GB1568333A - Method for obtaining higher tio2 grade anatase concentrates from lower tio2 grade anatase concentrates - Google Patents
Method for obtaining higher tio2 grade anatase concentrates from lower tio2 grade anatase concentrates Download PDFInfo
- Publication number
- GB1568333A GB1568333A GB8896/78A GB889678A GB1568333A GB 1568333 A GB1568333 A GB 1568333A GB 8896/78 A GB8896/78 A GB 8896/78A GB 889678 A GB889678 A GB 889678A GB 1568333 A GB1568333 A GB 1568333A
- Authority
- GB
- United Kingdom
- Prior art keywords
- concentrate
- tio2
- magnetic
- sulphidisation
- grade
- 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.)
- Expired
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 110
- 239000012141 concentrate Substances 0.000 title claims description 34
- 238000000034 method Methods 0.000 title claims description 20
- 239000002253 acid Substances 0.000 claims description 27
- 238000002386 leaching Methods 0.000 claims description 26
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 17
- 238000007885 magnetic separation Methods 0.000 claims description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 7
- 239000011707 mineral Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 description 35
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 235000011149 sulphuric acid Nutrition 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052976 metal sulfide Inorganic materials 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical class [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910010252 TiO3 Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000010405 reoxidation reaction Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 235000010269 sulphur dioxide Nutrition 0.000 description 2
- 239000004291 sulphur dioxide Substances 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- QENHCSSJTJWZAL-UHFFFAOYSA-N magnesium sulfide Chemical class [Mg+2].[S-2] QENHCSSJTJWZAL-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
(54) A METHOD FOR OBTAINING HIGHER TiO2 GRADE
ANATASE CONCENTRATES FROM LOWER TiO2 GRADE
ANATASE CONCENTRATES
(71) We, MINERACAO VALE DO PARANAIBA S.A.-VALEP, a
Brazilian Company of Rua Marquis de Maria NO 181, Belo Horizonte, Minas
Gerais, Brazil, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed to be particularly described in and by the following statement:
The present invention relates to a chemical up-grading process for lower TiO2 grade anatase concentrates which makes it possible to obtain therefrom higher
TiO2 grade anatase concentrates having chemical properties very similar to those of naturally occurring rutile ore, and containing a high percentage of titanium dioxide (TiO2) and only a small content of iron.
Titanium, which is one of the most abundant elements in the earth's crust, has hitherto been found to occur naturally in only two mineral forms of commercial importance, namely rutile and ilmenite. Rutile ore, when pure, consists basically of titanium dioxide (about 96% by weight), with very small percentages of iron.
Ilmenite, which is essentially a ferrous titanate (FeO. TiO2), theoretically has a
TiO2 content of 52.66% by weight. This value, however, may vary between 40 and 60% in commercially available products, depending mainly on the relative percentages of ferrous iron and ferric iron. This great variation in the titanium dioxide content of ilmenite is due to the presence of other mineral elements in the ilmenite lattice, in the case of the lower grade materials, and to dissociation of the iron oxides by weathering, in the case of higher TiO2 grade materials.
Titanium concentrates are used in the production of both pigments and titanium metal. Titanium metal is light and resistant to corrosion. It is widely used in the aeronautic, aerospace, and chemical industries. It is also applied in sea water desalination plants, in cryogenics, and in oceanography. Titanium dioxide, on the other hand, is the basic pigment used in paint manufacture, and is also widely used in the paper and plastics industries.
The demand for rutile has greatly increased in recent years due to its growing use in pigment production. Because of its very high TiO2 content, pigments can be produced from it with only minor pollution problems. For this reason, rutile has become an expensive ore, and currently known world deposits are limited.
The recent discoveries of large bodies of anatase in complex association with other minerals in vertical reins of ore of volcanic origin in the Brazilian states of
Minas Gerais and Goias, have opened up very promising prospects for the titanium raw material industry in Brazil. However, the anatase ore recently found is quite different from other known titaniferous ores, and it occurs in association with other
TiO2 minerals such as ilmenite (FeO. TiO3), perovskite (Ca.TiO3), and titaniferous magnetite.
After being mined, the anatase ore is subjected to mechanical beneficiation resulting in concentrates with TiO2 and Fe2O3 contents of between 70% and 80% by weight and between 8% and 15% by weight respectively.
The following is a typical analysis of an anatase concentrate thus obtained, the percentages being by weight: TiO2 = 78.12% MgO = 0.84% Fe2O3 = 1.09% CaO = 0.70% SiO2 = 1.09% Mb2Os = 0.67% P2Os= 1.74% L.I. = 1.85%
Awl203= 1.04%.
It is an object of the present invention to provide a method of upgrading the above-mentioned concentrates to a very high-grade product, similar in nature to rutile and having a high TiO2 content and a low Fe2O3 content.
According to the invention, there is provided a method of producing a higher
TiO2 grade anatase concentrate from a lower grade concentrate which comprises the steps of subjecting the lower grade concentrate to a reducing treatment in the presence of gaseous SO2 and/or H2S at elevated temperature, leaching the reduction product with mineral acid, and subjecting the leached product to magnetic separation, the non-magnetic fraction being withdrawn as the desired higher grade concentrate
The reduction step in the presence of gaseous SO2 and/or H2S, may be carried out at a temperature of, for example, 500 to 13000C. The hydrogen sulphide gas given off in the acid leaching step may be recycled to the reduction step. The acid leaching step may be carried out at a temperature between ambient temperature and the boiling point of the acid used.
The magnetic separation step may be carried out in a magnetic field having a strength of between 7000 and 25000 gauss. If desired, the magnetic fraction separated in this step may be recycled to the reduction step.
If desired, the acid-leached material may be subjected to alkaline leaching to reduce the phosphorus and aluminium contents.
In a preferred embodiment of the invention, the mechanically obtained anatase concentrate is initially reduced in the presence of SO2 (sulphur dioxide gas) and/or H2S (hydrogen sulphide gas) in a rotary kiln or any other type of kiln which permits a good gas/solid contact between the reducing gas and the concentrate.
The reducing gas mixture is produced by the combustion of gases in conventional burners. The reduction is effected at a temperature in the range of 500 to 13000C.
In addition to reducing the ore, the gaseous mixture opens up the crystal lattice of the impure titaniferous ore, thus allowing the iron and other metallic ions to react and form sulphides such as iron sulphides, magnesium sulphides, and the like.
After reduction, the material is cooled in a reducing or protective atmosphere to avoid reoxidation of the reduced material. It is then treated with a mineral acid solution, such as hydrochloric acid and/or sulphuric acid, at temperatures ranging from room temperature to the boiling point of the acid solution. The optimum concentration for the acids is usually from 10 to 20% for hydrochloric acid and from 20 to 30% for sulphuric acid, but other concentrations may be used. At this point, the metal sulphides formed and other impurities are leached by the action of the acid.
The main chemical reaction involved in the process are as follows: (1) FeO.TiO2 + SO2 + 3 CO = FeS + TiO2 + 3 CO2 (2) 2FeO.TiO2 + 2H2S + 2CO = FeS + TiO2 + H2O + 2CO (3) FeO.TiO2 + H2S + FeS + TiO2 + H2O (4) Me2O3 + 3H2S = 2MeS + 3H2O + S.
Iron sulphide (FeS) produced in any of reactions (1), (2) and (3) is leached in acid solution, which results in the formation of hydrogen sulphide (H2S), which is recovered and recycled in the system, thereby reigniting the operational cycle. The chemical reactions involved in this leaching operation can be represented as follows:
FeS + TiO + 2HCI = FeCI2 + TiO2 + H2S
FeS + TiO2 + H2SO4 = FeSO4 + TiO2 + H2S.
The other impurities in the original mechanical concentrate of lower TiO2 content are also eliminated by leaching with acid solution. The equations for the chemical reactions are as follows (Me representing an impurity metal): MeS + TiO2 + 2HCl = Meal2 + TiO2 + H2S
MeS + TiO2 + H2SO4 = MeSO4 + TiO2 + H2S.
After the acid treatment, the material is filtered, washed with water, and then submitted to magnetic separation with a high field intensity. Any remaining magnetic materials are recycled, and the final non-magnetic product obtained is the required high TiO2 grade anatase concentrate. Its composition includes a minimum TiO2 content of 94% by weight and a maximum Fe2O3 content of 2% by weight, and it has characteristics similar to those of natural rutile.
Where lower phosphorus and aluminium contents are required, these can be further reduced by an additional treatment, after the acid leaching, with sodium hydroxide solutions in concentrations of up to 20% by weight, at temperatures ranging from room temperature to the boiling point of the alkaline solution depending on the specific nature of the material being treated.
The invention is illustrated by the following non-limitative experiments: EXPERIMENTAL CONDITIONS
a) SULPHIDISATION -- 25 g of a low-grade anatase concentrate with an average particle size less than 80 mesh (Tyler Specification) were placed in a quartz tube which was put in a fixed bed furnace heated by an electric resistor. After the furnace temperature had attained the prescribed level, hydrogen sulphide gas (H2S) or sulphur dioxide was passed through the tube at a gas flow rate of 240 ml/min.
The reactor tube was rotated every five minutes by a manually-driven device in order to mix and expose more of the solids surface to the passing gas. At the end of the sulphidisation process, the sulphidised material was cooled in a non-oxidising atmosphere by passing an inert gas such as argon or nitrogen, thereby preventing reoxidation. These conditions were kept constant during the tests which were carried out to determine the influences of sulphidisation temperature and reaction time.
b) ACID LEACHING -20 g of the sulphidised material were leached with 50 ml of aqueous hydrochloric acid solution having a concentration of 20% by weight (200 g of HCI per litre of solution) for 3 hours under reflux. After leaching, the material was filtered and washed until all residual HCl had been washed away.
c) MAGNETIC SEPARATION -- The solid material from the acid leaching step was submitted to wet magnetic separation with a high field intensity, resulting in two fractions, one magnetic and the other non-magnetic.
The conditions described above for sulphidisation, acid leaching, sulphidisation temperature and reaction time were studied. The results obtained are given in the following Tables, in which all percentages are by weight.
EXPERIMENTAL RESULTS
a) Influence of sulphidisation temperature: material balance and chemical analysis (sulphidisation time was kept at 45 minutes for all runs).
TABLE 1
Non-magnetic Magnetic In fraction fraction solution Sulphidi station Time g (KO) g (it) g (%) 6000C 14.72 73.60 2.71 13.55 2.57 12.85 7000C 14.70 75.50 2.52 12.60 2.78 13.90 8000C 15.35 76.75 1.50 1.50 3.15 15.75 9000C 15.65 78.25 1.09 5.45 3.26 16.13 10000C 16.10 80.50 0.60 3.00 3.30 16.50 SULPHIDISATION
Temperature 6000C 7000C 8000C 9000C 10000C TiO2 % 93.00 94.25 93.2 93.75 94.25 Fe2O3 % 1.70 1.21 0.67 0.56 0.34 SiO2 % 0.64 0.64 0.86 0.64 0.50 CaO % 0.08 0.07 0.08 0.09 0.09 P205 % 1.05 1.02 0.94 1.20 1.12 Al203 % 1.11 1.27 1.34 1.32 1.28 MgO % 0.32 0.46 0.50 0.70 0.81 b) Influence of sulphidisation reaction time: (Sulphidisation temperature was
keDt at 1.0000C).
TABLE II
NonMagnetic Magnetic In fraction fraction Solution Suiphidisation Time (g) (%) (g) (%) (g) (%) 15 mins 15.75 78.75 1.11 5.55 3.14 15.70 30 mins 16.00 60.00 0.60 3.25 3 25 16.75 45 mins 15.90 79.50 0.70 3.50 3.40 17.00 60 mins 15.52 77.60 0.54 2.70 3.94 19.70 90 mins 15.55 77.75 0.86 3.30 3.79 18.95 120 mins 15.50 77.50 0.50 2.50 4.00 20.00 In addition to the factors indicated above, the acid leaching reaction time was also investigated. For these tests, the sulphidisation temperature was kept at 1000 C and the sulphidisation time at 60 mins, with magnetic separation with a high field intensity.
c) Influence of leaching reaction time: material balance and chemical
analysis (sulphidis ation temperature: 10000C; sulphidisation time
60 mins).
TABLE III
NonMagnetic Magnetic In fraction fraction Solution Acid Leaching time (g) (%) (g) (No) (g) (%) 1 hour 16.80 84.00 0.36 1.80 2.84 14.20 2 hours 16.50 82.50 0.40 2.00 3.10 15.50 4 hours 16.04 80.20 0.39 1.95 3.57 17.85 6 hours 16.20 81.00 0.28 1.40 3.52 17.60 TABLE IIIA
Acid Leaching % Fe2O3 SiO, CaO P2O A1203 MgO Time 1 hour 97.25 0.21 0.30 0.11 0.98 1.04 0.80 2 hours 96.80 0.19 0.22 0.10 0.52 1.02 0.80 4 hours 97.25 0.19 0.26 0.05 0.53 0.94 0.78 6 6 hours 97.50 0.17 0.40 0.07 0.33 1.02 0.91 On an industrial scale, the process can be described as follows. Low-grade anatase concentrate is fed into a furnace heated directly by combustible gas burning in a conventional burner with a neutral or slightly reducing flame.The sulphidising agent is fed into the furnace, together with the anatase, in excess of the amount required by the stoichiometric reaction. The sulphidised material passes through a cooling device and is directly discharged into the acid leaching system, continuously and in counter-current. The gases from this treatment, which basically consist of H2S (hydrogen sulphide gas) are collected and, together with the excess reactant from the sulphidisation furnace, are recycled to the sulphidisation step. The leached material is filtered and submitted to wet magnetic separation with a high field intensity. The magnetic fraction is recycled to the sulphidisation furnace. The non-magnetic fraction produced is the required high
TiO2 grade anatase concentrate.
WHAT WE CLAIM IS: l. A method of producing a higher TiO2 grade anatase concentrate from a lower grade concentrate which comprises the steps of subjecting the lower grade concentrate to a reducing treatment in the presence of gaseous SO2 and/or H2S, at elevated temperature leaching the reduction product with mineral acid, and
**WARNING** end of DESC field may overlap start of CLMS **.
Claims (9)
- **WARNING** start of CLMS field may overlap end of DESC **.In addition to the factors indicated above, the acid leaching reaction time was also investigated. For these tests, the sulphidisation temperature was kept at 1000 C and the sulphidisation time at 60 mins, with magnetic separation with a high field intensity.c) Influence of leaching reaction time: material balance and chemical analysis (sulphidis ation temperature: 10000C; sulphidisation time 60 mins).TABLE IIINonMagnetic Magnetic In fraction fraction Solution Acid Leaching time (g) (%) (g) (No) (g) (%) 1 hour 16.80 84.00 0.36 1.80 2.84 14.20 2 hours 16.50 82.50 0.40 2.00 3.10 15.50 4 hours 16.04 80.20 0.39 1.95 3.57 17.85 6 hours 16.20 81.00 0.28 1.40 3.52 17.60 TABLE IIIAAcid Leaching % Fe2O3 SiO, CaO P2O A1203 MgO Time 1 hour 97.25 0.21 0.30 0.11 0.98 1.04 0.80 2 hours 96.80 0.19 0.22 0.10 0.52 1.02 0.80 4 hours 97.25 0.19 0.26 0.05 0.53 0.94 0.78 6 6 hours 97.50 0.17 0.40 0.07 0.33 1.02 0.91 On an industrial scale, the process can be described as follows. Low-grade anatase concentrate is fed into a furnace heated directly by combustible gas burning in a conventional burner with a neutral or slightly reducing flame.The sulphidising agent is fed into the furnace, together with the anatase, in excess of the amount required by the stoichiometric reaction. The sulphidised material passes through a cooling device and is directly discharged into the acid leaching system, continuously and in counter-current. The gases from this treatment, which basically consist of H2S (hydrogen sulphide gas) are collected and, together with the excess reactant from the sulphidisation furnace, are recycled to the sulphidisation step. The leached material is filtered and submitted to wet magnetic separation with a high field intensity. The magnetic fraction is recycled to the sulphidisation furnace. The non-magnetic fraction produced is the required high TiO2 grade anatase concentrate.WHAT WE CLAIM IS: l. A method of producing a higher TiO2 grade anatase concentrate from a lower grade concentrate which comprises the steps of subjecting the lower grade concentrate to a reducing treatment in the presence of gaseous SO2 and/or H2S, at elevated temperature leaching the reduction product with mineral acid, andsubjecting the leached product to magnetic separation, the non-magnetic fraction being withdrawn as the desired higher grade concentrate.
- 2. A method as claimed in Claim 1, wherein the magnetic fraction produced in the magnetic separation step is recycled to the reduction step.
- 3. A method as claimed in Claim 1 or Claim 2, wherein said reduction step is carried out at a temperature in the range of 500 to 13000C.
- 4. A method as claimed in any one of the preceding Claims, wherein hydrogen sulphide gas given off in the acid leaching step is recycled to the reduction step.
- 5. A method as claimed in any one of the preceding Claims, wherein the acid leaching step is carried out at a temperature between ambient temperature and the boiling point of the acid.
- 6. A method as claimed in any one of the preceding Claims, wherein the leached material is submitted to magnetic separation in a magnetic field of strength between 7000 and 25000 gauss.
- 7. A method as claimed in any one of the preceding Claims, wherein the acidleached material is subjected to alkaline leaching prior to magnetic separation.
- 8. A method as claimed in Claim 1, of producing a higher TiO2 grade anatase concentrate from a lower grade concentrate substantially as hereinbefore described and exemplified.
- 9. A higher TiO2 grade anatase concentrate produced from a lower grade concentrate by a method as claimed in any one of the preceding Claims.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BR7701443 | 1977-03-09 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1568333A true GB1568333A (en) | 1980-05-29 |
Family
ID=4004101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8896/78A Expired GB1568333A (en) | 1977-03-09 | 1978-03-07 | Method for obtaining higher tio2 grade anatase concentrates from lower tio2 grade anatase concentrates |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JPS53127398A (en) |
| AU (1) | AU515999B2 (en) |
| FR (1) | FR2383127A1 (en) |
| GB (1) | GB1568333A (en) |
| NL (1) | NL7802201A (en) |
| ZA (1) | ZA781126B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5885536A (en) * | 1994-04-15 | 1999-03-23 | Technological Resources Pty Ltd | Process for alkaline leaching a titaniferous material |
| WO2005042405A1 (en) * | 2003-10-28 | 2005-05-12 | Companhia Vale Do Rio Doce | A PROCESS TO OBTAIN TITANIUM CONCENTRATES WITH HIGH CONTENTS OF TiO2 AND LOW CONTENTS OF RADIONUCLIDE ELEMENTS FROM ANATASE MECHANICAL CONCENTRATES |
| RU2453618C2 (en) * | 2010-05-11 | 2012-06-20 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Method for processing oil containing leucoxene flotation concentrate for producing rutile |
| RU2586190C1 (en) * | 2014-12-17 | 2016-06-10 | Федеральное государственное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for processing leucoxene concentrate and device therefor |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3924796A1 (en) * | 1989-07-27 | 1991-01-31 | Metallgesellschaft Ag | GAINING TIO (ARROW DOWN) 2 (ARROW DOWN) CONCENTRATES FROM TIO (ARROW DOWN) 2 (ARROW ABLE) CONTAINING SUBSTANCES |
| AU649441B2 (en) * | 1990-08-30 | 1994-05-26 | Almeth Pty Ltd | Improved process for separating ilmenite |
| CA2162266A1 (en) * | 1993-05-07 | 1994-11-24 | Michael John Hollitt | Process for upgrading titaniferous materials |
| ZA946864B (en) * | 1993-09-07 | 1995-09-04 | Tech Resources Pty Ltd | Upgrading titaniferous materials. |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3446590A (en) * | 1966-10-21 | 1969-05-27 | Nat Lead Co | Titanium dioxide concentrate and method for producing the same |
| CA923711A (en) * | 1969-09-12 | 1973-04-03 | Ishihara Sangyo Kaisha | Titanium dioxide concentrate and its manufacturing process |
| JPS5025499A (en) * | 1973-07-10 | 1975-03-18 | ||
| BR7604610A (en) * | 1976-03-12 | 1977-11-29 | A Lakschevitz Jr | PROCESS OF OBTAINING HIGH TIO2 ANATASIO CONCENTRATES FROM CONCENTRATES WITH HIGH TIO I CONCENTRATES FROM CONCENTRATES WITH LOWEST TIO I AND LOWER TIO2 |
-
1978
- 1978-02-27 ZA ZA00781126A patent/ZA781126B/en unknown
- 1978-02-28 NL NL7802201A patent/NL7802201A/en not_active Application Discontinuation
- 1978-03-07 JP JP2505078A patent/JPS53127398A/en active Pending
- 1978-03-07 GB GB8896/78A patent/GB1568333A/en not_active Expired
- 1978-03-08 FR FR7806691A patent/FR2383127A1/en active Granted
- 1978-03-09 AU AU34034/78A patent/AU515999B2/en not_active Expired
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5885536A (en) * | 1994-04-15 | 1999-03-23 | Technological Resources Pty Ltd | Process for alkaline leaching a titaniferous material |
| WO2005042405A1 (en) * | 2003-10-28 | 2005-05-12 | Companhia Vale Do Rio Doce | A PROCESS TO OBTAIN TITANIUM CONCENTRATES WITH HIGH CONTENTS OF TiO2 AND LOW CONTENTS OF RADIONUCLIDE ELEMENTS FROM ANATASE MECHANICAL CONCENTRATES |
| NO20062411L (en) * | 2003-10-28 | 2006-05-26 | Vale Sa | Process for obtaining high content of TiO2 and low content of radionuclide titanium concentrates from mechanical anatase concentrates |
| GB2422146A (en) * | 2003-10-28 | 2006-07-19 | Vale Do Rio Doce Co | A process to obtain titanium concentrates with high contents of tio2 and low contents of radionuclide elements from anatase mechanical concentrates |
| GB2422146B (en) * | 2003-10-28 | 2008-12-03 | Vale Do Rio Doce Co | A process to obtain titanium concentrates with high contents of TiO2 and low contents of radionuclide elements from anatase mechanical concentrates |
| AU2004284956B2 (en) * | 2003-10-28 | 2009-03-12 | Vale S.A. | A process to obtain titanium concentrates with high contents of TiO2 and low contents of radionuclide elements from anatase mechanical concentrates |
| US7572418B2 (en) | 2003-10-28 | 2009-08-11 | Companhia Vale Do Rio Doce | Process to obtain titanium concentrates with high contents of TiO2 and low contents of radionuclide elements from anatase mechanical concentrates |
| NO342486B1 (en) * | 2003-10-28 | 2018-05-28 | Vale Sa | Process for obtaining high content of TiO2 and low content of radionuclide titanium concentrates from mechanical anatase concentrates |
| RU2453618C2 (en) * | 2010-05-11 | 2012-06-20 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Method for processing oil containing leucoxene flotation concentrate for producing rutile |
| RU2586190C1 (en) * | 2014-12-17 | 2016-06-10 | Федеральное государственное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for processing leucoxene concentrate and device therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2383127B1 (en) | 1984-12-28 |
| NL7802201A (en) | 1978-09-12 |
| FR2383127A1 (en) | 1978-10-06 |
| ZA781126B (en) | 1979-01-31 |
| AU3403478A (en) | 1979-09-13 |
| AU515999B2 (en) | 1981-05-14 |
| JPS53127398A (en) | 1978-11-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3903239A (en) | Recovery of titanium dioxide from ores | |
| US3252787A (en) | Process for producing titanium dioxide concentrate and other useful products from ilmenite and similar ores | |
| US6699446B2 (en) | Methods for separation of titanium from ore | |
| US3597189A (en) | Process for the beneficiation of titaniferous ores | |
| Middlemas et al. | A new method for production of titanium dioxide pigment | |
| US4085190A (en) | Production of rutile from ilmenite | |
| BR112017018902B1 (en) | PROCESS | |
| US4019898A (en) | Beneficiation of ilmenite ore | |
| US4176159A (en) | Process for concentration of titanium containing anatase ore | |
| GB1568333A (en) | Method for obtaining higher tio2 grade anatase concentrates from lower tio2 grade anatase concentrates | |
| NZ199484A (en) | Benefication of titaniferous materials | |
| Kothari | Recent developments in processing ilmenite for titanium | |
| EP0014806B1 (en) | Processing of chromium ore | |
| US3875286A (en) | Beneficiation of ilmenite ores | |
| US3897537A (en) | Beneficiation of ilmenite ores | |
| US6803024B1 (en) | Benefication of titania slag by oxidation and reduction treatment | |
| CZ291224B6 (en) | Production process of titanium oxide | |
| US3627508A (en) | Process of beneficiation | |
| US3554733A (en) | Process obtaining sulfurous gases and magnetite or iron sponge from waste ferrous sulfate | |
| Lakshmanan et al. | Innovative process for the production of titanium dioxide | |
| Henn et al. | A review of proposed processes for making rutile substitutes | |
| US1902203A (en) | Process of preparing titanium dioxide | |
| US2381565A (en) | Chromium recovery | |
| Stambaugh | Hydrothermal processing—An emerging technology | |
| EP0869194B1 (en) | Process for preparing titanium dioxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed [section 19, patents act 1949] | ||
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 19930307 |