Method for processing oil containing leucoxene flotation concentrate for producing rutile

FIELD: metallurgy.

SUBSTANCE: method involves distillation of the oil fraction in an inert gas atmosphere, milling and reducing roasting of the mineral residue by petcoke. Then milling and sulphatisation of titanium cinder are performed with oleum and leaching of titanium-containing compounds with water.

EFFECT: increased chemical reactivity of the concentrate, elevated levels of anosovite phase in the concentrate, increasing increase cost-effectiveness activity of the process through utilisation of the oil fraction and absence of additional consumption of a reducing agent during roasting, reducing of environmental hazard due to decrease in temperature of recovery roasting and sulphatisation.

4 cl, 2 tbl, 1 ex


The invention relates to the metallurgy of rare and scattered metals, and in particular to methods of processing refractory concentrates, in particular leucoxene flotation concentrates, which are the product of the enrichment of oil-bearing silicon-titanium ores used to obtain synthetic rutile feedstock for the production of titanium chloride method and pigment titanium dioxide.

The technology for producing synthetic rutile from quartz-leucoxene concentrates composition, %: 56,3-59,6 TiO2; 28,7-31,5 SiO2; 0,7-1,1 Fe2O3; 2,8-3,9 FeO; 2,4-4,5 Al2O3; 0,2-0,3 CaO; 0,8-1 MgO; 0.05 to 0.15 MnO is relevant, since domestic and foreign markets demand high quality titanium mineral concentrates (mainly rutile), necessary for the production of titanium pigments, metallic titanium, titanium alloys and welding electrodes.

Known pyrometallurgical methods [1, 2] for producing synthetic rutile from ilmenite is not applicable in case of use of leucoxene concentrate due to thin mutual germination with rutile quartz, reaching 2-3 microns: the prevailing mass of grains leucoxene greenish-gray color on the outside covered with shirts or rims of fine-grained chlorite-quartz unit, in places containing siderite; inside the grains lacosse who have inclusions (several microns) quartz or pyrite.

The known method alkaline autoclave leaching fired at 900-1000°C flotation concentrate with getting rich in titanium products, %: 71-80 TiO2, 12-2 SiO2[3]. When performing additional processing of concentrate hydrochloric acid and subsequent refinement at the liner can improve the content of TiO2it up to 80-85%.

The disadvantages of this method are: the need for additional surgery (acid leaching); significant consumption of alkaline reagent (alkali, soda) and large amounts of alkaline solutions (5-6 m31 t TiO3) with a high content of SiO2(~110 g/DM3), not allowing to dispose of these solutions (e.g., deposition CaSiO3with the regeneration of the used alkaline reagent.

A method of obtaining of titanium dioxide pigment from leucoxene concentrates composition, %: 45-50 TiO3; 40-45 SiO2; 1,5-3 Fe(General)for sulfuric acid technologies, including regenerative firing at a temperature of 1200-1350°C for 20-150 min, grinding roasted concentrate to a particle size of 0.075 mm, mixing with concentrated sulfuric acid, then heated to 200°C and holding at that temperature for 1.5 hours, cooled and leached with water [4].

The disadvantages of this method include the big e is arguemnet, environmental hazard high temperature process sulfatization, the use of sophisticated technological equipment.

Closest to the claimed invention to the technical essence and the achieved result is a method for processing oily leucoxene concentrates, obtained during the concentration of silicon-titanium ores Yarega field, including the firing of the flotation concentrate in the presence of additives, cooling, grinding and beneficiation by separating grains of titanium oxide from silicates physico-chemical and/or mechanical methods [5]. Prior to firing the oil-titanous lanoxinbuy flotation concentrate is mixed with fuel sorption-active additives for the release of oil from the flotation concentrate. The firing is carried out by filtration combustion mode sverkhadiabaticheskoe heat in the reactor shaft. As inert additives use a circulating solid modifying additives in the form of refractory materials. The firing temperature in the combustion zone maintained within the range of 900-1300°C by regulating the mass fractions loaded into the reactor combustible and non-combustible material and oxygen, supplied with gas-oxidant. The technical result is to increase the chemical activity (scrivetemi) concentrate, increased levels of rutile phase to which centrate, increase the profitability of the process by obtaining and using the product gas for heat, electricity and own technological needs. The method adopted for the prototype.

With essential features of the invention match the following set of features: a method of processing titanium containing concentrates to obtain rutile, including regenerative firing leucoxene concentrates, further cooling, grinding and sulfatization burnt concentrates upon heating and subsequent leaching water sulfatizing cinder.

The disadvantages of this method are: irreversible loss of oil from oily concentrate due to her deep burning; use for roasting sophisticated technological equipment - reactor shaft type with different temperature zones (heating, drying, pyrolysis, combustion, cooling); high energy intensity of the process.

Technical problem solved by the claimed invention is a processing flotation of quartz-leucoxene concentrates in order to obtain synthetic rutile by extracting oil from netsolitaire titanium-silicon of leucoxene flotation concentrate, preparing for the more effective the further enrichment of titanium-silicon concentrate due to the implementation blugaria the different physico-chemical, mechanical and phase transformations inside concentrate under optimum conditions of the process of its reduction roast, sulfatization and leaching.

Technical results of the claimed invention are:

- increase the profitability of the refining process of flotation concentrates by extracting the oil in a separate faction;

the increased chemical activity (scrivetemi) by increasing the content of phase anosovite in quartz-leucoxene concentrates;

- no additional consumption of reducing agent during firing;

- reduce environmental hazards reduce the firing temperature of the mineral residue and sulfatization titanium containing calcine.

The technical result is achieved by a method for processing oil-titanous leucoxene concentrates to obtain rutile includes sublimation of the oil fraction in an inert gas (argon) at a temperature of 800°C and cooling the titanium-silicon concentrates, as well as the further reduction and recovery annealing the titanium-silicon concentrates at a temperature of 1100-1150°C for 50-60 minutes, cooling, grinding and sulfatization cinder with oleum at a temperature of 150°C for 50-60 min, cooling sulfatizing cinder and leaching of sulfate titanium water at a temperature of 90-95°C for 50-60 minutes

About the Eden applicant's analysis of the prior art, including searching by the patent and scientific and technical information sources and identify sources that contain information about the equivalents of the claimed invention, has allowed to establish that the applicant had not found the source, which is characterized by signs, identical all the essential features of the invention. The definition from the list of identified unique prototype as the most similar set of features analogue has allowed to establish the essential towards perceived by the applicant to the technical result of the distinctive features set forth in the claims. Therefore, the claimed invention meets the criterion of "novelty".

The inventive method of processing oil-titanous of leucoxene flotation concentrate to obtain rutile meets all the criteria of patentability.

Offer for patent protection an invention involves an inventive step, because its essence for professionals engaged in the metallurgy of rare and scattered metals, is not obvious from the prior art, i.e. not identified solutions that have the signs consistent with the distinctive features of the proposed method, and thus cannot be confirmed fame distinctive characteristics specified by the applicant, the technical result.

The home is jaimoe the invention is industrially applicable, because it can be used in production for its intended purpose, i.e. for the processing of such concentrates. No sign, taken separately, neither the totality of the features of the process does not contradict the possibility of their application in industry and does not impede the achievement perceived by the applicant of the technical result.

An example implementation of the method

Processing was subjected to the oily lanoxinbuy flotation concentrate to obtain rutile coming from the concentrator, in the form of a slurry of the following composition, wt.%: 46,6 - leucoxene concentrate (mineral phase); 21,7 - oil (organic phase); 31,7 is water.

For the normal process of sublimation of oil it is necessary that the moisture content of the flotation concentrate (68,2% mineral and 31.8% of organic phase) did not exceed 1.5-2 wt.%, why pulp defended, decantation water, and the solid phase was dried to the desired moisture level.

Sublimation of the crude oil (100%) spent in a metal reactor, the heated gas-burning devices, at a temperature of 800°C for 50-60 minutes in an atmosphere of inert gas (argon). The condensation of the gaseous products of sublimation was performed using the refrigerator at a temperature of 20°C. were obtained condensed fraction oil (81.5%), Neftegas (15.1%) in the composition of mineral OST the TKA and irreversible losses neskondensirovannyh gaseous component (3,4%).

Mineral titanium containing the remainder of the composition in %: 39,6 TiO2(24 Ti); 41,1 SiO2; 1,75 Fetotal; Stotal1,1; Ctotal5; CTV4,8, grinded by ball mill with peripheral discharge particle size up to -2 mm

The number of Neftekamsk (4.8 per cent) in the composition of the mineral titanium containing residue after distillation of oil is enough for remediation of firing in an inclined rotary kiln, which allows you to destroy the higher oxide rutile (TiO2) to more soluble lower oxide anosovite (Ti3O5), the lattice of which, being defective, and is more reactive, total responses:




Solid translation of the higher oxides of titanium in the lower (degree of decomposition of rutile γ=94,5-99%) occurs in the claimed method at lower temperatures (t=1100-1150°C) and over a shorter period of time (τ=50-60 min), compared with the prototype (t=1200-1350°C; τ=20-150 min) (table 1).

Table 1
Indicators of the recovery process rutile
Firing temperature, °/td> The content of TiO2/The degree of decomposition of TiO2, %
Flotation concentrate (τ=0,85-1 h)Charge (τ=2-2,5 h)

This result is achieved due to the presence on the surface of the titanium containing mineral balance of chemisorbed Neftekamsk from the primary oil fractions, selectively adsorbiruya on the surface of leucoxene concentrate and reduce its reactivity with flotation processing of the original quartz-lanoxinbuy ore composition, %: 90-93 mineral phase (Sandstone), including 16.3 lanoxin; 8.4 siderite; 75,3 quartz; 7-10 organic phase (oil).

Received such a cinder grinded article is renewal mill with peripheral discharge particle size up - 0.1 mm, was mixed with oleum (SO3≥19%) at T:W=1:(1-10), the slurry was heated to 150 C. and maintained for about 50-60 min in a sealed insulated apparatus, equipped with a stirrer, heating systems and gas recovery (SO2, SO3, water vapor) (table 2).

For sulfatization of anosovite ([Ti3O5]m·[SO3]n), restored from rutile, in the present method used oleum (GOST 2184-77) instead of concentrated sulfuric acid used in the prototype.

The presence of oleum 19-24% of free sulfur dioxide (SO3) helped to reduce the temperature and duration of the process of sulfatization of anosovite in the present method (t=150°C; τ=50-60 min) compared with the prototype (t=180-200°C; τ=90-120 min).

When chemically treated titanium containing calcine additionally there is a destruction of the structure of silicates and education of their individual fine fraction, which facilitates cleaning of grains anosovite from intergrowths.

After cooling, the slurry is leached sulfate titanium water at T:W=1:(1-10) for 50-60 minutes at a temperature of 90-95°C (table 2).

Table 2
The exponents of sulfatization of anosovite (α) oleum and sulfuric acid and the above is Oceania sulfate titanium (β) water
The ratio of T:Wα/β, %
Oleum (tc=150°C, twith=1 h)Sulphuric acid (tc=200°C, τc=2 h)

The degree of extraction of titanium is not less, %: 99 - in solution; 98 - of leucoxene flotation concentrate.

On the basis of the conducted research we can conclude that the aggregate of the stated characteristics are provided by the achievement of the technical result, namely the most effective decomposition of oily leucoxene concentrate to obtain rutile with high extraction of titanium sulfate in solution.

Thus, the inventive method allows re what s the most important technical challenges in the processing of oily flotation concentrates to obtain rutile:

- to increase the profitability of the process by separating the oil in the form of individual fractions suitable for further processing in refineries;

to increase the chemical activity (skrivemate) due to the transfer of rutile phase anosovite in quartz-leucoxene concentrates the reductive roasting;

- to refuse additional consumption of reducing agent during firing;

in the process of sulfatization additionally to destroy the structure of silicates and clean grain anosovite from splices;

to reduce the temperature, duration and, consequently, the degree of environmental hazards with sulfatization titanium containing calcine.


1. Elger G.W., D.E. Kirby and Rhoads S.C. Producing Synthetic Rudle from Ilmenite by Pyrometallurgy Pilot Plan Stadies and economic Evaluadon / Rept. Invest Bur. Mines U.S. Dep. Inter., 1976.

2. Titanium / Under redviagra. M.: metallurgy, 1983. S.

3. Fedorov mathematical SCIENCES. Chemical finishing of titanium concentrate by autoclave leaching of the silicic acid. In kN. Titanium and its alloys, B.9. M.: Izd-vo an SSSR, 1963. P.36-41.

4. Pat. 2001138 (RF). The method of processing of leucoxene concentrate / Lugulake, Amerenue, Nautolan and others, 1991.

5. Pat. 2334799 (RF). A method of processing oil-titanous leucoxene concentrates / Averagin, Tan, Howardson and others 2007.

1. A method of processing netsolitaire of leucoxene fotokasten the rata to obtain rutile, including restorative roasting, grinding, sulfatization, decomposition and leaching, wherein the pre-distilled oil fraction in the atmosphere of inert gas at a temperature of 800°C for 50-60 minutes, if sulfatization use oleum containing 19-24% of free sulfur dioxide (SO3) at a temperature of 150°C for 50-60 minutes

2. The method according to claim 1, characterized in that as the reductant, the firing of use Neftegas after the distillation of a petroleum fraction.

3. The method according to claim 1, characterized in that the recovery annealing is carried out at a temperature of 1100-1150°C for 50-60 minutes

4. The method according to claim 1, characterized in that the leaching is carried out with water at T:W=1:5 for 50-60 minutes at a temperature of 90-95°C.


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