A method of processing stanovova concentrate

 

(57) Abstract:

Usage: processing of such raw materials, in particular of sphene, technology titanium containing products used in the leather industry, in the manufacture of plastics, paints, paper. The inventive decomposition stanovova concentrate lead in the presence of aluminum oxide, which is injected in the amount of 8 - 15% Al2O3to the weight of the concentrate. Crystallization of titanium containing product from the liquid phase is carried out by adding a liquid phase in a solution of ammonium sulfate to ensure the weight ratio of sulfuric acid to ammonium sulfate is 1:0.4 to 0.6, with obtaining a titanium aluminum product. The solid residue is treated with lime milk to a residual content of aluminum in a solution of 0.5 - 2.0 g/l on Al2O3. Separating the treated residue and recycle it in a known manner with the receipt of the pigment composition. table 2.

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.

Know the 10 hours from the receipt of such SPECA, which is subjected to leaching in three stages with obtaining titanium containing solution from which, after preliminary additives lime milk by the method of thermal hydrolysis produce a residue consisting of calcium sulfate and titanium hydroxide. Sludge calcined at 850oC, and it goes in pigment composition approximate composition CaSO4:TiO265:35%

Of calcium-silicate residue after leaching sulfuric acid SPECA) when the ignition turns beige filling material used for the production of plastics, and oil paints bright colors.

Extract (degree of decomposition) of the main component (titanium) from sphene is 92 on TiO2the extraction of titanium at the stage of thermal hydrolysis - 92% of the Total extraction of titanium in titanically pigment and filler 87% of the duration of the main stages 47 h (Reel D. L. Maksimov, K. Sphene and chemical processing of titanium pigments. L. Science, 1983, 88 C.). The described method is characterized by a low degree of extraction of titanium, long, end products of titanium-calcium pigment and calciumsilicate filler used to prepare paint materials used for the internal concentration of 950 to 1100 g/l H2SO4when heated suspension and aging it at a temperature of 130 155oC for 1 to 4.0 hours Then filtered to separate the solid residue from the liquid phase (titanium-containing solution) by the method of crystallization at a temperature of 130 155oC, isolated precipitate, which is a titanylsulphate monohydrate TiOSO4H2O; the latter is dissolved in water at 60 - 90oC for 1 to 4 h, the solution is subjected to thermohydraulic in the presence of "germs". Thermal hydrolysis is carried out in the mode of boiling for 5 h with dilution of the suspension with water after 2.5 to 3 hours from the beginning of the boil. Hydroxide titanium precipitate was separated from the liquid phase, washed with water at T:W 1: 4. The washed precipitate Rasulova in water to a concentration of TiO2300 g/l, add in relation to the TiO2, rutilius embryos of 1.5 (TiO2), zinc sulfate 1,0 (ZnO), potash 0,3 (K2O), stirred for 0.5 h, filtered, the residue is calcined at 850oC content in the final product of rutile at least 95% of the Properties of this pigment: bleaching ability 1700 srvc.ed. white 97,0 srvc.ed.

The degree of extraction of titanium in the liquid phase decomposition stanovova concentrate in the known method is on average 88% recovery of titanium from the solution by tuoba characterized by a low degree of decomposition of sphene, and due to this the inability to use calcium-silicate residue to obtain a filling material (the presence of a significant number of unopened dark-coloured particles sphene) without additional processing by hindered (A. S. N 1331828, class C 01 G 23/00, C 09 C 1/36, BI N31, 1987).

The invention is directed to solving the problem of increasing the decomposition rate of the concentrate and produce new kinds of scarce titanium-containing products - titanomagnievoe of leather tanning agent and pigment composition with a high performance paint performance.

The solution of this problem is achieved in that in the method of processing stanovova concentrate, including the decomposition of concentrate sulfuric acid when heated, the separation of the solid residue and crystallization of titanium containing product from the liquid phase, the decomposition of lead concentrate in the presence of hydrated aluminum oxide, which is injected in the amount of 8 to 15% Al2O3to the weight of the concentrate, the crystallization is carried out by adding a liquid phase in a solution of ammonium sulfate to ensure the weight ratio of sulfuric acid to ammonium sulfate is 1:0,4 0,6, obtaining titanomagnievoe product, and solid UB>3separating the treated residue and recycle it in a known manner with the receipt of the pigment composition.

Decomposition concentrate at the rate of hydrated aluminum oxide less than 8% Al2O3reduce the degree of extraction of titanium from stanovova concentrate in the liquid phase and at a rate higher than 15% on Al2O3the degree of extraction of titanium in the liquid phase decreases drastically due to the loss of stability. Consumption of titanium-aluminum complex of ammonium sulfate is less than 0.4 century p.m. to 1 century including sulfuric acid by crystallization reduces tanning properties titanomagnievoe product (temperature welding), more than 0.6 century, including tanning properties practically no effect. To achieve a residual aluminum content in the solution is less than 0.5 g/l Al2O3requires a considerable excess of milk of lime, which adversely affects the properties of the resulting pigment composition. Significantly reduced the opacity at a residual aluminum content of more than 2.0 g/l Al2O3decreases the extraction of titanium and aluminum pigment composition.

The method is as follows. Stanovy concentrate loaded with stirring heated to 1 the m is increased to 140 145oC 1 3 h after reaching the specified temperature, the suspension is injected hydrated aluminum oxide in the amount of 8 to 15% Al2O3to the weight of the concentrate, maintain the reaction mass is 0.5 to 2.5 hours under heating and stirring. The degree of decomposition of the concentrate is 90 to 95% Then the suspension is cooled to 50 to 60oC, add water to the concentration of TiO2in the liquid phase 70 g/l and filtered with separation of the solid residue, which is a calcium-silica residue containing impurity compounds of titanium and aluminum. From the liquid phase by the method of crystallization produce such a product. The crystallization is carried out by introducing the liquid phase in a solution of ammonium sulfate (concentration (NH4)2SO4- 800 to 1000 g/l). The consumption of the latter is taken from the calculation of ensuring weight ratio of sulfuric acid to ammonium sulfate 1:0,4 0,6. Additive liquid phase is carried out gradually while stirring for 2 to 2.5 hours and Then the suspension is incubated for another 2 hours the Liquid phase decanted, and evaporated mass is added wash water (solution of ammonium sulfate 400 450 g/l (NH4)2SO4from the calculation of T:W 1:0,5. The suspension is stirred and filtered. The washed precipitate is own the high-quality leather. It includes tanning compounds of titanium and aluminum with a weight ratio of TiO2:Al2O3- 1:0,25 0,50. Calciumsilicate residue after decomposition of the concentrate is injected into the milk of lime, the amount of which is adjusted in the neutralization process control residual aluminum content in the solution (0.5 to 2.0 g/l on Al2O3). The residue in the milk of lime is injected slowly under stirring. The total time of contact of the reaction mixture 2 to 3 hours Then it was added phosphoric acid at the rate of 0.2 to 0.3% of P2O5in relation to the weight of the residue, the mixture is stirred for 0.5 h and filtered. The treated residue is calcined at 600 700oC obtaining calcium silicate pigment composition containing 9 to 13.5% of TiO2and 1.3 to 3.0% Al2O3with the following pigment characteristics: white is 95.6 96.8% of the oil absorption 26,4 27,4 g/100 g pigmentation treatment. opacity 59,1 68,4 g/m2.

Example 1.

Take 1 kg stanovova concentrate and add it under stirring heated to 100oC sulfuric acid 1080 g/l). The temperature of the reaction mass is raised to 145oC. After 1 h from the moment of attaining the above temperature is injected hydrated aluminum oxide at a rate of 8% Al the I of titanium in the liquid phase during the decomposition of the concentrate is 90% At the end of the process the mixture is cooled to 50 to 60oC and add water until the content in the liquid phase titanium 70 g/l, TiO2followed by filtration and separation of the solid residue. The liquid phase ( 2.5 l) contains g/l: H2SO4700, TiO270, Al2O325. It is added during 2 h in a solution of ammonium sulfate, the amount of which provides a weight ratio of sulfuric acid to ammonium sulfate 1 to 0.4, the duration of the move after the addition of the liquid phase 2 o'clock Titanomagniyevij product, crystallising in this case, washed with a solution of ammonium sulfate. The content of tanning components corresponds to a weight ratio of TiO2:Al2O 1:0.25 in. Weight 1135 g, the temperature of the welding 87oC.

The solid residue after decomposition (1300 g) is injected into the milk of lime. The residual content of aluminum in a solution of 0.5 g/l Al2O3.

The suspension is filtered and the obtained residue is processed in a known manner with getting calciumsilicate pigment composition (1550 g) containing 9% of TiO2, 2.7% of Al2O3with the following pigment characteristics: white 95.6% of the oil absorption compared to 27.4 g/100 g, the spreading rate is 64.3 g/m2.

Example 2.

Take 1 kg stanovova concentrate and add at paramesh is SUP>oC. After 2.0 hours from the moment of reaching the specified temperature enter the hydrated aluminum oxide, the rate of 12% Al2O3to the weight of the concentrate, the suspension is incubated for 1.5 hours under heating and stirring. The degree of extraction of titanium in the liquid phase during the decomposition of the concentrate is 92% At the end of the process the mixture is cooled to 50 to 60oC and add water until the content in the liquid phase titanium 70 g/l, TiO2followed by filtration and separation of the solid residue. The liquid phase ( 2.6 liters) contains in g/l: H2SO4650, TiO270, Al2O330,5. It is added during 2 h in a solution of ammonium sulfate, the amount of which provides a weight ratio of sulfuric acid to ammonium sulfate 1 to 0.5, the duration of mixing after the addition of the liquid phase 2 o'clock Titanomagniyevij product, crystallizing at the same time, washed with a solution of ammonium sulfate. The content of tanning components corresponds to a weight ratio of TiO2: Al2O31:0,35, weight 1150 g of Solid residue after decomposition (1300 g) is injected into the milk of lime. Residual aluminum content in the solution is 1.0 g/l Al2O3. The suspension is filtered and the obtained residue is processed in a known manner to obtain the mi pigment characteristics: white 96,1 g/l, the oil absorption of 26.4 g/100 g, opacity 59,1 g/m2.

Example 3.

Take 1 kg stanovova concentrate and add it under stirring heated to 100oC sulfuric acid 1080 g/l). The temperature of the reaction mass is raised to 145oC. After 3.0 hours from the moment of reaching the specified temperature is injected hydrated aluminum oxide at the rate of 15% Al2O3to the weight of the concentrate, the suspension is incubated for 0.5 h with heating and stirring. The degree of extraction of titanium in the liquid phase during the decomposition of the concentrate is 95% At the end of the process the mixture is cooled to 50 to 60oC and add water until the content in the liquid phase titanium 70 g/l, TiO2followed by filtration and separation of the solid residue. The liquid phase ( 2.7 l) contains in g/l: H2SO4600, TiO2- 70, Al2O335. It is added during 2 h in a solution of ammonium sulfate, the amount of which provides a weight ratio of sulfuric acid to ammonium sulfate 1 0,6, length of mixing after the addition of the liquid phase 2 o'clock Titanomagniyevij product, crystallizing at the same time, washed with a solution of ammonium sulfate. The content of tanning components corresponds to a weight ratio of TiO2:Al2O3. The suspension is filtered and the obtained residue is processed in a known manner with getting kallavaramlani pigment composition (1450 g) containing 11.8% of TiO2with 1.0% Al2O3with the following pigment characteristics: white 96.8% of the oil absorption of 26.5 g/100 g, opacity - to 68.4 g/m2.

In table. 1 shows examples justifying the selected optimal parameters. Table. 2 contains data showing the advantages of the inventive method compared to known.

Thus, the proposed method can improve the degree of decomposition of concentrate with an average 5% it out new products

titanomagniyevij the leather tanning agent, as well as white calciumsilicate pigment composition containing titanium dioxide and aluminum oxide, with a good paint-technical properties opacity 59,1 68,4 g/m2. Due to the presence in the product of the aluminum deposited on the surface of the particles, the composition can be used to prepare paint materials used not only indoors, but also for external coatings.

A method of processing stanovova concentrate, including the decomposition of the concentrate with the coy phase, characterized in that the decomposition of lead concentrate in the presence of hydrated aluminum oxide, which is injected in the amount of 8 to 15% Al2O3to the weight of the concentrate, the crystallization is carried out by adding a liquid phase in a solution of ammonium sulfate to ensure the weight ratio of sulfuric acid to ammonium sulfate equal to 1 (0,4 0,6), with titanomagnievoe product, and the solid residue is treated with lime milk to a residual content of aluminum in a solution of 0.5 to 2.0 g/l on Al2O3separating the treated residue and recycle it in a known manner with the receipt of the pigment composition.

 

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FIELD: mining industry.

SUBSTANCE: perovskite concentrate, which can be used for manufacture of pigment titanium dioxide for paints, paper, enamels, and plastics, is processed as follows. 1 kg of concentrate is treated under atmosphere conditions with concentrated HCl at 90-100оС for 10 to 20 h to solubilize 75-85% of titanium, radioactive, and other acid-soluble components. Concentration of HCl is then lowered by diluting it with 1-5% HCl solution until TiO2 concentration 50-100 g/L. Thermohydrolysis of solution at 100-105оС accompanied by distilling away HCl leads to residual HCl concentration 20-100 g/L. Distilled HCl is sent to processing of perovskite concentrate. Titanium-containing precipitate is separated from mother liquor, washed first with 15-37% HCl solution and then with water to pH 3. Washed precipitate is treated with aluminum acid phosphate with pH 2-4. Aluminum acid phosphate uptake (on conversion to Al2O3) constitutes 0.5 to 5.0% content of TiO2. Treated precipitate is separated and calcined at 850-870оС to give pigment titanium dioxide. From mother liquor (after separation of Ti-containing precipitate), radioactive components are isolated by 4-6-step extraction with tributyl phosphate. Organic phase-to-water phase ratio is (1.5-2.0):1. Degree of titanium recovery is at least 98%, whiteness at least 96.5 conv. units, brightening power 1650-1800 conv. units, spreading capacity 38.0-40.0 g/m2, oil capacity 25-27 g/100 g pigment. Yield of pigment TiO2 is 95.7-98.0%. Amount of radioactive precipitate does not exceed 0.06 kg.

EFFECT: optimized perovskite concentrate processing parameters.

12 cl, 4 ex

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