The method of processing of such raw materials

 

(57) Abstract:

The invention relates to the processing of such raw materials, the products of which will be used to obtain finely dispersed titanium and micaceous iron pigments. The pigments used in paint, ceramic, construction, leather and paper industries. The invention consists in the method of processing of such raw materials. The method is based on the fusion of such concentrates with hydrovhloride ammonium subsequent water leaching SPECA, Department of precipitated at pH 7-8 salts perferated ammonium and crystallization of the purified from iron solution hexafluorotitanate ammonium. The technical result of the method is to improve the quality of basic commodity products (micaceous iron and titanium pigments), the lower energy process and simplifying the processing of ilmenite feedstock. 4 C.p. f-crystals.

The invention relates to the technology of processing of mineral raw materials, in particular to the processing of ilmenite raw materials with the aim of obtaining titanium and micaceous iron pigments.

The opening of ilmenite feedstock carried out in various ways, however, know the e effective process compared to treatment with sulfuric, hydrochloric or nitric acids (R. K. Biswas, M. G. K. Mondal. Hydrometallurgy., 1987, N 17, p. 385 - 390).

A known method for the production of titanium pigment containing 99.9% of TiO2and of 0.004% Fe, including the processing of ilmenite by the HF solution, the precipitation of titanium compounds and iron NaOH solution, dissolution of the solid residue with hydrochloric acid 7.5 M, two-phase extraction of Fe(III) mixture, extraction of titanium 2-ethylhexylamine acid, it is extracted from the organic phase with 0.5 M Na2CO3and subsequent annealing to TiO2when 1000oC. (R. K. Biswas, M. C. Habib, N. C. Dafadev. Hydrometallurgy., 1992, N 28, p. 119 - 126).

However, this method is unnecessarily complicated, expensive, requiring a large number of reagents, which must be regenerated.

Use for opening the titanium raw material hydrovhloride ammonium (NH4HF2) significantly simplifies the processing circuit (N. C. Cabeldu, J. H. Moss, A. Wright. Proc. Conf. High Temperature Chemistly of Inorganic and Ceramic Materials (Keeic, 1976) London, 1977, p. 154).

Closest to the claimed is a method of processing titanium containing minerals, including fluoridation of raw materials by sintering it with hydrovhloride of ammonia in the ratio of 95 - 117 wt.% from stagione is shonky, pyrohydrolysis foraminifera complex titanium with obtaining titanium dioxide. Remaining after sublimation of titanium sludge hydrolyzing at 800 - 840oC with getting "doped" iron oxide (p. RF N 2058408, publ. 20.04.96).

Thus obtained titanium dioxide is contaminated with iron, as the iron content in the feedstock 25% and more difficult to prevent pylones fine fluorides of iron at the stage of sublimation. In addition, since the iron oxide obtained by pyrohydrolysis, dirty along with other impurities fluorides of calcium and magnesium, which are not subject to hydrolysis in the specified temperature range, it cannot be used as micaceous iron pigment of high purity. The main stage of the process - the stage of sublimation is energy-intensive and complex process involving decomposition of herocomplex titanium and iron, which leads to the excretion of ammonia. The liberated ammonia is partially restored with titanium tetravalent to trivalent, which is painted in the color purple, which degrades the quality of the final product TiO2. In addition, at the stage of sublimation in the gas phase gets volatile compound of vanadium, so that its content in wasgone e - to improve the quality of basic commodity products - titanium and micaceous iron pigments, to reduce the energy intensity of the process and to simplify the processing of ilmenite raw materials.

The problem is solved by the proposed method for processing titanium containing materials, in which after fluoridation source of raw materials by sintering with hydrovhloride ammonium formed sintered leached with water at T: W = 1: (2-4), unreacted raw materials return to the stage of sintering, and the resulting solution was decanted, separating the precipitate formed complex compounds of fluorides of iron from solution, the pH is then adjusted to 7-8 appearing at this precipitate perferate ammonia is separated and the remaining solution crystallized hexafluorotitanate ammonium.

The method is as follows.

The original ilmenite concentrate is mixed with hydrovhloride ammonium (NH4HF2) in a mass ratio close to the stoichiometric (95-117%, as in the prototype), and heated to 150 - 200oC. the Fluorination of ilmenite is described by the equation:

FeTiO3+ (3,5+x)NH4HF2+ { (x+2)/4} O2---> (NH4TiF7+ (NH4)xFeF2x+0,5 NH3+ (2+x/2)H2O
oC yields a red-brown pigment - Fe2O3.

The ratio of T : W > 1 : 2 leads to saturation of the solution and premature precipitation of the crystals (NH4)2TiF6and T : W < 1 : 4 leads to wasted water and increase the time the subsequent crystallization of hexafluorotitanate ammonium.

In the solution after decanting, add ammonium hydroxide to pH 7-8 with the aim of decreasing the solubility foraminifera complex of iron (NH4)xFeF2x(2 < x 3), which in these conditions, the precipitates.

The claimed pH interval is determined by the need for the most complete selection of iron from solution. At pH < 7 increases the solubility formoney iron complexes, which subsequently leads to contamination of titanium dioxide, and at a pH > 8 leads to the formation of exitronix titanium which precipitates, which in turn leads to losses of titanium dioxide and pollution of iron oxide.

To raise pH, it is advisable to use formed during the fluorination of ammonium hydroxide.

Dropped after this operation sieges who agree hexafluorotitanate ammonium (NH4)2TiF6the iron content of which is not more than 110-1wt.%. The number of the resulting (NH4)2TiF6approximately 30% of the contained in the solution. In the remaining mother liquor make the next portion is released from the iron solution hexafluorotitanate ammonium and again subjected to crystallization. Thus, the proposed process is a continuous, excluding losses titanium.

To further reduce the iron content in the final product are recrystallization (NH4)2TiF6in the presence of ammonium carbonate, which reduces the level of iron content in crystals up to 3 510-3wt.%.

Obtained by the proposed method hexafluorotitanate ammonium is then processed by known methods on TiO2for example, by pyrohydrolysis, as in the prototype.

The precipitation of the complex fluoride iron (NH4)xFeF2x(2 < x 3), treated with a solution of ammonium carbonate, allows you to get the orange oxyhydroxide iron - FeOOH, which has a high pigment properties (G. F. white, I. C. Riskin. "Chemistry and technology of pigments". Leningrad: Khimiya, 1974. S. 370).

The concentration of the solution the carb is hexafluorotitanate ammonium, does not affect the final result of the operations and is determined only by the need to maintain a minimum degree of dilution of the solutions. Therefore, the amount of ammonium carbonate for carrying out these processes as a minimum should be two times the stoichiometric required

Thus, the inventive method of processing ilmenite raw materials can significantly reduce the content of impurities in the final titanium product as impurities such as, for example, vanadium, non-clogging single crystalline precipitate hexafluorotitanate ammonium, as in the processing or remain in the sediment of peroperative ammonium, which does not affect the quality of micaceous iron pigments, either in solution after recrystallization of hexafluorotitanate ammonium. The absence of such energy-intensive stages as sublimation and sublimation leads to simplification of the method and significant gains in energetic consumption.

The content of iron and titanium determine the atomic absorption method on the device.

An example of performing the method.

30 g of ilmenite concentrate containing (wt. %) 28,2 Ti and 31.0 Fe, mixed with 66 g of NH4HF2placed in stilografica glass 0.5 l and nahrawess fluoridation water vapor and ammonia. Hot speck pour 350 ml of water (T:F = 1:3.5), and with stirring, poured a cloudy solution in a glass, with heavy particles of unreacted ilmenite (m=1,9 g) settle to the bottom. The precipitate is washed by adding 50 ml of water. A cloudy solution advocated separating the precipitate fluoride compounds iron (NH4FeF3+ (NH4)xFeF2x), the mass of which is 26.7,

The resulting product is placed in an oven heated to 400oC with simultaneous transmission of water vapor. Formed 9.5 g of red-brown Fe2O3.

In the solution after separation of the main part of iron, containing 20 mg/ml of Ti and 1.8 mg/ml Fe, add 6 ml of 25% solution of NH4OH to pH 8. The solution is left to stand for evaporation. Formed transparent single crystals of (NH4)xFeF2x. Treating the crystals with a solution of ammonium carbonate (40 g/l), receive a fine orange powder oxyhydroxide iron - FeOOH.

The solution, freed from the iron and containing hexafluorotitanate ammonium slowly evaporated by half and separate the precipitation (NH4)2TiF6weighing 9 grams, containing 0.1% Fe. Recrystallization of the resulting sludge from the aqueous solution reduces the content of jer>% iron.

1. A method of processing titanium containing materials, including fluoridation materials by sintering it with hydrovhloride ammonium, wherein after sintering is conducted leaching SPECA water at T:W=1(2-4), the resulting solution was decanted, separating the precipitate of the complex fluorides of iron from solution, then the pH of the solution was adjusted to 7-8 appearing at this precipitate perferate ammonia is separated and the remaining solution crystallized hexafluorotitanate ammonium.

2. The method according to p. 1, characterized in that for the deposition of perferate ammonium use the ammonia released at the stage of sintering.

3. The method according to p. 1, characterized in that the precipitate of perferate ammonium are pyrohydrolysis at 300-400oC.

4. The method according to p. 1, characterized in that the precipitate of perferate ammonium treated with a solution of ammonium carbonate.

5. The method according to p. 1, characterized in that the precipitate of hexafluorotitanate ammonium treated with a solution of ammonium carbonate.

 

Same patents:

The invention relates to the chemical industry and can be used in the manufacture of dyes for inks, plates, ink and paper

The invention relates to the production of titanium dioxide pigment

The invention relates to a method of obtaining titanium dioxide and products on its basis

The invention relates to a method of surface treatment of the pigment of titanium dioxide and pigment of titanium dioxide

The invention relates to a method for producing pigmentary titanium dioxide from titanium containing waste, which can be used in the manufacture of paints and as a component for creating white

The invention relates to the production of pearlescent pigments based on mica flakes, flake graphite, etc., used for the manufacture of wall-paper, plastics, and paint, textile, etc

The invention relates to pigment rutelinae titanium dioxide, the method of its production and can be used in the production of paints, plastics and laminated plates on a paper basis

The invention relates to a technology of inorganic pigments, in particular pearlescent pigment used in the paint industry, in the manufacture of decorative plastic film materials, cosmetics, etc

The invention relates to chemical technology of inorganic substances, in particular to the technology of such products used in the leather industry, in the manufacture of plastics, paints, paper, etc

The invention relates to chemically-treated inorganic dyes - pigments suitable for use in thermoplastic resins

The invention relates to the technology of production of iron oxide pigments used as colorants

The invention relates to the production of highly resistant inorganic pigments that can be used for coloring plastics, rubber, natural and artificial leather, manufacture of paints and varnishes, as well as decoration of building ceramics, etc

The invention relates to the production of highly resistant inorganic pigments that can be used for coloring plastics, rubber, natural and artificial leather, manufacture of paints and varnishes, etc

The invention relates to the production of inorganic, in particular iron oxide pigments used for the production of paints, enamels for painting plastics of all types, as well as linoleum, paper, etc

The invention relates to the field of technology for inorganic pigments and can be used to obtain shell micaceous iron pigment

The invention relates to the field of technology for inorganic pigments and can be used to obtain inorganic iron-containing modified pigment

The invention relates to a method for brown phosphate of iron oxide pigment

The invention relates to chemical technology of inorganic substances, in particular, to a technology of such products used in leather, paint industry, paper manufacturing, cosmetics and so on

The invention relates to the powder of the complex metal oxide containing at least two metal element, which is used as a starting powder of an oxide ceramic, which is used as a functional material for structural material, which is used in dispergirovannom state as a filler or pigment, or used as a source of powder to obtain a single crystal or coating applied by the method of flame spraying, and the method of its production
Up!