 is a + 28 mesh fraction and the undersize fraction 336 is a - 28 mesh fraction.
  • the hydrosizer vessel 340 is operated with an upward flow velocity of about 1.25 gallons per minute per square foot (about 6 centimeters per minute).
  • the elutriation vessel 354 is operated with an upward flow velocity of about 1.25 gallons per minute per square foot (about 6 centimeters per minute).
  • the pH adjustment reagent 436 is sulfuric acid.
  • the pH in the pH adjustment tank 434 is at an acidic pH of about pH 5.
  • the flocculant reagent 425 is Superlfloc A-l 10 (Kemira), an anionic f occulent reagent.
  • Slurring densities are designed for about 35 percent in the blunger vessel 304; about 12.5 percent in the conditioning vessels 324, 326 and 328 and the hydrosizer vessel 340; about 55 percent in underflow 344 from the hydrosizer vessel 340; about 10 percent in overflow 342 from the hydrosizer vessel 340; about 3 percent in the elutriation vessel 354; about 1-2 percent in overflow 358 from the elutriation vessel 354; about 60 percent in underflow 360 from the elutriation vessel 354; about 20 percent to the first low-intensity magnetic separators 366, 368 and 370; about 20 percent to the high-intensity magnetic separators 394, 396 and 398; about 11 percent in the tailings thickener vessel 426; and about 1-2 percent in the tailings thickener vessel 456.
  • Additions of the clay dispersant reagent are about 2 kilograms per tonne total, with about half being added in the b
  • FIG. 13 shows a blunger vessel 480 including a dual impeller agitator 482 with opposing impeller blades 484, 486.
  • a partition barrier 488 is disposed within the vessel 480 to create a restricted space in the vessel 480 between the opposing impellers blades 484, 486.
  • a feed 490 may be introduced into the blunger vessel 480 and processed material 492 may be removed as overflow.
  • the shaft of the dual impeller agitator 482 is rotated causing rotation of the impeller blades 484 and 486.
  • the impeller blades 484 and 486 direct circulation of fluid within the blunger vessel 480 as shown by the arrows within the blunger vessel 486, such that the impeller blades 484 and 486 force into the restricted space in the middle portion of the vessel 480, creating a high shear environment conducive to promoting disaggregation and dispersion of particulates.
  • a "stage” as used herein means a stage in series of a process step or unit operation. Any processing shown or described may be performed in multiple parallel processing sequences. Any process flow or material shown or described may be in a single of multiple separate steams or portions.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

L'invention concerne une méthode de traitement de matériaux minéraux contenant de l'ilménite avec une teneur élevée en argile comprenant une séparation par vitesse de sédimentation afin de préparer un premier concentré d'ilménite, suivie d'un traitement par séparation magnétique afin de préparer un deuxième concentré d'ilménite. La séparation par vitesse de sédimentation peut comprendre une séparation par sédimentation différentielle principalement afin d'éliminer l'argile et les fines de silice suivie d'une élutriation pour l'élimination de la silice grossière et d'autres fines. L'invention concerne aussi des produits à base de concentré d'ilménite haute qualité et des produits à base de scories avec de faibles concentrations en matériaux contaminants problématiques.
PCT/US2011/056164 2010-10-15 2011-10-13 Méthode de traitement de matériaux minéraux contenant de l'ilménite avec une teneur élevée en argile, et produits associés Ceased WO2012051424A2 (fr)

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US39379810P 2010-10-15 2010-10-15
US61/393,798 2010-10-15
US201161510375P 2011-07-21 2011-07-21
US61/510,375 2011-07-21

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WO2012051424A2 true WO2012051424A2 (fr) 2012-04-19
WO2012051424A3 WO2012051424A3 (fr) 2012-07-19
WO2012051424A9 WO2012051424A9 (fr) 2012-09-20

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WO2015104324A1 (fr) 2014-01-08 2015-07-16 Basf Se Procédé pour réduire par élutriation le débit volumique d'un flux comprenant des agglomérats magnétiques
CN105439195A (zh) * 2015-05-18 2016-03-30 华东理工大学 一种硫酸法钛白工艺酸解渣中钛资源的高效回收方法和装置
EP3153776A1 (fr) * 2015-10-08 2017-04-12 Improbed AB Cycle de gestion de lit pour une chaudière à lit fluidisé et dispositif correspondant
US9896918B2 (en) 2012-07-27 2018-02-20 Mbl Water Partners, Llc Use of ionized water in hydraulic fracturing
US10036217B2 (en) 2012-07-27 2018-07-31 Mbl Partners, Llc Separation of drilling fluid
CN110019620A (zh) * 2017-12-07 2019-07-16 核工业北京地质研究院 一种适用于砂岩型铀矿层间氧化方向的判别方法
US11708286B2 (en) 2020-08-19 2023-07-25 Marmon Industrial Water Llc High rate thickener and eductors therefor

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9896918B2 (en) 2012-07-27 2018-02-20 Mbl Water Partners, Llc Use of ionized water in hydraulic fracturing
US10036217B2 (en) 2012-07-27 2018-07-31 Mbl Partners, Llc Separation of drilling fluid
US10486086B2 (en) 2014-01-08 2019-11-26 Basf Se Process for reducing the volume flow comprising magnetic agglomerates by elutriation
CN105873653A (zh) * 2014-01-08 2016-08-17 巴斯夫欧洲公司 通过淘析减少包含磁性附聚物的体积流的方法
CN105873653B (zh) * 2014-01-08 2018-08-10 巴斯夫欧洲公司 通过淘析减少包含磁性附聚物的体积流的方法
WO2015104324A1 (fr) 2014-01-08 2015-07-16 Basf Se Procédé pour réduire par élutriation le débit volumique d'un flux comprenant des agglomérats magnétiques
CN105439195A (zh) * 2015-05-18 2016-03-30 华东理工大学 一种硫酸法钛白工艺酸解渣中钛资源的高效回收方法和装置
EP3153776A1 (fr) * 2015-10-08 2017-04-12 Improbed AB Cycle de gestion de lit pour une chaudière à lit fluidisé et dispositif correspondant
CN108700289A (zh) * 2015-10-08 2018-10-23 因姆普朗伯德公司 用于流化床锅炉的床管理循环及相应的装置
US11187406B2 (en) 2015-10-08 2021-11-30 Improbed Ab Bed management cycle for a fluidized bed boiler and corresponding arrangement
CN110019620A (zh) * 2017-12-07 2019-07-16 核工业北京地质研究院 一种适用于砂岩型铀矿层间氧化方向的判别方法
US11708286B2 (en) 2020-08-19 2023-07-25 Marmon Industrial Water Llc High rate thickener and eductors therefor
US12600656B2 (en) 2020-08-19 2026-04-14 Marmon Industrial Water Llc High rate thickener and eductors therefor

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WO2012051424A9 (fr) 2012-09-20
AR082460A1 (es) 2012-12-12
WO2012051424A3 (fr) 2012-07-19
PE20131491A1 (es) 2014-01-10
BRPI1104050A2 (pt) 2015-05-26

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