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. The method includes grinding of the concentrate to the size of particles of at least 0.075 mm, opening loparite concentrate nitric acid at atmospheric pressure and temperatures above 100C To produce a hydrated oxide of the refractory metal and nitric acid solution of rare earth elements, filtering hydrate cake and the subsequent processing of the products obtained. An autopsy carried out at the initial concentration of nitric acid in the pulp 350-500 g/l and a temperature of 105-110C in the presence of catalyst additives of fluorine-containing compounds in amounts of from 1.0 to 7.5% by weight of the concentrate in the calculation of the fluoride ion. As fluorine-containing compounds using HF, NH4F, NH4HF2, NaF, CaF2and mixtures thereof. The method allows to reduce the cost of finished products and to increase the efficiency of the process. 1 C.p. f-crystals table 1.

The invention relates to the hydrometallurgical processing of ore concentrates, and more particularly to the processing of loparite concentrate.

Loparite concentrate isoamyl for processing the concentrate of the brand CL-1 contains at least 95% of loparite and more. In accordance with the applicable specifications loparite contains, wt%:

oxide of tantalum (Ta2O5) - 0,57,

oxide of niobium (Nb2O5) - 8,14,

- titanium oxide (TiO2) - 38,1,

- oxides of rare earth metals cerium group, mainly the oxides of lanthanum, cerium, praseodymium and neodymium - 32,

- sodium oxide - 7,9-9,06,

- calcium oxide - 4,2-5,7,

oxide of thorium - 0,54

and small amounts of strontium, iron, silicon, aluminum, potassium and phosphorus.

From loparite concentrate extract the most valuable elements: tantalum, niobium, titanium and rare earth metals.

Widely known method of processing of loparite concentrate using concentrated sulfuric acid for the opening of loparite (see A. N. Zelikman and other "metallurgy of rare metals), metallurgy, 1991, S. 101, 103-105; J. G. Gorodenka "Physico-chemical studies of the processing of rare earth titanoniobates sulfuric acid method, an SSSR, Moscow-Leningrad, 1960).

Sulfuric acid method is based on the decomposition of loparite concentrate with sulfuric acid in the presence of ammonium sulfate and the separation of valuable components using differences in solubility of the double sulphate ttrat loparite is crushed to a particle size of not less than 0.075 mm. The opening of the concentrate conduct of 92.5-95% sulphuric acid, spent based 2,78 t and 0.2 t of ammonium sulfate per 1 ton of concentrate. At autopsy, runs at a temperature of 270-280oC, niobium and tantalum are part of the double sulfates of titanium in the form of isomorphic admixture. Rare earth elements are part of the double sulphate type - R2(SO4)3(NH4, Na)2SO4. Product sulfatization - sulfate spec subjected to water leaching. In the solid phase remain double sulphates REE, and in solution - titanium, niobium and tantalum. The major part of the thorium remains in the solid phase. Titan is released from the solution by 70-80% in the form of a titanium salt (NH4)2TiO(SO4)2H2O. Double titanyl sulphate and ammonium is used as a tanning agent in the leather industry. The solution of tantalum and niobium is subjected to fluorination 40% HF. Then the tantalum and niobium is removed from solution and separated using solvent extraction with tributyl phosphate. Sulfates REE are more independent technological cycle conversion to carbonates.

This method of processing of loparite concentrate has a number of significant drawbacks. The main of them is that the Oia tantalum and niobium is necessary to carry out additional processing of the dump cake REE. In addition irretrievably lost tantalum and niobium with crystals of titanium salt when salting out from sulfuric acid solution. Sulfuric acid method is sequential, consisting of separate periodic operations that cannot be automatically combined into a single control circuit. All this makes the method complicated, expensive, and cumbersome for hardware design.

All these drawbacks are eliminated in the method for processing of loparite concentrate on the patent of Russia No. 2145980 from 27.07.99 by M. CL.722 In 59/00, which is the prototype of the claimed invention.

In accordance with this method the original loparite concentrate is ground to particle sizes of not more than 0.075 mm by wet grinding. Opening loparite concentrate conduct concentrated 70-75% nitric acid when the initial concentration of the acid in the pulp With = 600-700 g/l and temperature 115-118oC. as a result of opening of concentrate nitric acid is produced nitrate slurry of hydrated oxide oxides of refractory metals (GCP) and the United nitric acid solution of rare earth elements (REE) with impurities and activity. Then nitrate hydrate slurry cake is diluted with water and cooled. the myvcu clean water from nitrate solutions of rare earth elements and impurities. Hydrate cake is the starting product for the production of a refractory oxides of metals. United nitric acid solution of rare earth elements with all the impurities and activity is subjected to decontamination followed by filtration. Net nitrate solution REE is the starting product for the production of a carbonate of rare earth elements.

Compared to sulfuric acid technology processing of loparite concentrate this method has several advantages. Way already at the initial stage of opening ensures a complete separation of tantalum, niobium and titanium from rare earth elements, radioactive and other impurities. The obtained hydrated cake GCP and nitrates REE are suitable for further processing.

For all its advantages prototype method has a number of disadvantages. Opening loparite concentrate is only special 70-75% nitric acid. 70-75% nitric acid is a highly valid poisonous substance (VP), which complicates its transportation, storage and more. Due to the very high strength and packing density of the crystal lattice of the mineral, even so the concentrate. The method has significant energy costs resulting from high temperature and long duration of the process. Additionally, when implementing the method has a low rate of filtration of the resulting slurry opening because of the presence of the gel formed at such high temperatures of compounds of silicon contained in the impurity minerals (quartz, aegirine) and released during their decomposition.

The present invention was used to develop the method for processing of loparite concentrate, in which an autopsy would be carried out under such conditions that provided increased penetration of loparite concentrate and decreased his time, was achieved by reducing energy consumption for the process and improved the filterability of the resulting pulp opening, thus reducing cost and increasing efficiency of the production as a whole.

The problem is solved in that in the method for processing of loparite concentrate, including the grinding of the concentrate to the size of particles of at least 0.075 mm, opening loparite concentrate nitric acid at atmospheric pressure and tampellini elements, filtering hydrate cake and the subsequent processing of the obtained products, what's new is that the autopsy carried out at the initial concentration of nitric acid in the pulp 350-500 g/l and a temperature of 105-110oC in the presence of catalyst additives of fluorine-containing compounds in amounts of from 1.0 to 7.5% by weight of the concentrate in the calculation of the fluoride ion.

This solution fluoride ions catalytic additives contribute to the loosening of the crystal lattice of loparite, which speeds up the process and increases the degree of opening of the concentrate, allows the use of low concentrations of the acid and reduce the energy consumption of the process by reducing the temperature and duration of opening. Also increases the rate of filtration of the resulting slurry, because at these temperatures in the presence of fluoride ion is not education in the solution of gel compounds of silicon. All of this together and reduces the cost of the finished product and efficiency of production in General.

The new way is so that as the fluorine-containing compounds, using HF, NH4F2, NH4HF2, NaF, CaF2and mixtures thereof.

The use of these seeing small consumption and low cost of most of them.

The following is the essence of the invention is explained in more detail by examples, confirming the possibility of its implementation.

The inventive method of processing of loparite concentrate is carried out as follows. Loparite concentrate is ground to particle sizes 0,040-0,074 mm Then perform an autopsy particles loparite, which concentrate Rasulova at atmospheric pressure of nitric acid at its initial concentration in the pulp 350-500 g/L. the slurry is injected catalyzing additives fluorine-containing compounds in amounts of from 1.0 to 7.5% by weight of the concentrate in the calculation of the fluoride ion. At the same time as the source of fluoride ion using HF, NH4F, NH4HF2, NaF, CaF2and mixtures thereof. The slurry is heated to 105-110oC and maintained at peremeci-aniii to practically complete opening of loparite.

Taken in the specified quantities of fluoride ion, is introduced into the slurry leaching, exhibits catalytic properties and contributing to the loosening of the crystal lattice of loparite, speeds up the process of opening while increasing its weight. This allows you to use for opening the weaker acid and low in comparison with the method of the prototype temperature. Plea 80% - in hydrated Keke together with oxides of tantalum, niobium and titanium.

Reduction of the fluoride ion is less than 1% leads to a reduction in the degree of opening of the concentrate. With increasing content of fluoride ion over 7.5% is the formation of insoluble fluorides of rare earth elements, which reduces the degree of translation of the REE into solution and the efficiency of the process as a whole.

Selected parameters of the initial concentration of nitric acid in the pulp of the opening equal to 350-500 g/l and a temperature equal to 105-110oC are optimal from the point of view of completeness of dissection concentrate and minimize the cost of energy and chemicals. There is no gel formation of compounds of impurity minerals (quartz, aegirine).

The resulting opening of the slurry is filtered. This filtration rate due to the lack of gel of silicon is several times larger than the filtration rate, the method prototype and reaches 0.5 m3/m2h against 0.1 m3/m2hour.

By filtering the receive hydrated cake oxides of refractory metals and nitric acid solution of rare earth elements. They are end products of the proposed method and then each of them pererabotka illustrates a concrete example of its implementation.

Example.

Loparite concentrate Caracortado field with lattice parameter a = 3,888 in the amount of 1 kg, containing, %: 0,54 That, 6,7 Nb, 38,0 TiO2, 30,0 R2O3crushed to a particle size 0,040-0,074 mm, repurposable 2.5 l of nitric acid with the initial concentration of 450 g/L. the slurry was injected fluorine in the form of hydrofluoric acid in the amount of 26.4 g, which is 2.5% by weight of concentrate in terms of fluoride ion. The slurry was heated to a temperature of 107oC and kept under stirring for 15 hours.

The resulting slurry autopsy was subjected to filtration. The filtration rate was 0.5 m3/m2hour. By filtering the obtained precipitate crystal structure of anatase, which is hydrated cecom oxides of refractory metals containing, wt.%: the basis of TiO2, 14% of Nb2O3, 1%, Ta2O5and 3-6% aegirine, as well as the nitric acid solution of rare earth elements REE content of more than 140 g/l with an impurity, g/l: 0,2-0,6 TiO2, 0,01-0,02 Nb2O5, less than 0.01 TA2O5. The degree of extraction of rare earth elements in the solution is of 99.3%, and the degree of opening of loparite close to 100%.

The resulting products are added is about concentrate on the parameters of the proposed method is additionally illustrated by the ten examples United in the table below at a flow rate of nitric acid 1.15 t/t of concentrate and the ratio of solid phase to liquid - T:W = 1,0:2,5.

It should also be noted that during the processing of loparite Umbozero field with a more dense packing of the crystal lattice of the mineral and = 3,873 in accordance with the inventive method the time of opening increases to 35 hours while maintaining the other parameters.

From the specific embodiments of the claimed invention for any specialist in this field are obvious possibilities for its realization with the simultaneous solution of the set task. It is also obvious that the invention can be made small changes, but which will not exceed the scope of the invention defined by the following claims.

The inventive method of processing of loparite concentrate was pilot check processing 300 tons of loparite concentrate. It provides a possibility for opening loparite concentrate nitric acid. The use of the proposed method allows to increase the degree vskrytii process of opening the concentrate up to 3 times essentially intensify stage filtration and reduce energy costs 4-6 times. All this reduces the cost of the finished product and efficiency of production in General.

1. Method for processing of loparite concentrate, including the grinding of the concentrate to the size of particles of at least 0.075 mm, opening loparite concentrate nitric acid at atmospheric pressure and a temperature of more than 100oWith obtaining hydrated oxide of the refractory metal and nitric acid solution of rare earth elements, filtering hydrate cake and the subsequent processing of the products obtained, characterized in that the autopsy carried out at the initial concentration of nitric acid in the pulp 350 - 500 g/l and a temperature of 105 - 110oIn the presence of catalyst additives of fluorine-containing compounds in amounts of from 1.0 to 7.5% by weight of the concentrate in the calculation of the fluoride ion.

2. The method according to p. 1, characterized in that as the fluorine-containing compounds using HF, NH4F, NH4HF2, NaF, CaF2and mixtures thereof.

 

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