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WO1993022465A1 - PROCEDE DE PURIFICATION DE MINERAI D'OXYDE DE TITANE (TiO2) NATUREL - Google Patents

PROCEDE DE PURIFICATION DE MINERAI D'OXYDE DE TITANE (TiO2) NATUREL Download PDF

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Publication number
WO1993022465A1
WO1993022465A1 PCT/US1992/003445 US9203445W WO9322465A1 WO 1993022465 A1 WO1993022465 A1 WO 1993022465A1 US 9203445 W US9203445 W US 9203445W WO 9322465 A1 WO9322465 A1 WO 9322465A1
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WO
WIPO (PCT)
Prior art keywords
ore
temperature
mineral acid
contacting
percent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US1992/003445
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English (en)
Inventor
Tze Chao
Wallace L. Kremer
Marcelo Jose da FONSECA MOURÃO
Jose Marcio JARDIM PAIXÃO
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Vale SA
EIDP Inc
Original Assignee
Companhia Vale do Rio Doce
EI Du Pont de Nemours and Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Application filed by Companhia Vale do Rio Doce, EI Du Pont de Nemours and Co filed Critical Companhia Vale do Rio Doce
Priority to PCT/US1992/003445 priority Critical patent/WO1993022465A1/fr
Priority to AU23359/92A priority patent/AU2335992A/en
Publication of WO1993022465A1 publication Critical patent/WO1993022465A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
    • C22B34/1213—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by wet processes, e.g. using leaching methods or flotation techniques

Definitions

  • This invention relates to an improved method for purifying anatase Ti ⁇ 2 ore which contains numerous impurities.
  • the purified ore can be used to make Ti ⁇ 2 pigment or titanium metal or be used in any other process where a purified Ti ⁇ 2 ore is required.
  • phosphorus can cause processing problems in the chloride Ti ⁇ 2 process, and thorium and uranium may concentrate in the Ti ⁇ 2 process and present a potential health hazard.
  • impurities of aluminum, rare earths, phosphorus, thorium, and uranium are additionally a problem because they are especially resistant to removal by conventional mechanical or chemical means.
  • impurities which are especially important to reduce to acceptable levels are calcium, barium, strontium, thorium and uranium. It is important to reduce calcium, barium and strontium to acceptable levels because they can cause sticking and, thus, operability problems in the fluidized bed chlorinator, which is the first step in the chloride Ti ⁇ 2 process. Reducing thorium and uranium to acceptable levels is important because they can be potential health hazards. Unfortunately, such impurities are especially resistant to reducing to acceptable levels.
  • the calcium will not exceed about 0.25 weight percent calculated as CaO; the combined calcium, barium and strontium will not exceed about 0.30 weight percent; and the combined thorium and uranium will not exceed about 200 parts per million. More preferably in the beneficiated Ti ⁇ 2 ore, the calcium will not exceed about 0.20 weight percent; the combined calcium, barium and strontium will not exceed about 0.25 weight percent; and the combined thorium and uranium will not exceed about 150 parts per million. (The foregoing percentages in this paragraph are percent by weight, based on the weight of the ore and are calculated as the metallic oxide.)
  • prethermal treatment such as prereduction as an essential step.
  • Prethermal treatment is undesirable because it is expensive (due to substantial energy and investment requirements) and tends to make it more difficult to remove radionuclides such as thorium and uranium. It, therefore, would be desirable to have a beneficiation process which did not require prethermal treatment as an essential step.
  • U. S. Patent 4,176,159 discloses a process for the removal of impurities from anatase ore. The process requires high temperature calcining, cooling, reducing, cooling, magnetic separation, mineral acid leaching, neutralizing, and washing.
  • U. S. Patent 4,562,048 discloses the bene ⁇ ficiation of titaniferous ores by leaching with a mineral acid.
  • the temperature used is 120-150 degrees C.
  • the pressure used is 10-45 pounds per square inch gauge ("psig") .
  • An essential aspect is the venting of water vapor generated during the leaching process. Prior to leaching, the ore is reduced at about 600-1100*C.
  • U. S. Patent 4,321,236 discloses a process for beneficiating titaniferous ore.
  • the process requires preheating the ore and a mineral acid prior to admixing them in a leaching operation.
  • the temper ⁇ ature is maintained at 110-150 degrees C.
  • the pressure is maintained at 20-50 psig.
  • reductive roasting at about 800-1100 ⁇ C is suggested prior to leaching.
  • U. S. Patent 4,019,898 discloses the addi ⁇ tion of a small amount of sulfuric acid to the leach liquor used to beneficiate ilmenite ore.
  • the te pera- ture used is 100-150 degrees C.
  • the pressure used is up to 50 psig.
  • the ore is reduced prior to leaching at a temperature of about 700-1200"C.
  • Process for beneficiating anatase titanium dioxide ore comprising:
  • step (b) removing the leachate from the product of step (a) .
  • Such purified Ti ⁇ 2 ore is especially suitable for making Ti ⁇ 2 pigment by the chloride process.
  • the process of this invention is highly useful and desirable because it can make practical the utilizat ⁇ tion of low grade, inexpensive and more abundant anatase Ti ⁇ 2 ore which contains numerous impurities.
  • the process is also simple and requires few steps.
  • the process of this invention can have considerably less energy requirements and investment requirements than many prior art processes because a roasting step prior to leaching generally is optional.
  • the process of this invention can reduce calcium, barium, strontium, thorium and uranium to acceptable levels.
  • the process of this invention (1) often can reduce the calcium in the beneficiated ore to a level generally not exceeding about 0.25 percent by weight, and often not exceeding about 0.20 percent by weight; (2) often can reduce the combined thorium and uranium to a level less than about 200 parts per million, and often less than about 150 parts per million; and (3) often can reduce the combined calcium, barium and strontium to a level not exceeding about 0.30 percent by weight, and often not exceeding about 0.25 percent by weight. (In this paragraph, the foregoing percentages are percent by weight, based on the weight of the ore and calculated as the metallic oxide) .
  • DETAILED DESCRIPTION OF THE INVENTION The following sets forth a detailed descrip ⁇ tion of this invention. It should be noted that the process of this invention can be run on a batch or continuous basis.
  • anatase titanium dioxide ore in any form can be used for the process of this invention.
  • Preferred is Brazilian anatase, and especially preferred is anatase from a carbonatite source.
  • anatase titanium dioxide ore includes the raw ore and beneficiates and derivatives thereof such as reduced titania, blowover fines from chlorinators or other process streams from a i ⁇ 2 manufacturing process.
  • Crandallite sub-group minerals such as Florencite CeAl 3 (P0 4 )2(OH)6
  • the impurities which can be removed in accordance with the process of this invention include alkali metals, alkaline earth metals, rare earth metals, iron, aluminum, phosphorus, thorium, uranium, chromium, manganese, vanadium and yttrium.
  • Especially suitable for removal by the process of this invention are the impurities of iron, phosphorus, aluminum, calcium, barium, strontium, chromium, manganese, vanadium, yttrium, lanthanum, cerium, neodymium, thorium, and uranium.
  • impurities of phosphorus, aluminum, iron, calcium, barium, strontium, and radionuclides such as thorium and uranium are especially detrimental to the chloride process for making Ti ⁇ 2 pigment? such impurities can be readily reduced to acceptable levels by the process of this invention.
  • impurities of aluminum, rare earths, phosphorus, thorium, and uranium are especially resistant to removal by conventional chemical or mechanical means, they can readily be reduced to acceptable levels by the process of this invention.
  • the high levels of impurities of phosphorous, rare earth elements, thorium and uranium are quite unique to the Brazilian carbonatite anatase ores. Effective removal of these impurities are critical to the Ti ⁇ 2 chloride process and is a unique feature of this invention.
  • impurities is meant the foregoing metals in their elemental state, oxides thereof, salts thereof and other complexes thereof.
  • the ore should be in particulate form.
  • the optimum particle size for any Ti ⁇ 2 ore desired to be processed can readily be determined by comminuting (such as by grinding, crushing, milling, etc.) the ore into several different particle sizes and evaluating the amount of impurities removed by the process of this invention.
  • the ore should have a particle size of less than about one-fourth inch. If ore treated in accordance with this invention is to be used in the chloride process for making Ti ⁇ 2 its particle size can be adjusted so that it is compatible with such process. In such case, the particles preferably will fall within the range of about -20 mesh to +400 mesh. Of course, some ores in their natural state have a particle size within this range. If so, additional comminuting is not necessary.
  • mineral dressing is meant mechanical processes which can remove some of the undesired impurities, including desliming (removing fine particles by a cyclone, grating or settling process) , crushing, grinding, classification, screening, flotation, electrostatic separation and magnetic separation.
  • the magnetic separation is one of the important steps of this invention and generally involves low, medium and high intensity magnetic field strength and/or gradient; including, preferably, staged magnetic separation sequential through low, medium and high intensity magnetic field strengths.
  • Suitable mineral dressing processes are disclosed in U.S. Patent 4,243,179, which is hereby incorporated by reference. If mineral dressing is used, it can be designed to reduce the ore to the desired particle size in order to satisfy both mineral liberation and Ti ⁇ 2 ore chlorination requirements.
  • the ore prior to the leaching process of this invention, can be subjected to low temperature reductive roasting.
  • the purpose of such low temperature reductive roasting is to convert some of the iron bearing minerals to magnetic form, which can be removed by magnetic separation techniques.
  • low temperature reductive roasting it generally will be carried out at a tempera- ture in excess of ambient conditions up to about 400 degrees C. , in the presence of a carbonaceous reducing agent.
  • a carbonaceous reducing agent Preferably the temperature will be about 200-400 and most preferably about 250-300 degrees C.
  • Suitable carbonaceous reducing agents include coke, lignite char, charcoal, coal, lignite, petroleum such as residual oil, carbon monoxide, producer gas. hydrogen, gaseous hydrocarbons, and natural gas. Preferred is carbon monoxide. Note that to use reducing agents other than carbon monoxide, the roasting temperature should exceed about 300 degrees C. The roasting should take place under reductive conditions, i.e., in the substantial absence of air or oxygen or under conditions which favor reduction rather than oxidation.
  • low temperature roasting it can be carried out by any suitable means, process or device.
  • a fixed bed, rotary kiln, fluidized bed, a plasma jet, batch or continuous process can be utilized.
  • the time required for the low temperature roasting step can readily be determined by making several experimental trials and selecting those which produce the desired results with the lowest tempera ⁇ ture and the least time so that output can be opti ⁇ mized and energy consumption can be minimized. Suitable times often will be in the range of about five minutes to 8 hours, preferably about five minutes to 2 hours, and most preferably about 15 minutes to one hour.
  • the low temperature roasting step preferably should be followed-up with wet or dry magnetic separation to remove the iron containing materials which have been converted to magnetic form.
  • low temperature reductive roasting may make phosphorus, aluminum, thorium and uranium more resistant to the leaching step of the process of this invention. Therefore, if these impurities are present in appreciable amounts, low temperature reductive roasting may not be suitable. Running a few experimental tests can readily determine whether or not a low temperature reductive roast will be beneficial. If the low temperature reactive roasting is not used, the anatase ore should be subjected to medium and high intensity and gradient magnetic separations to a desired level of Ti ⁇ 2 and FeO x before the leaching process of this invention.
  • the ore prior to the leaching process of this invention, can be subjected to a high temperature reductive roasting. It has been found that such roasting can further reduce the amounts of phosphorus compounds in the ore and lower the tempera ⁇ ture needed for the leaching step. If a high tempera ⁇ ture reductive roasting is used, it generally will be carried out at a temperature of about 900-1700 degrees C, in the presence of a carbonaceous reducing agent. Suitable carbonaceous reducing agents include coke, lignite char, charcoal, coal, lignite, petroleum such as residual oil, carbon monoxide, producer gas, hydrogen, and natural gas.
  • the roasting should take place under reductive conditions, i.e., in the sub ⁇ stantial absence of air or oxygen or under conditions which favor reduction rather than oxidation.
  • a preferred temperature range is about 1100-1500 * C. It has also been found that a high temperature reductive roasting can enhance the removal of thorium and uranium, but may be detrimental to the removal of aluminum.
  • roasting it can be carried out by any suitable means, process or device.
  • a fixed bed, rotary kiln, fluidized bed, a plasma jet, batch or continuous process can be uti ⁇ lized.
  • the time required for the high temperature roasting step can readily be determined by making several experimental trials and selecting those which produce the desired results with the lowest tempera ⁇ ture and the least time so that output can be opti ⁇ mized and energy consumption can be minimized. Suitable times often will be in the range of about five minutes to 8 hours, preferably about five minutes to 2 hours, and most preferably about 15 minutes to one hour.
  • a substantial advantage of this invention is that it generally can produce a high quality beneficiated ore without the use of any reductive roasting, and this can save substantial investment and operating costs.
  • the ore prior to the leaching step, can be subjected to a preleach operation.
  • the purpose of the preleach step is to remove impurities which can be removed with milder conditions than the leaching step described below. Use of the preleach step could enhance the economics of the process and, in some grades of ore, could improve quality.
  • the acids and concentration of acids described below for the leaching step can be used.
  • the spent acid from the leach step can be used as the feed for the preleach step. Suitable temperatures are about 50-100"C, preferably about 60-90'C and most preferably 70-80 # C. The pressure ordinarily will be about atmospheric.
  • suitable acids include hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, and mixtures thereof. Especially preferred are hydrochloric acid, nitric acid, hydrofluoric acid, and mixtures thereof. Most especially preferred is hydrochloric acid.
  • the acid should be utilized in an effective amount, i.e., an amount and concentration sufficient to solubilize substantially the impurities. Analysis of the leachate, i.e., the acid solution containing the dissolved impurities, and the leached ore can readily determine whether or not the amount and/or concentration of acid is sufficient.
  • the acid concen ⁇ tration should be at least 3% by weight, based on the total weight of the solution. Ordinarily, the acid will be present in an amount of about 3-30% by weight, based on the total weight of the solution. Prefer ably, the concentration of the acid will be about 5-25 percent, and most preferably about 15-25 percent by weight, based on the total weight of the solution. If sulfuric acid is used, lower concentrations within the foregoing ranges may be preferable because higher concentrations of sulfuric acid may dissolve undesir ⁇ able amounts of Ti ⁇ 2 «
  • the acid leaching treatment will take place at a temperature and pressure, and for a time which is sufficient to solubilize substantially the mineral impurities present. Ordinarily, the time required will be at least about 5 minutes. Typical ranges of time are about 10 minutes to four hours, preferably about 10 minutes to two hours and most preferably about 10 minutes to one hour.
  • the temperature will ordinarily be about 160-300, preferably about 160-250, and most preferably about 170-210 degrees C.
  • the broadest temperature range is about 150-300 * C and preferably is in excess of 150'C up to about 300*C.
  • An especially preferred temperature range is about 190-210'C.
  • An especially preferred temperature is about 190 * C.
  • the pressure will generally be autogenous, i.e.
  • the pressure range will be about 4-100 atmospheres abso ⁇ lute, preferably about 5-75 atmospheres absolute, and most preferably about 10-60 atmospheres absolute.
  • concentrate substantially as used to describe the leaching treatment, is meant the concentration of acid and conditions of temperature, pressure, and time which will solubilize at least about 10% by weight of the total impurities. Prefer ⁇ ably, at least 50% of the total impurities will be solubilized. Often, a graph of the concentration of the acid and conditions of temperature and time, compared to the amount of impurities removed will help to determine trends and optimizations.
  • the ore can be subjected to washing with an aqueous solution of an alkali metal compound after the leachate has been removed from the ore. It has been found that such washing can be helpful to reduce further the amount of phosphorus, aluminum, and silicon impurities.
  • Suitable alkali metal compounds which can be used include sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, lithium hydroxide, and lithium carbonate. Preferred are sodium hydroxide and sodium carbonate. Most preferred is sodium hydroxide.
  • the alkali metal compound should be used in an effective amount, i.e., an amount and concentration sufficient to solubilize substantially at least some of the impurities.
  • Analysis of the leachate, i.e., the solution of the alkali metal compound containing the dissolved impurities, and the leached ore can readily determine whether or not the amount and concentration of alkali metal compound are sufficient.
  • the concentration of alkali metal compound will be about 3-30 percent, preferably about 5-15 percent, and most preferably about 10-15 percent by weight, based on the total weight of the solution.
  • the washing treatment with the aqueous solution of an alkali metal compound will take place at a temperature, pressure, and time which is suffi ⁇ cient to solubilize at least some of the remaining mineral impurities.
  • the time required will be at least about one-half minute. Typical ranges of time are about one-half minute to three hours, preferably about one minute to two hours, and most preferably about one minute to one hour.
  • the temperature ordinarily will be about ambient to about the boiling point of the washing solution. It should be noted that elevated temperature often will decrease the amount of wash time required.
  • atmo ⁇ spheric pressure will be adequate, although elevated pressures can be used if desired. If only atmospheric pressure is used for this step of the process, after the leachate has been removed from the ore, the washing can be done by spraying alkali solution onto the ore which is on a filter or screen.
  • the leachate is removed from the treated Ti ⁇ 2 ore.
  • this is done by removing the leachate followed by washing with water or by washing with water alone.
  • the leachate can be removed by any suitable means, including filtering. decanting, centrifuging or use of a hydroclone.
  • the water will be hot, i.e., up to its boiling point. The amount of washing required can readily be determined by analyzing the wash water for the presence of impurities, acid and/or alkali.
  • the ore After the ore has been treated in accordance with the process of this invention, it can be used to make Ti ⁇ 2 pigment or titanium metal or be used in any process where a purified Ti ⁇ 2 ore is desired.
  • the Ti ⁇ 2 ore treated by the process of this invention can be used to make Ti ⁇ 2 pigment, and most preferably, to make Ti ⁇ 2 pigment by the chloride process.
  • Suitable chloride processes and reactors for using the Ti ⁇ 2 ore treated in accordance with the process of this invention are disclosed in U.S. Patents 2,488,439, 2,488,440, 2,559,638, 3,203,763, 2,833,626, 3,284,159, and 2,653,078, which are hereby incorporated by reference.
  • An anatase titanium-bearing ore derived from a carbonatite deposit was upgraded by ore-dressing to about 65 percent Ti ⁇ 2 hereinafter referred to as mechanical concentrate or "MC". Twenty grams of this MC were leached hydrothermally with 200 milliliters of 20 percent HCl (220 grams HCl/liter) at 190 C for 60 minutes in a tantalum-clad steel bomb at a pressure which varied during the reaction from about 13.6-34 atmospheres absolute. The bomb was mounted on a rocking mechanism for agitation during the reaction. After reaction, the reactor mass was cooled to approximately 100" C before discharge. The dis ⁇ charged sample was then filtered immediately while still hot and washed with hot water 3 times.
  • MAGNETIC SEPARATION Low intensity ca. 500 gauss Magnetic fraction 37.5% (ca. 20% Ti ⁇ 2 loss)
  • the reactor mass was treated in a similar fashion as described in Example 1, including a wash with 20% NaOH.

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Abstract

L'invention concerne un procédé destiné à enrichir du minerai d'oxyde de titane naturel et consistant (a) à mettre en contact le minerai avec une solution aqueuse d'un acide minéral ayant une concentration d'environ 3 à 30 pour cent en poids, ceci ayant lieu à une température d'environ 160 à 300 degrés C, jusqu'à ce que la quantité désirée d'impuretés soit solubilisée et le produit de lixiviation formé, et (b) à éliminer le lixiviat du produit de l'étape (a).
PCT/US1992/003445 1992-05-01 1992-05-01 PROCEDE DE PURIFICATION DE MINERAI D'OXYDE DE TITANE (TiO2) NATUREL Ceased WO1993022465A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/US1992/003445 WO1993022465A1 (fr) 1992-05-01 1992-05-01 PROCEDE DE PURIFICATION DE MINERAI D'OXYDE DE TITANE (TiO2) NATUREL
AU23359/92A AU2335992A (en) 1992-05-01 1992-05-01 Process for purifying anatase TiO2 ore

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PCT/US1992/003445 WO1993022465A1 (fr) 1992-05-01 1992-05-01 PROCEDE DE PURIFICATION DE MINERAI D'OXYDE DE TITANE (TiO2) NATUREL

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022076564A1 (fr) * 2020-10-06 2022-04-14 The Mosaic Company Procédé de production de dioxyde de titane à partir de minerai anatase par digestion à l'acide sulfurique, suivie d'une lixiviation, d'une hydrolyse et d'une calcination

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2804375A (en) * 1953-05-28 1957-08-27 Nat Distillers Chem Corp Cyclic process for the beneficiation of titania ores and slags
US2875039A (en) * 1955-08-26 1959-02-24 Columbia Southern Chem Corp Method of leaching unreduced ironcontaining titaniferous ores
EP0243725A2 (fr) * 1986-04-03 1987-11-04 E.I. Du Pont De Nemours And Company Procédé de purification de minerai d'oxyde de titane
US5011666A (en) * 1988-07-28 1991-04-30 E. I. Du Pont De Nemours And Company Method for purifying TiO2 ore

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2804375A (en) * 1953-05-28 1957-08-27 Nat Distillers Chem Corp Cyclic process for the beneficiation of titania ores and slags
US2875039A (en) * 1955-08-26 1959-02-24 Columbia Southern Chem Corp Method of leaching unreduced ironcontaining titaniferous ores
EP0243725A2 (fr) * 1986-04-03 1987-11-04 E.I. Du Pont De Nemours And Company Procédé de purification de minerai d'oxyde de titane
US5011666A (en) * 1988-07-28 1991-04-30 E. I. Du Pont De Nemours And Company Method for purifying TiO2 ore

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022076564A1 (fr) * 2020-10-06 2022-04-14 The Mosaic Company Procédé de production de dioxyde de titane à partir de minerai anatase par digestion à l'acide sulfurique, suivie d'une lixiviation, d'une hydrolyse et d'une calcination
US20230373809A1 (en) * 2020-10-06 2023-11-23 The Mosaic Company Process for the production of titanium dioxide from anatase ore through sulphuric acid digestion, followed by leaching, hydrolysis, and calcination

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