Method for processing of loparite concentrate

 

(57) Abstract:

The invention relates to the hydrometallurgical processing of ore concentrates, and more particularly to the processing of loparite concentrate, and can be used in complex extraction of compounds of titanium, niobium and tantalum. Method for processing of loparite concentrate includes opening hydrochloric acid when heated, and receiving from the liquid phase of hydrated oxide hydroxides of titanium, niobium and tantalum. Thus ukryta exercise 26-32% hydrochloric acid to the extent of decomposition of 70-90%. After that, unopened concentrate separated. Before getting hydrated cake liquid phase is evaporated by 10-30% by volume with carbon capture and condensation of the vapor of hydrochloric acid. Then the liquid phase is diluted with water to the original volume, give it the initiating additive in the amount of 2-10% by weight of the original concentrate and maintained at boiling for 3-6 h to obtain hydrated cake. The method is easy to implement, involves the use of standard equipment. Its implementation is designed to reduce the time of receipt of hydrated cake and consumption of hydrochloric acid. 3 C.p. f-crystals.

The invention relates to hydrometallurgical is used for complex extraction of titanium compounds, niobium and tantalum.

There is a method of processing of loparite concentrate using concentrated acid (A. N. Zelikman, and A. Miron. Metallurgy of rare metals. M , metallurgy, 1991, S. 101-105). The method consists in the fact that crushed loparite concentrate with a particle size of 95% less than 74 microns reveal 95% sulfuric acid at a temperature of 270-280oWith consumption 2,78 t per tonne of concentrate. When this type of 0.2 tonnes of ammonium sulfate to prevent sintering of the reaction mass. The resulting water leached with water. While titanium, niobium and tantalum into solution (86-93%), from which the titanium is precipitated by ammonium sulfate in the form of poorly soluble in sulfuric acid solutions of titanium salt (NH4)2TiO2(SO4)2H2O. the Degree of precipitation is 80% of the content of TiO2in the solution. The degree of co-precipitation of niobium and tantalum and titanium salt is 5-10%. From the solution after separation of the titanium salts spend the emission of compounds of niobium and tantalum by the method of extraction in the presence of fluoride ion.

This method has several significant disadvantages. This is, firstly, the use at the stage of opening the concentrate of the two reagents sulphuric acid and ammonium sulphate, which complicates t is and calcium, which goes to dump. The disadvantages include high temperature process, requiring additional measures to ensure the safety and equipment of the process, the impossibility of separating unopened part of concentrate, which leads to irreversible loss of valuable components. It should be noted that the method does not effectively separate the radioactive component of the concentrate and receive radio-friendly products and intermediates.

More advanced and closest to the claimed method is a method of processing of loparite concentrate its opening hydrochloric acid (magazine "non-ferrous metals", 10, 2000, S. 52-53). The method includes opening loparite concentrate 28-30% hydrochloric acid at atmospheric pressure for 8-10 hours at a temperature of 100-105oC. the Precipitate containing unopened loparite and aegirine, share. From the separated liquid phase of the pulp hydrolysis, subject to certain conditions, are precipitated hydroxides of titanium, niobium and tantalum.

The method eliminates the loss of valuable components in comparison with the above analog. However, he has a greater length of time to get hydrated cake and to develop a method for processing of loparite concentrate, which process would occur under such conditions and with such reagents, to ensure the reduction of the time of receipt of hydrated cake and consumption of acid, which is the technical result of the claimed invention.

The technical result is achieved in that in the method for processing of loparite concentrate, including the opening of hydrochloric acid when heated, and receiving from the liquid phase of hydrated oxide hydroxides of titanium, niobium and tantalum, what's new is that the autopsy carried out 26-32% hydrochloric acid to the extent of decomposition of 70-90%, then unopened concentrate is separated, before getting hydrated cake liquid phase is evaporated by 10-30% by volume with carbon capture and condensation of the vapor of hydrochloric acid, the liquid phase is diluted with water to the original volume, give it the initiating additive in the amount of 2-10% from the mass of the initial concentrate and maintained at boiling for 3-6 hours to get hydrated cake.

This solution reduces the time of receipt of hydrated cake and reduces the consumption of hydrochloric acid.

New is also that unopened concentrate return for a second autopsy.

This posea, what caught when Parke hydrochloric acid is directed into the circulation.

Thanks to this additionally reduces the consumption of hydrochloric acid.

Also new is the fact that as the initiator of the additive use of hydrated cake.

It is economically feasible, because the use of hydrated cake as initiating additive eliminates the use in the way of additional reagents.

Below the essence of the invention is explained in more detail detailed examples of its implementation.

The inventive method is carried out as follows.

Prepared by stirring a suspension consisting of 26-32% hydrochloric acid and loparite concentrate ratio (T:W=1:4), is heated to a temperature of 95-105oC with continuous stirring for 8-10 hours to achieve the degree of decomposition concentrate 70-90%. Unopened part of loparite concentrate is separated by filtration from the liquid phase and sent for re-opening. The liquid phase is evaporated by 10-30% by volume with carbon capture vapors of hydrochloric acid, condensation and return of the acid on the opening of the condensate. One stripped off, the solution was diluted with water to the original volume of the additive use of hydrated cake. The resulting mixture was heated to boiling and incubated for 3-6 hours. As a result of this get hydrated cake consisting of titanium oxide, niobium and tantalum. Under such conditions, iron is found primarily in the divalent state, and the oxide of thorium in the cake not deposited. Their presence in hydrated Keke conditioned only by the efficiency of the washing thereof. Obtained under such conditions hydrated cake has the following composition, wt.%: TiO2is 55.2-58,5; Nb2O5- the 11.6-15,3; Ta2O5- 0,92-1,22; the amount R2ABOUT3- 0,1-0,8; ThO2less than 0.001, Fe2ABOUT3- 0,09-0,11.

Evaporation of the liquid phase after separation unopened concentrate and further dilute it with water to reduce the acidity of the resulting solution, and the introduction of initiating additive (hydrated cake) significantly reduces the boiling required to obtain hydrated cake.

When using hydrochloric acid concentration of less than 26% is premature to hydrate cake that pollutes unopened part concentrate and worsens the terms of his separation from the liquid phase. The use of hydrochloric acid with a concentration of more than 32% is impractical because more kontsentrirovannej the cake.

When conducting the process of opening less than 8 hours before the decomposition rate of the concentrate is less than 70%, the accumulation of iron in the liquid phase due to the higher rate of solubility in comparison with other components present in the concentrate, and as a consequence of increased content of iron compounds in the hydrated cake. When conducting the process of opening more than 10 hours to the degree of decomposition concentrate more than 90% increases the probability of premature formation in the liquid phase hydrate cake and pollution unopened concentrate.

Consumption initiating additive is less than 2% of the initial mass of the concentrate leads to a significant increase in the time duration of the process, reduce the degree of aggregation of particles of hydrated cake and the increased content of iron. At a rate higher than 10% as hydrated cake is not changed.

Evaporation of the liquid phase by 10-30% by volume provides optimum conditions for Hcl vapor recovery, condensation and return to the process.

Return unopened part of loparite concentrate on re-opening can increase the degree of transition of valuable components in the liquid phase to 100%.

Use as iniciaron reagents.

The nature and advantages of the invention can be explained with detailed examples:

Example 1.

Take 1 kg of loparite concentrate and suspension it in 4 liters of 28% hydrochloric acid. The suspension is heated to 100oC and maintained under stirring for 10 hours to the degree of decomposition of the concentrate of 82.5%. Then separated by filtration unopened part concentrate (175 g) and sent it to re-opening. The filtrate is evaporated to 20% by volume with trapping the Hcl. One stripped off, the solution was diluted with water to the original volume and injected into him initiating additive in the form of hydrated oxide in the amount of 2.5% of the original weight of the concentrate. The solution is heated to boiling and incubated for 4.5 hours with the release of hydrated oxide, which is separated from the liquid phase and washed with 28% hydrochloric acid. Weight obtained hydrated cake - 580, Composition, wt.%: TiO2- 57,3, Nb2O5- 13,1, TA2O5- 1,22, the amount R2ABOUT3- 0,1, ThO2less than 0.001, Fe2ABOUT3- 0,09. The total duration of 20 hours.

Example 2.

Take 1 kg of loparite concentrate and suspension it in 4 liters of 24% hydrochloric acid. The suspension is heated to 1052- 55,8, Nb2O5- 11,6, TA2ABOUT5to 0.92, the amount R2ABOUT3to 0.8, ThO2less than 0.001, Fe2O3- 0,11. The total duration of 20 hours.

Example 3.

Take 1 kg of loparite concentrate and suspension it in 4 liters of 32% hydrochloric acid. The suspension is heated to 95oC and maintained under stirring for 10 hours to the degree of decomposition of the concentrate of 90.0%. Then separated by filtration unopened part concentrate (110 g) and sent it to re-opening. The filtrate is evaporated to 10% by volume with the trapping model HC1. One stripped off, the solution was diluted with water to the original volume and injected into him initiating additive in the form of hydrated oxide in the amount of 10.0% of the original weight of the concentrate. The solution to the basics and washed with 32% hydrochloric acid. Weight obtained hydrated cake - 590, Composition, wt.%: TiO2- 58,5, Nb2O5and 15.3, TA2O5- 0,96, the amount of TR2O3to 0.3, ThO2less than 0.001, Fe2O3- 0,11. The total duration of 20 hours.

Example 4.

Take 175 g unopened loparite concentrate from decomposition (example 1) and 825 g of fresh concentrate and suspension the mixture into 4 liters of 28% hydrochloric acid. The suspension is heated to 105oC and maintained at paramedian for 10 hours to the degree of decomposition of the concentrate of 82.5%. Then separated by filtration unopened part concentrate (175 g) and sent it to re-opening. The filtrate is evaporated to 20% by volume with the trapping model HC1. One stripped off, the solution was diluted with water to the original volume and injected into him initiating additive in the form of hydrated oxide in the amount of 5.0% of the original weight of the concentrate. The solution is heated to boiling and incubated for 4.5 hours with the release of hydrated oxide, which is separated from the liquid phase and washed with 28% hydrochloric acid. Weight obtained hydrated cake - 585, Composition, wt.%: TiO2- 58,5, Nb2O5and 15.3, TA2ABOUT5- 0,96, the amount of TR2O3to 0.3, ThO2less than 0.001, Fe2ABOUT3

The inventive method is easy to implement, involves the use of standard equipment. Its implementation is designed to reduce the time of receipt of hydrated cake and consumption of hydrochloric acid.

1. Method for processing of loparite concentrate, including the opening of hydrochloric acid when heated, and receiving from the liquid phase of hydrated oxide hydroxides of titanium, niobium and tantalum, wherein the autopsy carried out 26-32% hydrochloric acid to the extent of decomposition of 70-90%, then unopened concentrate is separated, before getting hydrated cake liquid phase is evaporated by 10-30% by volume with carbon capture and condensation of the vapor of hydrochloric acid, the liquid phase is diluted with water to the original volume, give it the initiating additive in the amount of 2-10% from the mass of the initial concentrate and maintained at boiling for 3-6 h to obtain hydrated cake.

2. The method according to p. 1, characterized in that unopened concentrate return on re-skriti Orot.

4. The method according to p. 1, characterized in that as the initiator of the additive use of hydrated cake.

 

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FIELD: nonferrous metallurgy.

SUBSTANCE: invention aims at recovering uncommon metals from silicate ores and concentrates in processing of zirconium concentrates. Method according to invention envisages treating cake obtained by caking zircon concentrate with calcium oxide in presence of nitric or sulfuric acid. Concentrated acid is added to water-slurried cake at constant speed during 30-60 min in two steps so that 18-25% of acid is added during first 30 min, whereupon zirconium is leached at 80-90оС.

EFFECT: increased filtration velocity and simplified process due to reduced number of operations.

2 cl, 2 dwg, 4 ex

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