The method of decomposition of mineral and technogenic raw materials

 

(57) Abstract:

The invention relates to the technology of mineral and technogenic raw materials used to produce compounds of titanium, niobium, tantalum and rare earth elements. The invention consists in that the feedstock is treated in sealed hydrochloric acid with a concentration of 35.5-40% at T:W=1:3,4-20,0, and the temperature of 75-100°C. as a source of raw materials used loparite, ilmenite, sphene, perovskite, titanomagnetite and lithium niobate. Treatment is carried out at an initial pressure of 0.2-0.5 MPa. In addition, the process is conducted in countercurrent mode. The method allows to reduce the energy intensity of the process by reducing the processing temperature while providing a high degree of extraction in a solution of valuable components, as well as to simplify the instrumentation process. 3 C.p. f-crystals.

The present invention relates to technology of mineral and technogenic raw materials used to produce compounds of titanium, niobium, tantalum and rare earth elements.

There is a method of decomposition of mineral and technogenic raw materials, in particular perovskite concentrate (see German patent N 285083, IPC C 01 G 23/04, 1990), by treatment"ptx2">

There is a method of decomposition of mineral and technogenic raw materials, in particular of ilmenite concentrate (see E. Belyakova P., Demakova A. A. Decomposition of ilmenite concentrate hydrochloric acid //Ukr.chem.W. 1963, 29, N 6, 633-636), by treatment with 20% hydrochloric acid at a temperature of 220oC in the autoclave.

The disadvantages of these methods are high decomposition temperature, high energy consumption and complexity of instrumentation.

There is a method of decomposition of mineral and technogenic raw materials, in particular metaniobate lithium (see Kulibaev C. K., Myakishev L. C. development of a comprehensive utilization technology of niobium and lithium from waste and scrap production of single crystals of lithium niobate // 2nd international Symposium on Problems of complex use of ores, 19-24 may 1996, S.-Petersburg, S. 337), by sintering with a slight excess of lithium carbonate at a temperature of 700-725oC obtaining antoniobuy lithium, which is decomposed with hydrochloric acid.

The disadvantage of this method is the necessity of high-temperature sintering metaniobate lithium with an excess of lithium carbonate, which leads to additional energy costs, makes the process of multi-operational and Tristan the method of decomposition of mineral and technogenic raw materials, in particular loparite concentrate (see Murach N. N., Povazska L. G., Kulibaev C. K. proceedings of the. Inst. flourish. met. them. M. I. Kalinin. 1963, N 35, 171-174), by treatment with 35% hydrochloric acid in an autoclave at T:W = 1: 4.75 V and a temperature of 110-120oC for 4 hours. Before processing the concentrate is ground to a particle size of 740 μm. For the more active acid exposure in autoclave load porcelain balls. Extraction of valuable components concentrate in the solution is 95-97%. The output of the solid residue does not exceed 8-10%.

The disadvantages of this method are the high temperature process, a lack of full recovery of valuable components, the implementation process in the autoclave, which complicates its instrumentation.

The present invention is directed to solving the problem of reducing the energy intensity of the process and simplify hardware design, while ensuring a high degree of extraction in a solution of valuable components.

The problem is solved in that in the method of decomposition of mineral and technogenic raw materials containing a metal selected from the group comprising niobium, tantalum, titanium, by processing the feedstock in an airtight conditions of concentrated hydrochloric to is the temperature value 75-100oC.

On the solution of the problem is also aimed that the quality of raw materials used loparite, ilmenite, sphene, perovskite, titanomagnetite and lithium niobate.

The solution of this problem is achieved by the fact that the treatment is carried out at an initial pressure of 0.2 - 0.5 MPa.

The problem is solved also by the fact that the process is conducted in countercurrent mode.

Increasing acid concentration of more than 35.5 per cent reduces the decomposition temperature without compromising the degree of extraction of valuable components and duration of the process. The upper limit concentration of 40% is determined by the solubility of hydrochloric acid. With decreasing concentrations of less than 35.5 per cent increase material flow and reduced the degree of extraction of valuable components in the solution.

Carrying out processing in an airtight conditions provides the use of acids without loss of interaction with the raw materials.

The temperature increase of more than 100oC complicates the instrumentation process. The temperature decrease of less than 100oC simplifies the selection of construction materials and method of heating, and also reduces energy consumption, but when the temperature drops below 75oC reduces revised 0.5 MPa. The lower limit pressure of 0.2 MPa is determined by the residual hydrochloric acid and the temperature of the process.

The process mode allows backflow in the claimed range of concentrations and temperatures to achieve 99% extraction of all valuable components and their maximum concentration in the final solution.

The nature and advantages of the proposed method can be explained by the following Examples.

Example 1. 5 g of loparite concentrate particle size of 50 μm with the composition, wt.%: TiO246,30; the amount of REE 26,19; SrO 2,20; Nb2O56,16; Ta2O50,47; CaO 5,40; K2O 1,80; SiO22,10; Fe2O30,6; ThO20,63; insoluble in hydrochloric acid minerals (aegirine, feldspar) 4,80, process sealed 37% hydrochloric acid at T:W=1:5 and a temperature of 100oC for 6 hours. Separated by filtering the insoluble residue. The weight of the remainder of 0.39, the Degree of extraction for insoluble in hydrochloric acid components is 96.8%. The filtrate contains, g/l: TiO285,40); the amount of REE 48,30; Nb2O511,40; Ta2O50,80.

Example 2. Process loparite concentrate of Example 1, but at the 90oC and the pressure at the beginning of the process 0, 11,50; Ta2O50,90.

Example 3. Process loparite concentrate of Example 1, but at the 75oC. the weight of the remainder of 0.77, the Degree of extraction 88,9%. The filtrate contains, g/l: TiO278,30); the amount of REE 44,30; Nb2O5the 10.40; Ta2O50,80.

Example 4. Process loparite concentrate of Example 1, but at T:W= 1: 4 and a temperature of 90oC. the weight of the remainder of 0.42, the Degree of extraction 96,3%. The filtrate contains, g/l: TiO2106,00; the amount of REE 59,90; Nb2O514,10; Ta2O51,10.

Example 5. Process loparite concentrate of Example 1, but at the 90oC for 4 hours. The weight of the remainder of 0.45, the Degree of recovery of 95.7 per cent. The filtrate contains, g/l: TiO284,30); the amount of REE 47,70; Nb2O511,20; Ta2O50,85.

Example 6 carry out the acid treatment the amount of insoluble residue formed in the process according to Examples 1-5, i.e., use the countercurrent mode, additionally increasing the degree of extraction.

Example 6. of 2.36 g of insoluble residue obtained in Examples 1-5, treated with 37% hydrochloric acid at T:W=1:7, the temperature of the 75oC for 4 hours. The pressure at the beginning of the process of 0.2 MPa. The weight of the insoluble residue of 0.68, crystal optics EN is th acid in countercurrent mode is achieved almost complete extraction of valuable components in the solution.

Example 7. 5 g perovskitelike concentrate particle size of 100 μm with the composition, wt.%: TiO253,0); the amount of REE 2,0; (Nb,Ta)2O50,8; CaO 36,0; SiO24,2; Fe2O32,0; FeO 0,9; insoluble in hydrochloric acid minerals (metasilicate, olivine) 12,0, process sealed 39% hydrochloric acid at T:W=1:5 and a temperature of 100oC for 7.5 hours. Separated by filtering the insoluble residue. The weight of the remainder of 0.64, the Degree of extraction for insoluble in hydrochloric acid components is 99.0%. The filtrate contains, g/l: TiO292,0; (Nb,Ta)2O51,4; CaO 62,7.

Example 8. Process perovskites concentrate according to example 7, but 38% hydrochloric acid at T: W=1:3.4 and a temperature of 95oC for 8 hours. The weight of the residue 0,88, the Degree of extraction 94,0%. The filtrate contains, g/l: TiO287,3; (Nb,Ta)2O51,3; CaO 59,3.

Example 9. Process perovskites concentrate according to example 7, but 40% hydrochloric acid at T:W=1:5 and a temperature of 90oC for 6 hours. The weight of the residue 0,69, the recovery of 98.3%. The filtrate contains, g/l: TiO291,3; (Nb,Ta)2O51,38; CaO 62,0.

Example 10. Process perovskites concentrate according to example 9, but at T: W=1:4. Weight balance 0,80, the Degree Izv what about the concentrate particle size of 250 microns, with composition, wt. %: TiO233,1); the amount of REE 0,5; CaO 24,9; SiO230,0; Fe2O31,6-3,6; insoluble in hydrochloric acid components 30,0, process sealed 38% hydrochloric acid at T:W=1:5 and a temperature of 95oC for 4 hours. Separated by filtering the insoluble residue. The weight of the remainder of 1.55, the Degree of extraction for insoluble in hydrochloric acid components is to 98.4%. The filtrate contains, g/l: TiO245,7; CaO 34,3.

Example 12. Process stanovy concentrate according to example 11, but at a temperature of 75oC for 6 hours. The weight of the residue 2,00, the extraction rate of 85.7%. The filtrate contains, g/l: TiO239,7; CaO 29,9.

Example 13. 5 g of ilmenite concentrate with a particle size of 70 μm with the composition, wt.%: TiO246,0; Fe2O35,0; FeO 35,0; SiO26,0; MgO 2,0; insoluble in hydrochloric acid components 6,0, process sealed 38% hydrochloric acid at T:W=1:5 and a temperature of 95oC for 5 hours. Separated by filtering the insoluble residue. The weight of the remainder of 0.29, the Degree of extraction for insoluble in hydrochloric acid components is 99.0%. The filtrate contains, g/l: TiO286,6; Fe2O39,4; FeO 65,9.

Example 14. Process of ilmenite to the, g/l: TiO282,0; Fe2O38,8; FeO 62,5.

Example 15. 5 g of magnetite concentrate with particle size of 200 μm with the composition, wt.%: TiO215,5; Fe 56,5; SiO22,3; insoluble in hydrochloric acid components 8,0, process sealed 38% hydrochloric acid at T:W=1:5 and a temperature of 95oC for 7.5 hours. Separated by filtering the insoluble residue. The weight of the remainder of 0.42, the Degree of extraction for insoluble in hydrochloric acid component of 99.5%. The filtrate contains, g/l: TiO228,4; Fe 95,0.

Example 16. 5 g waste lithium niobate with a particle size of 50 μm, obtained by cutting a wafer from a single crystal, is treated in an airtight conditions of 37% hydrochloric acid at T:W=1:20 and a temperature of 95oC for 7 hours. Separated by filtering the insoluble residue. The weight of the residue 0,175, the recovery of 96.5%. The filtrate contains, g/l: Nb2O543,0; Li2O 4,9.

Example 17. Process waste lithium niobate for Example 16, but at T:W= 1: 15 for 8 hours. The weight of the remainder of 0.28, the recovery of 94.5%. The filtrate contains, g/l: Nb2O556,5; Li2O 6,4.

Thus, from these Examples it follows that the present invention provides the treatment in the solution of valuable components, and also to simplify the instrumentation process.

1. The method of decomposition of mineral and technogenic raw materials containing a metal selected from the group comprising niobium, tantalum, titanium, by processing the feedstock in an airtight conditions of concentrated hydrochloric acid under heating and stirring, characterized in that the processing of raw materials lead hydrochloric acid with a concentration of 35.5 - 40% at T : W = 1 : 3,4 - 20,0 and a temperature of 75 - 100oC.

2. The method according to p. 1, characterized in that the feedstock used loparite, ilmenite, sphene, perovskite, titanomagnetite and lithium niobate.

3. The method according to p. 1 or 2, characterized in that the treatment is carried out at a pressure of 0.2 - 0.5 MPa.

4. The method according to any of paragraphs.1 to 3, characterized in that the process is conducted in countercurrent mode.

 

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