The method of decomposition titanosilicates raw materials

 

(57) Abstract:

The invention relates to technology for processing titanosilicates raw materials, in particular to the decomposition stanovova concentrate. Stanovy concentrate is treated with nitric acid with a concentration of 15-25% at a temperature of 110-130oC for 5 hours Then the reaction mass is then cooled to 20-25oC and filtered with the Department of titanium containing solid residue. Nitric acid treatment titanosilicates raw materials is preferably carried out at a reactor pressure of 1.2-2.4 kg/cm2. The technical result is to increase the extraction of calcium in solution to 93.5-98,0% and the fraction of reactive anatase form of titanium dioxide in the solid residue up to 40-60%. 1 C.p. f-crystals, 1 table.

The invention relates to technology for processing titanosilicates raw materials, mainly to the decomposition stanovova concentrate, and can be used for the production of scarce and high-quality products based on titanium.

There is a method of decomposition titanosilicates raw materials (see ed. mon. THE USSR 592756, IPC2C 01 G 23/00, With 22 In 3/00, 1978), in particular stanovova concentrate, including the processing of finely ground concentrate 70% sulfuric acid at temporary decrease of temperature down to 130-140oWith a speed of 2.5 to 0.2oC/min within 0.3-3 h, additional sulfatization in these conditions within 2-6 h with stirring, the growing mass with subsequent maturation custody for 10 hours.

The disadvantages of this process are the formation of a number of sulfates of titanium and calcium complex structure with unclear distribution between the solid and liquid phases, which limits the recovery of useful components, high decomposition temperature stanovova concentrate and the use of concentrated sulfuric acid, complicating the process, high residual acidity of the reaction mass, complicating its further processing and leading to excessive consumption of reagents, as well as a large (16.5 hours), the duration of the decomposition process.

There is also known a method of decomposition titanosilicates raw materials (see Kostrikin C. M. , Melent'ev B. N., Reznichenko Century A. Autoclave opening perovskitelike concentrate. The refining and processing of mineral raw materials. The compilation. "Minerals". M.: Nedra, 1966, vol. 3, S. 63-69), in particular perovskite concentrate comprising autoclaving the ground to 150 mesh concentrate 50% nitric acid with excess consumption of 20% at temperature with additional extraction of calcium in the solution, filtering with the Department of titanium containing solid residue and rinse. The titanium in the solid residue contained mainly in rutile form. Removing the calcium in the solution is not more than 92%.

The disadvantages of this method are the relatively low extraction of calcium in solution, high temperature processing of the concentrate, which contributes to the preferential formation of residue rutile forms titanium, high concentration used nitric acid, and the decomposition of the concentrate under conditions of high pressure, which complicates the implementation process.

The present invention is directed to solving the problem of increasing the degree of extraction of calcium in the solution and increase the balance in the proportion of titanium in a more reactive anatase form. The invention also solves the problem of reducing energy consumption of the method.

The problem is solved in that in the method of decomposition titanosilicates raw materials, including autoclave processing of raw materials nitric acid when heated with translation of the calcium nitrate solution and the concentration of titanium in the solid residue, and separating residue, according to the invention as a source of raw materials used stanovy "ptx2">

The problem is solved also by the fact that the processing stanovova concentrate is carried out at a pressure of 1.2-2.4 kg/cm2.

The invention consists in that the solubility of calcium nitrate in solutions of nitric acid has an inverse dependence on the concentration of free nitric acid in the system. Therefore, the decrease of the concentration of the acid up to 15-25% during the decomposition of the concentrate increases the extraction of calcium in the solution and increases the balance in the proportion of titanium in the anatase form, is more chemically active than rutile.

When the concentration of nitric acid of less than 15% or more than 25% and a temperature below 110oWith reduced extraction of calcium in solution, and at temperatures above 130oWith significantly (more than 2.4 kg/cm2) increases the pressure in the apparatus, the declining share of the anatase form of titanium dioxide in the balance.

Nitric acid treatment titanosilicates raw materials is preferably carried out at a reactor pressure of 1.2-2.4 kg/cm2that helps to reduce energy costs and simplifies hardware design process and operation of the equipment.

The nature and advantages of the invention can be illustrated by the Cao, 37,1 Tio2, 26,5 SIO, SIS2process in the reactor 25% nitric acid, taken with excessive in relation to the calcium 10% flow, at a temperature of 110oC and a pressure of 1.2 kg/cm2within 5 hours the Reaction mass is then cooled to 20-25oC and filtered with the Department of titanium containing residue. Removing the calcium in the solution was 93.5%. The share of the anatase form of Tio2in the remainder equal to 60%.

The main technological parameters and the results obtained in Examples 1-6 according to the claimed method, and Examples 7-10 with transcendent values and Example 11 of the prototype presented in the Table.

Example 2. 20 g of finely stanovova concentrate is treated analogously to Example 1, but with excessive in relation to the calcium 20% consumption of acid at a temperature of 120oC and a reactor pressure of 1.6 kg/cm2. Removing the calcium in the solution amounted to 98%. The share of the anatase form of TiO2in the remainder equal to 55%.

Example 3. 25 g of finely stanovova concentrate is treated analogously to Example 1 but at a temperature of 130oC and a reactor pressure of 2.3 kg/cm2. Removing the calcium in solution were $ 97.6%. The share of the anatase form of TiooC and a reactor pressure of 2.1 kg/cm2. Removing the calcium in the solution amounted to 96.4 per cent. The share of the anatase form of TiO2the remainder is 46%.

Example 5. 10 g of finely stanovova concentrate is treated analogously to Example 1, but 15% nitric acid at a temperature of 130oC and a reactor pressure of 2.4 kg/cm2. Removing the calcium in the solution amounted to 96.6%. The share of the anatase form of TiO2the remainder is 40%.

Example 6. 10 g of finely stanovova concentrate is treated analogously to Example 1, but 15% nitric acid at a temperature of 120oC and a reactor pressure of 1.8 kg/cm2. Removing the calcium in the solution was 94,9%. The share of the anatase form of TiO2the remainder is 54%.

As seen from the above Examples, the use of the proposed method improves the extraction of calcium in solution to 93.5-98,0% and the fraction of reactive anatase form of titanium dioxide in the remainder up to 40-60%. Implementation of the proposed set of features can also reduce the energy intensity of way.

1. The method of decomposition titanosilicates raw materials, including autoclave processing of raw materials nitrogen kilo Department balance, characterized in that the feedstock used stanovy concentrate, and the nitric acid treatment is carried out at acid concentration of 15-25% and a temperature of 110-130oC.

2. The method according to p. 1, characterized in that the processing stanovova concentrate is carried out at a pressure of 1.2-2.4 kg/cm2.

 

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