Procedure for extraction of niobium from water solution containing fluorine

FIELD: metallurgy.

SUBSTANCE: procedure for extraction of niobium from water solution containing fluorine consists in sorption by contacting solution and anionite. Anionite is subjected to acidic or water treatment before sorption. Sorption is carried out with anionite of grade ANP containing exchange groups at pH=2-4.

EFFECT: optimal conditions for fast and efficient procedure for niobium extraction out of water solution containing fluorine.

4 dwg, 2 tbl, 3 ex

 

The method of extraction of niobium fluoride aqueous solution relates to the field of extraction of substances with the use of sorbents and can be used in ferrous and nonferrous metallurgy, as well as for the treatment of industrial and domestic wastewater.

It is known the use of ion exchange resins for processing solutions integrated (HF) anions niobium [R. Ripen and I. Kitano. Inorganic chemistry. Volume 2. Chemistry of metals. M.: Mir. 1972. .183]. To this end, apply a strongly basic anion exchange resin followed by elution of the niobium solution of NH4Cl and Hcl.

The disadvantage is that no sorption of fluoride-niobates from aqueous solutions by ion-exchange resin brand AMP.

The closest technical solution is the method of extraction of niobium fluoride aqueous solution, including sorption by contacting the solution and the anion brand AMP [Lebedev K.B. Ion exchangers in nonferrous metallurgy, M., metallurgy, 1975, s].

The disadvantage of this method is that it is not given optimal conditions sorption of niobium fluoride aqueous solutions by ion-exchange resin brand AMP.

Task to be solved by the claimed invention is directed, is to find the optimum conditions for rapid and effective method of extraction of niobium in the form of anion NbF72-of the fluorine-containing aqueous solution.

Technical R is the result, which can be achieved by implementation of the invention is the efficiency of the process of adsorption of anion NbF72-of the fluorine-containing aqueous solution.

This technical result is achieved by the known method of extraction of niobium fluoride aqueous solution, including sorption by contacting the solution and the anion brand AMP, before sorption conduct preliminary acid or water processing anion-exchange and sorption of lead at pH=2-4 anion exchange resin containing exchange group

The essence of the method is illustrated in the data of table 1 and table 2 and figures 1 - 4, where there are dependencies residual concentration of niobium, mg/DM3and sorptive exchange capacity (SOY) sorbent, mg, Nb on 1 g of sorbent, from the time of sorption, h, pH and method of pre-treatment sorbent.

Examples of specific implementation method

Sorption Nb was obtained from 100 cm3the original solution of K2NbF7the mass of sorbent 1, the Sorbent previously in the day was kept at 0.1 N. solutions of NaOH, HCl or distilled water.

Gel strong basic anion exchanger AMP with a spherical granules obtained by aminating HMS styrene and 3.5 to 4.0% DVB pyridine. The particle size of the granules 0,63-1,60 mm; specific volume of the swollen resin of 2.7-2.9 cm3/g, the mechanical strength of 98-99%; OYe 3,3-3,7 mg-ekvg. Exchange group:

The concentration of ions of niobium was determined on the photocolorimeter brand KFK-3, and acid-base characteristics of the solution was controlled by a pH-meter pH-121.

In the absorption process of mixing and maintaining the set value of pH was carried out until a constant value SOY sorbent, testified to the occurrence of sorption equilibrium.

Sorption was carried out at room temperature.

Using the values of the concentrations of niobium ions in aqueous solution source and after sorption, the expected SOYBEAN, mg/g

Example 1 (1)

Figure 1 from a solution with an initial concentration of 500-900 mg/DM3Nb given according SOY, mg/g of sorbent from the pH and pre-treatment sorbent (graphics processing sorbent: 1 acid, 2 - water, 3 - alkaline to pH interval=1-6.

Research has shown that the best results were obtained at pH=2-4 at acidic or aqueous processing of the sorbent. Through the day, sorption, there is a slight precipitate. In the case of the alkali treatment of the sorbent, as well as at pH=5-6 with aqueous or acidic treatment of the sorbent solution became turbid immediately, as soon as there was contact of the sorbent and solution, and in the process of sorption soon fell sediment. The appearance of turbidity in the solution reduces the results of sorption.

Example 2 (table 1, figure 2).

the Sorbent previously in the day was kept at 0.1 N. the solution is Hcl.

In table 1 and figure 2 are given the results of sorption Nb ions at pH=4 within 24 hours of adsorption and the initial concentration 979-2994 mg/DM3. It is seen that at pH=4 and acidic treatment of the sorbent best results sorption obtained at the time of sorption of no more than 3 hours. It is established that SOY sorbent increases with increasing concentration of the original solution, when the concentration of the initial solution 2555 mg/DM3Nb SOY=160 mg/g

Example 3 (table 2 and figure 3).

Sorbent previously in the day was kept in distilled water.

In table 2 and figure 3 are given the results of sorption Nb ions at pH=3 within 24 hours of adsorption and the initial concentration 979-2994 mg/DM3. It is seen that at pH=3 and water handling sorbent best results sorption obtained at the time of sorption of less than 4 hours when there is no clouding of the solution. It is established that SOY sorbent increases with increasing concentration of the original solution, when the concentration of the initial solution 2555 mg/DM3Nb SOY=149 mg/g

Figure 4 according to table 1 and table 2 and figure 2 and 3 shows the isotherms of sorption - dependence SOY, mg/g of sorbent from the equilibrium solution concentration, mg/DM3Nb, at acidic (figure 1) and water (graph 2) treatment of the sorbent for the sorption time 4 hours

From the data table. 1 and 2 and figure 1-4 shows that at room temperature the results of the sorption depend on before kiteley processing sorbent, the initial solution concentration, pH of the solution in the process of sorption and sorption time.

Compared with the prototype sorption on ion-exchange resin brand AMP under optimal conditions is a quick and effective method of extraction of niobium ions of the fluorine-containing water solutions.

Table 1
The dependence of the residual ion concentration Nb from the time of adsorption and the initial concentration of the solution at acidic treatment of the sorbent, pH=4
Time, hResidual concentration, mg/DM3Nb
09791535194225552994
169261121011292799
241255107710531931
344247/td> 57510211509
4--5869561585
24-2395469611384

Table 2
The dependence of the residual ion concentration Nb from the time of adsorption and the initial concentration of solution in water handling sorbent, pH=3
Time, hResidual concentration, mg/DM3Nb
09791535194225552994
182299119113081877
288285 114512811828
38528069712481688
4--59410641541
24-25663010701557

Method for the recovery of niobium from a fluorine-containing aqueous solution, comprising the sorption by contacting the solution and the anion brand AMP, characterized in that before sorption conduct of acid or water processing anion-exchange and sorption of lead at pH 2-4 anion exchange resin containing exchange group



 

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