Method for extraction by sorption and removing ions of non-ferrous metals from thallium

FIELD: hydraulic metallurgy of thallium, possibly extraction and removing ions of non-ferrous metals from isotope-enriched thallium.

SUBSTANCE: method comprises steps of sorption of thallium from nitrate solutions; before sorption treating initial nitrate solutions with organic reducing agent such as alcohol or formaldehyde solution until pH 1.5 - 2.5; adding complexone II or III in quantity 1.2 - 1.5 mol of complexone per 1 mol of total quantity of impurities; correcting solution until pH 4 - 5 by means of ammonium; realizing desorption of thallium by means of ammonium sulfate solution (2 - 4 M) after preliminary removal of impurities from cationite by washing it with water and with solution of complexone II or III; or performing after-purification (after desorption) of eluates with use of anionite of epoxy-polyamine type.

EFFECT: lowered number of operations, reduced consumption of reagents, prevention of outbursts of harmful matters to atmosphere, improved effectiveness.

3 cl, 11 tbl, 11 ex

 

The present invention relates to hydrometallurgy thallium and can be used for extraction and purification from non-ferrous metals ions isotope-enriched thallium using sorption processes.

A known method for simultaneous sorption of thallium, indium, zinc, cadmium by sorption on their sulfoxylate the cation exchange resin KU-2 at pH≈4 followed by desorption of thallium acid solutions. [“Ion exchange technology in hydrometallurgy” Alma-ATA, Nauka, 1970, p.15-23]. This method is taken as a prototype, as the closest to the claimed method and characterized by high efficiency of extraction of thallium from complex solutions. A significant drawback of the prototype method is the lack of selective sorption of thallium from solutions, which suggests the presence of further operations on removing thallium from the eluates. In addition, the high concentration of metal ion impurities, such as copper, iron(III), sorption of thallium on the sulfonic cation exchanger is virtually absent due to preferential sorption of ions of divalent or trivalent metals (competitive sorption of impurities). Marked as for the method-analogue, has led to the loss of expensive isotope, or the processing of eluates obtained during desorption of thallium and other commodities, by the way, op is sliding in the analog, which leads to the complication of the technology of metal extraction and losses.

The task of the invention is to eliminate these disadvantages of the known method, ensuring the productivity of the process in the processing of nitrate callistephi solutions by sorption extraction isotopologues thallium, provide clearance thallium impurities on stage sorption and obtain eluates, suitable for the production of high-purity metal thallium electrolysis directly from eluates or its compounds.

The technical result is achieved by the method sorption of thallium on sulfoxylate the cation exchanger, comprising the sorption of thallium from solutions of complex composition and desorption of thallium, while the sorption of thallium lead from nitric acid solutions before sorption original nitrate solution is treated with an organic reducing agent, such as alcohol or formaldehyde solution until a pH of 1.5 to 2.5, enter complexone II or III in the amount of 1.2 to 1.5 mol complexone on 1 mol of the amount of impurities and adjust the solution to pH 4.0 to 5.0 ammonia desorption of thallium are 2-4 M solution of ammonium sulfate or after pre-treatment of the cation from impurities by washing with water and the solution complexone II or III, or with the subsequent purification obtained the donkey desorption eluates on the anion exchange resin epoxypropanol type, for example, EN-31, an organic reducing agent take 3.5-4 fold excess of stoichiometry in relation to the content of nitric acid in the original solution, and washing the cation exchange resin after sorption of thallium are 0.02 M solution complexone II or III with the value of pH of 4.0 to 5.0.

It should be noted that all specified conditions of preparation of the solutions to the sorption provide a high degree of extraction of thallium subject large sorption load of the resin on the extracted metal and achieve high pepsin purity compounds of thallium in the eluate and the final product. In particular, sulfonation can provide high sobiraemosti thallium from his pure nitrate solutions. However, sorption of thallium from solutions with a concentration of nitric acid over 0.5 M sorption of thallium practically does not occur. By neutralizing nitric acid with an alkaline reagent ions appear alkali metal or ammonium, which have competing effects on the sorption of thallium, which ultimately leads to a sharp decrease in the sorption capacity for thallium sulfoxylate cation exchanger. Therefore, the first stage is used as a neutralizing reagent is a reducing agent alcohol or formalin, which destroys nitric acid without the introduction of additional cations. Additional neutralization of the solution to pH 4,0-5,0 determine eleesa the following reasons.

The increase or decrease of pH callistephi solutions below 4.0 or above 5,0 unacceptable. When the pH value of the solutions below 4.0 there is a sharp decrease in solubility complexone II or III and the destruction of nenormiruemym cation exchange resin complex compounds impurities. Increasing the pH of the solution above this limit leads to the formation of positively charged ammonium complexes, such as copper, which are well are sorbed cation exchange resin. Thus, sorption of thallium from solutions with pH less than 4.0 and above 5,0 leads to sorption along with thallium ions of impurities and to obtain eluates contaminated components, impurities and does not give a positive effect.

The use of ammonia as a neutralizing agent due to the fact that ammonium ions have the lowest possible competitive action thallium, while sorption to the concentration of NH4NO30.5 M

The decrease in the ratio of the combined II or III to the amount of the impurities from the stoichiometry of less than 1.2 leads to incomplete binding of impurities in nenormiruemym cation exchange resin complex ion, therefore, sorption latest cation and reduction of the degree of purification of thallium from these impurities. A slight excess complexone II or III is required to ensure complete binding of impurities in naservirujeme connection. The increase in the ratio comp is exon II or III to the amount of impurities in excess of this ratio is not appropriate, because it does not further increase the positive effect and leads to excessive complexone II or III.

When the content in the solution of a large number of impurities with respect to thallium there is a small transition from phase solution in the cation exchanger. Therefore, for complete cleaning of thallium from the admixture of the cation exchanger after sorption of thallium wash solution complexone II or III. High concentration complexone leads to desorption with impurities of thallium and its losses with the washing solution. Low concentration complexone provides complete desorption of impurities while maintaining thallium in the phase of the cation. The pH of the leaching solution in the range of 4.0 to 5.0 provides full binding impurity ions by chelating agents and their desorption from the cation exchanger. Subsequent washing of the cation exchanger water necessary to remove combined with the mother liquor from the phase of the cation.

If necessary obtain high purity thallium or when the content of impurities, such as copper, Nickel, zinc, etc. above the allowable values obtained eluate of ammonium sulfate was filtered through a bed of anion exchange resin epoxypropanol type, for example the anion an-31. While impurities are sorbed anion exchange resin, and thallium passes into the filtrate. This operation can be performed, except the washing of the cation exchange resin KU-2 complexone II or III or Umeda these processes, using purification by ion-exchange resin eluates obtained after desorption of thallium sulfate of ammonium cation exchanger KU-23, washed with a solution of complexone II or III.

Thus, the analysis of the proposed technical solution shows that the distinctive features of the proposed method and achieve this result there is a new cause-and-effect relationship: the presence of these characteristics in the characteristics of the claimed method provides a positive effect, but the absence of these signs does not have effect, the aim of the invention.

In the patent and scientific literature contains no data on sorption of thallium from solutions in the presence of impurities, such as copper, zinc, iron, lead, etc., sorption using complexone II or III with the preliminary neutralization of solutions of organic reducing agents, such as alcohol or formalin, and data cleaning of thallium from impurities by ion-exchange resin epoxypropanol type.

Therefore, the proposed technical solution is characterized by novelty and has significant differences. Comparison of the performance of the proposed and previously known method (prototype) is shown in the examples.

Due to the fact that leaching of thallium nitric acid in the solution formed compounds of the metal article is singing oxidation of +1 in all examples, the data on sorption extraction of T1 (I).

Example 1. In table 1 the results of sorption of thallium (I) from a solution containing thallium 4 g/l at different pH value. Sorption was carried out in dynamic mode at a speed of filtration solutions of 1 ml/min·cm2through the cation exchanger KU-23 loading on the sorbent 10, Conditions and results of sorption are shown in table 1.

Table 1
Sorption of thallium on the cation exchanger KU-23 depending on the pH Osorno acid solution
№ p/pThe pH nitrate solutionDynamic exchange capacity thallium, mg/gFull dynamic exchange capacity thallium, mg/g
10,40,000,00
21,00,02,24
31,51,624,86
42,02,028,96
53,07,1222,00
63,518,7034,02
74,026,0064,17
84,532,2576,19
9 5,041,1593,30
105,565,05EUR 102.11
116,066,13103,73
126,561,1294,30

As follows from the presented data, with increasing pH of the solution increases the capacity of the sulfonic cation exchanger for thallium (I) and reaches its maximum value at pH 6. Thus, sorption of thallium even from individual solutions should be carried out from solutions with pH 4,0 more.

Example 2. This example shows the effect of cations by neutralizing agents on the sorption of thallium. By neutralizing nitric acid alkaline reagents, the formation of salts of the respective metals or ammonium, therefore, to simulate the neutralized solution into the solution of thallium nitrate was dissolved nitrate salts of potassium, sodium, ammonium and calcium in the amount of 0.5 g-EQ/L. Sorption of thallium were from solutions with a pH value of 4.5 with a concentration of T1 (I) - 2.4 g/l under static conditions when the ratio of the mass of the resin to the volume of solution equal to 1:50. The contact time of the solution with the resin for 24 hours. The results of the sorption of thallium are presented in table 2.

Table 2
Sobiraemosti of thallium on the sulfonic cation exchanger KU-23 from nitrate solutions containing ions of potassium, sodium, ammonium and calcium
№ p/pSalt is introduced into a solution of T1 (I)The capacity of the ion exchanger for thallium, mg/gThe degree of extraction of thallium, %
1KPO326,422,0
2NaNO338,2of 31.8
3NH4NO354,745,2
4The N316,0the 13.4
5No additives72,360,3

The obtained data testify to the competing influence of cations on the sorption of thallium, but to a lesser extent inhibits the sorption of thallium ion ammonium, therefore, to neutralize the nitric acid solution before adsorption of thallium should be used as the alkaline reagent solution of ammonia.

Example 3. In the original solution of thallium concentration of metal 4.0 g/l and a pH value of 4.5 was injected different amounts of ammonium nitrate. From the prepared solutions were sorption of thallium on the cation exchanger KU-23 in dynamic mode under the conditions described in example 1. The results of the experiments are presented in table. 3. The data obtained show that HC is the increase in the concentration of ammonium nitrate leads to a significant suppression of adsorption of thallium.

Therefore, from nitric acid solutions with a high concentration of acid after neutralization with aqueous ammonia thallium will absorb small amounts, therefore, to neutralize the main part of HNO3you must apply the reagent, precluding the introduction of cations, in particular organic reducing agents, such as alcohol or formaldehyde, and to bring the pH to the desired value of the ammonia.

Example 4. In the example shown the possibility of using as a reducing agent ethyl alcohol solution of formaldehyde (formalin) for the destruction of nitric acid, therefore, to reduce the acidity of the solution. In the original solution with a concentration of nitric acid of 2 M was added various amount of reducing agent. In the recovered solution to measure the pH value. The data presented in table 4

0,1
Table 4
Data recovery of nitric acid, alcohol and formalin
№ p/pThe reagent is a reducing agentThe ratio of reducing agent: nitric acid from stoichiometryThe pH of the solution after recovery NGO3
1Ethanol1,0
2 2,00,8
33,01,5
44,02,5
5Formalin1,00,2
6 2,00,7
73,01,3
84,01,8

From these results it follows that studied reductants effectively restores nitric acid, which reduces the acidity of the solution and to reduce the consumption of ammonia in the subsequent neutralization of the nitric acid solution of thallium. Fundamentally can almost completely restore nitric acid, but this is not advisable because of the high excess reagent, it is sufficient to introduce the reducing agent into the 3.5-4 fold excess of stoichiometry with respect to nitric acid.

Example 5. Production solutions contain ions of impurities, the main of which is the copper (II). Moreover, the copper concentration reaches 10-12 g/l when the concentration of thallium about 3-4 g/L. Therefore, in this example, the conditions under which copper stops absorb the sulfonic cation of solutions that are close to neutral.

The solution of nitrate of copper, neutralize the Ali ammonia up to pH 5.5 to 6.0, after which he entered the complexone II or complexone III in amounts of 0.8, and 1.0, 1.2 and 1.5 from the stoichiometric ratio. When dissolved chelating agents, the pH of the solution was dropped to 3-3,5, so the solutions was adjusted with ammonia to a predetermined pH 4-5. After adjustments were copper sorption on cation exchange resin by filtration of the solution through a bed of sorbent at a rate of 1 ml/min cm2. After the sorption resin was washed with water and then treated with 4 M solution of ammonium sulfate and determined the concentration of copper in the eluates. Copper content in the eluates defined sobiraemosti copper cation, which are listed in table 5.

Table 5
Sobiraemosti copper (mg/g) on the cation exchanger KU-23 from solutions with different contents of chelating agents and pH
The pH of solutionsThe number entered complexone II from stoichiometryThe number entered complexone III from stoichiometry
 0,81,01,21,50,81,01,21,5
3,515,411,37,16,315,2 the 11.67,06,0
4,013,21,20,40,013,61,10,30,0
4,56,12,40,10,05,82,00,00,0
5,08,33,11,00,78,13,30,80,6
6,010,24,53,63,010,84,23,32,9
6,514,712,37,45,115,012,17,05,5

Thus, the obtained data show that at pH 4-5 and abundant complexone within 1.2 to 1.5 copper cation exchange resin is practically not sorbed. To determine the effect complexone II or III on the sorption of thallium were conducted similar experiments with thallium at pH 4-5 and found that the chelating practically do not change the value of sobiraemosti thallium cation exchange resin (PL. 6).

Table 6
Sorbed the TB thallium (mg/g) on the cation exchanger KU-23 from solutions with different contents of chelating agents and pH
The pH of solutionsThe number entered complexone II from stoichiometryThe number entered complexone III from stoichiometry
 0,81,01,21,50,81,01,21,5
4,065,364,965,665,164,864,865,164,7
4,577,177,076,976,677,3of 76.877,077,1
5,0a 94.293,8a 94.2a 94.293,993,994,0a 94.2

Example 6. For comparison of the proposed and known methods was prepared with nitric acid solution of thallium concentration of the component, g/l: T1 (I) - 4,2; Cu (II) - 10,5; NGO3- 156. The sample was divided into two parts, 1 L. the First half of the solution was treated with alcohol in the amount of 4 l, then the solution was evaporated to 900 ml, in order to save the initial concentration of metal ions was Donatelli ammonia until a pH of 4.5 was added complexone III (2 water) in an amount of 71, After the introduction of combined Ali adjustment of pH with ammonia to a value of 4.5 each of the obtained solutions have missed through the sorption column, loaded with 400 ml of cation exchanger KU-23. In the filtrate was determined by the content of copper and thallium. After the sorption column was washed with water until the absence of copper ions in the wash water, after which he desirerable metal ions from the resin 4 M solution of ammonium sulfate.

Example 7. If thallium procorporate even small amounts of impurities, the main of which is copper, it will degrade the quality of the final product. In experiments it was determined that co-sorption of thallium and copper in the presence of chelating agents in the resulting eluates along with thallium copper is present and its concentration is from 3 to 10 mg/L. In this example, the results for additional purification eluates on the anion an-31. The original structure solution T1 (I) - 9600 mg/l, Cu (II) - 50 mg/l (NH4)2SO4- 400 g/l, pH 4.2 was filtered through a layer of the anion an-31. After sorption, the anion exchange resin was washed with water until no thallium in the wash water. Wash water was combined with the main solution and this has resulted in solutions with a concentration on metal: T1 (I) - 7300 mg/l, Cu - 0.06 mg/L. From this example it follows that additional purification by ion-exchange resin epoxypropanol enables obtaining tallic solutions of high purity.

Example 8. In the original nitrate solution containing thallium (I) to 4.2 g/l and copper - 12 g/l is introduced complexone II with an excess of the stoichiometric ratio of copper to 1.5, neutralized to a pH of 4.5 and was filtered through a bed of cation exchanger KU-23. After that, the resin was washed with 5 volumes of distilled water to 1 volume of resin. After washing the resin was analyzed for copper, the content of which was 4 mg/g of cation exchanger. After that, the cation exchanger was divided into 3 equal parts, was placed in a separate column and each of them was washed with solutions complexone (III) with a concentration of 0.01, 0.02 and 0.03 M and the pH value of these solutions to 4.5. The washing water was analyzed for the content of thallium and copper. Thallium in solutions has not been detected, and the concentration of copper in the leachate in a separate factions reached 200 mg/L. Then spent desorption of thallium and identified in the eluates concentrations of metals. The results are shown in table. 7. As follows from the obtained results during sorption of thallium on the sulfonic cation exchanger KU-23 without the introduction of complexone III the degree of extraction of thallium is very low (24%) compared with the proposed method (about 100%).

In addition, when using the proposed method achieved a high degree of purification of thallium on copper, which amounts to 30,000 times, while the known method not only cleans thallium on copper, but is enriched eluates by Cu (II). This example illustrates a significant advantage of the proposed method of extraction and purification of thallium from impurities in comparison with the known.

Table 7
Sorption extraction of thallium in the presence of copper ions on the cation exchanger KU-23 from solutions with addition and without adding complexone III
Sorption from solutions by adding complexone IIISorption from solutions without adding complexone III (prototype)
The content of metal ions in the filtrate, gThe content of metal ions in the wash water, gThe content of metal ions in the eluate, gThe degree of extraction of thallium, %The degree of purification of thallium from copperThe content of metal ions in the filtrate, gThe content of metal ions in the wash water, gThe content of metal ions in the eluate, gThe degree of extraction of thallium, %The degree of purification of thallium from copper
T1 (I)Cu (II)T1 (I)Cu (II)T1 (I)Cu (II)  T1 (I)Cu (II)T1 (I)Cu (II)T1 (I)Cu (II)  
0,00710,15 0,00051,844,190,0004~100300002,864,650,341,141,016,2224,050,46

Example 9. In the original nitrate solution containing thallium (1) - 4 g/l and copper - 12 g/l is introduced complexone III with an excess of the stoichiometric ratio of copper to 1.5, neutralized to pH 4.5 and was filtered through a bed of cation exchanger KU-23. After that, the cation exchange resin was washed with 5 volumes of distilled water. After washing the cation exchange resin was analyzed for copper, the content of which was 4 mg/g of cation exchanger. After that, the cation exchanger was divided into 3 equal parts, was placed in a separate column and each of them was washed with solutions complexone (III) with a concentration of 0.01, 0.02 and 0.03 M and the pH value of these solutions to 4.5. The washing water was analyzed for the content of thallium and copper. Thallium in solutions has not been detected, and the concentration of copper in the leachate in a separate factions reached 200 mg/L. Then spent desorption of thallium and identified in the eluates concentrations of metals. The results are shown in table. 8

Table 8
The effect of the concentration complexone in wash solutions for purity tallic eluates
p/the Content complexone III in the washing solution, MThe concentration of metal ions in the eluates, mg/l
  1Cu
10,0143000,8
20,0243100,05
30,0343000,04

From the experimental results it follows that the solution complexone III with a concentration of 0.02 M quite effectively desorption of naturally copper from the cation exchanger, i.e. backwashing the combined may be used as the cleaning operation is equally as filter eluates through the anion an-31.

Example 10. Nitrate solutions isotope production composition by major component, g/l: NGO3- 130; T1 (I) - 4,04; Cu - 11,7; Pb - 0,4; Sn - 0,05; Zn - 0,8; Ni - 0,9; Fe - 2,4, volume 14 l was treated with 800 ml of ethyl alcohol. After treatment, the pH value was 2.2. Then made the adjustment of the pH of a 25%ammonia solution to 5.5. In the resulting solution was introduced complexone III with an excess of 1.5 from the stoichiometric ratio for all impurities and again brought the pH to 4.5 with ammonia. After complete dissolution complexone III prepared solution pass through the layer of cation exchange resin KU-23 volume 2 l (700 g). After the end the of cation sorption washed 8 l of water. After washing the spent desorption of thallium 3 M solution of ammonium sulfate. When desorption eluate were selected fractions 5 l composition of the obtained eluates are presented in table. 9.

Table 9
The composition of the eluates after desorption of thallium from the cation exchanger KU-23 C M solution of ammonium sulfate
No. factionVolumeThe content of metal ions in the eluate, mg/l
eluatesfaction, lT1CuZnFePbSnNi
15150055320<0,75<a 7.1<0,0051,5
259100of 5.40,7<0,750,58<0,0052,4
354700,430,72<0,75being 0.036<0,0053,7

These results showed that the first step of purification of thallium has been remarkably effective cleaning T1 (I) from the main mass of impurities, but in the eluates were relatively large numbers the creation of copper, zinc and Nickel, so for purification eluates joined them and was filtered through a layer of weakly basic anion exchange resin an-31 volume of 1 liter Volume of the first fraction of the eluates was 12 l, the second fraction - 3 HP After the process is complete, the cation EN-31 washed 9 l of water and the wash water was combined with the second fraction. The results of the analysis of the obtained solutions are presented in table. 10.

Table 10
The composition tallic solutions further purified on an anion-31
No. of fractions

eluates
Volume

faction, l
The content of metal ions in the eluate, mg/l
T1CuZnFePbSnNi
11221000,070,52<0,750,093<0,005<0,05
23+9=1226000,020,05<0,750,051<0,005<0,05

As a result of these experiments it was shown that this solution provides a high degree of purification of thallium from impurities, direct you the ode over 99%.

Example 11. The original solution, prepared according to the method described in example 10, was filtered through a cation exchanger KU-23. Next, the resin was washed with 4 volumes of water per 1 volume of the cation exchanger. After water washing, the resin was washed with 5 l of 0.02 M solution complexone III. Next, the resin was washed with 4 l of water and held desorption of thallium 3 M solution of ammonium sulfate. The composition of the obtained eluates are shown in table. 11.

>2
Table 11
The composition of the eluates after desorption of thallium from the cation exchanger KU-23 C M solution of ammonium sulfate with a clean-up operation of the sorbent by washing the complexone III
No. of fractions

eluates
Volume

faction, l
The content of metal ions in the eluate, mg/l
T1CuZnFePbSnNi
1525602,3>0,05>20,04>0,05>0,05
2543900,5>0,05>20,06>0,01>0,05
3543900,3>0,05>0,05>0,01>0,05

Thus, it is shown that the washing of the combined cation provides a high degree of purification of thallium from impurities, and the second stage adsorption on the anion an-31.

Feasibility the implementation of this invention is to reduce the number of operations and reagent consumption, emission of harmful substances into the atmosphere, increasing productivity. The technology for the proposed method it is possible to use standard equipment without additional training.

1. The way sorption of thallium on sulfoxylate the cation exchanger, comprising the sorption of thallium from solutions of complex composition and desorption of thallium, characterized in that the sorption of thallium lead from nitric acid solutions before sorption original nitrate solution is treated with an organic reducing agent, such as alcohol or formaldehyde solution until a pH of 1.5 to 2.5, introducing complex II or III in the amount of 1.2 to 1.5 mol complexone on 1 mol of the amount of impurities and adjust the solution to pH 4.0 to 5.0 ammonia desorption thallium lead 2-4M solution of ammonium sulfate or after pre-treatment of the cation from impurities by washing with water and the solution complexone II or III, or with the subsequent purification of the obtained settlement is e desorption eluates on the anion exchange resin epoxypropanol type, for example, EN-31.

2. The method according to claim 1, characterized in that the organic reducing agent take 3.5-4-fold excess of stoichiometry in relation to the content of nitric acid in the original solution.

3. The method according to claim 1, characterized in that the washing of the cation exchanger after sorption of thallium are 0.02 M solution complexone II or III with the value of pH of 4.0 to 5.0.



 

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