Method for sorption extraction of iron from nitrate salt solutions

FIELD: chemistry.

SUBSTANCE: invention relates to ion exchange and can be used for sorption extraction of iron from salt solutions formed when processing aluminium-containing material using acid techniques. Extraction of iron to residual content of Fe2O3 in the purified solution of not more than 0.001% is carried out through sorption of iron with a cationite in H-form, containing aminodiacetic functional groups. The iron sorption and desorption steps are alternated without intermediate washing of the cationite. Iron is desorbed in counterflow conditions with nitric acid solution.

EFFECT: method enables elective extraction of iron, reduces acid consumption and prevents loss of aluminium in the process.

3 cl, 1 tbl, 6 ex

 

The invention relates to the field of processes of sorption removal of impurities from solutions, as well as to the processing of aluminium-containing raw materials by acid methods.

Decomposition of aluminium-containing raw materials, in particular of nepheline, acids pass into the solution ions of aluminum, sodium, potassium, iron and other elements. The resulting salt solution processed into marketable products: alumina of different grades, aluminum hydroxide, and others. In accordance with the technical requirements for metallurgical alumina ratio of Al2About3/Fe2About3must be at least 3500. To achieve the specified relationship is the deep treatment of a solution of salts of iron.

Decomposition of aluminium-containing raw material with nitric acid mass fraction of iron in terms of oxide Fe2About3in the solution of nitrate salts coming on the stage of cleaning is 0,01-0,10%, the residual iron content in the solution after treatment in terms of Fe2O3should be not more than 0.001%.

The most comprehensive treatment of aqueous solutions of iron provide sorption methods using liquid and solid adsorbents.

A known method of extraction of iron ions from acidic aluminium-containing solutions is ion-exchange sorption (extraction) of high molecular weight fatty the acids, for example stearic, and salts of these acids. (Waaler. Complex processing of aluminium-containing raw materials by acid methods. S-136.) Another method consists in the extraction of iron ions naphthenic acids. (A.S. USSR. No. 513006. "Method of purification of acidic solutions of salts of non-ferrous metals from iron compounds". Published 05.05.76 g) the Ratio of Al2About3/Fe2About3in solutions after cleaning these methods reaches 2500-3000. The disadvantages of these methods are:

- the complexity of the hardware design process;

- insufficient regeneration of the extractant nitric acid and, as a consequence, a gradual decrease of the effect of extraction of iron;

- the ratio of Al2About3/Fe2About32500-3000 get only after three successive stages of refinement.

A known method of removing iron ions from acidic aqueous solutions of nitrate, sulfate or aluminum chloride with a liquid ion exchange extractant containing di(2-ethylhexyl)-phosphate (DEHHP) and tributyl phosphate or a primary amine (U.S. patent 3586477 published 16.10.68 year). The disadvantage of this method is that the content of Fe2About3in purified solution is not less than 0,0035%, in addition, requires a large consumption of organic extractant (1 volume 2-10 volumes of the processed solution), the process is egenerali which is not specified.

There is also known a method of extracting Nickel from acidic production of solutions containing iron at pH 1-2 using cation exchange resin (cation) chelate type with functional groups of bis-(2-pyridylmethyl) amine (patent RF №2352654 published, 20.04.09). This method is designed to extract the target product and inefficient for deep purification of acidic solutions of iron.

The known method of ion exchange with cation exchange resin containing phosphonate functional group, and the regeneration of the cation exchange resin for the extraction and removal of iron from the sulfuric acid solution containing metal ions (U.S. patent 5582737 published 07.11.95 year). This method is used to remove iron from the electrolyte solution during electrolytic recovery of copper. Regeneration of the cation exchanger includes catalytic reduction of ions of trivalent iron to divalent ions with the use of copper ions and sulfurous acid. This method is not practicable in other processes, in particular when azotnokislogo processing of aluminium-containing raw material, which is a disadvantage of this method.

Thus, information on the process of extracting iron from solutions of nitrate salts containing aluminum, the adsorption is absent. Analogues proposed izaberete who their authors are unknown.

The technical result, which directed the present invention is to extract iron from solutions of nitrate salts containing aluminum, to a residual content of iron in terms of oxide Fe2About3not more than 0.001%, obtaining relations Al2O3/Fe2O3in purified solution is not less than 3500 and implementation of the cleanup process without waste.

This object is achieved in that according to the proposed method the extraction of iron from solutions of nitrate salts containing aluminum, to a residual content of Fe2O3in purified solution is not more than 0.001% is held by selective sorption of iron on the cation exchanger containing iminodiacetate functional groups in the H form, stage sorption and desorption of iron alternate without intermediate washing of the cation, the desorption of iron from the cation exchange resin is carried out in counter-current mode with a solution of nitric acid, the nitric acid solution after desorption of iron is returned to the production process, the purified solution with the ratio of Al2About3/Fe2About3not less than 3500 goes for further processing.

The use of counterflow mode desorption of iron from the cation exchanger and an exception stages of washing of the sorbent before desorption eliminates loss of the target product - Alu is INIA - and the need for disposal of acid wash water. The return of the nitric acid solution after desorption of iron from the cation to the stage of decomposition of the raw materials or other stage makes waste, reduces consumption of acid and to avoid the loss of aluminum.

The process of extracting iron from solutions of nitrate salts containing aluminum, and desorption of iron from the cation exchange resin is carried out at a temperature of solutions is not more than 70°C. When the temperature of the solutions above 70°C possible thermal and mechanical destruction of the cation.

Desorption of iron from the cation exchange resin is a solution of nitric acid with a concentration of 8-12%, with no negative effect of nitric acid on the cation exchanger and ensures efficient extraction of iron from the cation exchanger.

New and significant in the proposed technical solution is:

- the use of a cation exchange resin containing iminodiacetate functional groups in the protonated form, for the sorption of iron from solutions of nitrate salts containing aluminum;

- carrying out desorption of iron from the cation exchanger in counter-current mode using solutions of acids that are used in the decomposition of raw materials, including nitric acid;

exception stages of washing the cation exchange resin before and after desorption.

The claimed technical solution is based on the use of available IO obmennoi resin. The method of sorption extraction of iron from a solution of nitrate salts containing aluminum, cation-exchange and desorption of iron from the cation exchange resin characterized by its simplicity of execution and eliminates loss of the target product is aluminum. If the process does not generate waste.

Below are examples of the method of sorption extraction of iron from solutions of nitrate salts containing aluminum, the cation exchanger Purolite S930, manufactured by Purolite international limited. To implement the proposed method can be used similar cation containing iminodiacetate functional groups, other manufacturers of resins, under other brand names, the results will not change.

Example 1. The solution of nitrate salts containing 4.2% of aluminum nitrate in terms of oxide of Al2About3, 0,021% of iron in terms of oxide Fe2O3and 6.5% of the amount of nitrates of sodium, potassium and other elements, was filtered at the solution temperature of 25°C. through a column loaded with 0.1 DM3cation-exchange resin Purolite S-930 with iminodiacetate functional groups in the protonated form. The purified solution was selected portions and analyzed for iron content. The results of the analysis calculated the ratio of Al2About3/Fe2About3in a purified solution. The process is carried out is about increasing mass fraction of Fe 2About3the filtrate more than 0.001%. The volume of the purified solution was 6.4 DM3or 64 volume 1 volume of the cation exchanger. Then there was the desorption of iron from the cation exchange resin with a solution of nitric acid with a concentration of 10 wt%. in the amount of 0.3 DM3. Upon completion stage of desorption, the cation exchange resin used for the purification of a solution of nitrate salts, without leaching. The purified solution of nitrate salts were received for further processing, the spent nitric acid solution after desorption of iron from the cation exchanger was returning to the stage of decomposition of the raw material.

Example 2. The solution of nitrate salts containing 4.2% of aluminum nitrate in terms of oxide of Al2O3, 0,0275% of iron in terms of oxide Fe2About3and 6.5% of the amount of nitrates of sodium, potassium and other elements, was filtered at the solution temperature of 65°C. through a column loaded with 0.1 DM3cation-exchange resin Purolite S-930 with iminodiacetate functional groups in the protonated form. The purified solution was selected portions and analyzed for iron content. The results of the analysis calculated the ratio of Al2About3/Fe2About3in a purified solution. The process is carried out to increase the mass fraction of Fe2About3the filtrate more than 0.001%. The volume of the purified solution was 5.9 DM3or 59 volumes to 1 volume of the cation exchanger. Then conducted on the sorption of iron from the cation exchange resin with a solution of nitric acid with a concentration of 10 wt%. in the amount of 0.3 DM3. Upon completion stage of desorption, the cation exchange resin used for the purification of a solution of nitrate salts, without leaching. The purified solution of nitrate salts were received for further processing, the spent nitric acid solution after desorption of iron from the cation exchanger was returning to the stage of decomposition of the raw material.

Example 3. From a solution of nitrate salts containing 4.3% of aluminum nitrate in terms of oxide of Al2About3, 0,048% of iron in terms of oxide of Fe2O3and of 6.65% of the amount of nitrates of sodium, potassium and other elements, pull the iron through cation exchange resin. Stage sorption process, desorption of iron from the cation exchange resin, the processing of the purified solution of nitrate salts, the return of spent nitric acid solution after desorption of iron from the cation to the stage of decomposition of the raw materials was carried out similarly to example 1. The volume of the purified solution was 3.5 DM3or 35 volumes to 1 volume of the cation exchanger.

Example 4. From a solution of nitrate salts containing 4.3% of aluminum nitrate in terms of oxide of Al2O3, 0,048% of iron in terms of oxide Fe2About3and of 6.65% of the amount of nitrates of sodium, potassium and other elements, pull the iron through cation exchange resin. Stage sorption process, desorption of iron from the cation exchange resin, recycling PTS the seal solution of nitrate salts, the return of spent nitric acid solution after desorption of iron from the cation to the stage of decomposition of the raw materials was carried out similarly to example 2. The volume of the purified solution was 3.4 DM334 volume 1 volume of cation exchange resin.

Example 5. From a solution of nitrate salts, containing 4.5% of aluminium nitrate in terms of oxide of Al2About30,077% of iron in terms of oxide Fe2About3and 6,70% of the amount of nitrates of sodium, potassium and other elements, pull the iron through cation exchange resin. Stage sorption process, desorption of iron from the cation exchange resin, the processing of the purified solution of nitrate salts, the return of spent nitric acid solution after desorption of iron from the cation to the stage of decomposition of the raw materials was carried out similarly to example 1. The volume of the purified solution was 2.5 DM3or 25 volumes to 1 volume of the cation exchanger.

Example 6. From a solution of nitrate salts, containing 4.5% of aluminium nitrate in terms of oxide of Al2About3, 0,048% of iron in terms of oxide Fe2About3and 6,70% of the amount of nitrates of sodium, potassium and other elements, pull the iron through cation exchange resin. Stage sorption process, desorption of iron from the cation exchange resin, the processing of the purified solution of nitrate salts, the return of spent nitric acid solution after desorption VC is for from the cation to the stage of decomposition of the raw materials was carried out similarly to example 2. The volume of the purified solution was 2.6 DM3or 26 volumes to 1 volume of the cation exchanger. The results of examples 1-6 are presented in the table.

no experienceThe temperature of the solution of nitrate salts, °CFe2About3in the original solution, %Fe2O3in the solution after treatment (average), %The amount of purified solution/volume of the cation exchangerAl2About3/Fe2About3after cleaning
1250,0210,00068606176
2650,02750,00060597000
3250,0480,00082355244
4650,0480,00079345443
5250,0770,00086255233
6650,0770,00089265056

1. The method of sorption extraction of iron from solutions of nitrate salts containing aluminum, which consists in the fact that the extraction of iron to a residual content of Fe2About3in purified solution is not more than 0.001% is carried out by selective sorption of iron cation exchange resin containing iminodiacetate functional groups in the protonated form, stage sorption and desorption of iron alternate without intermediate washing of the cation, the desorption of iron from the cation exchange resin is carried out in counter-current mode with a solution of nitric acid, the nitric acid solution after desorption of iron from the cation exchanger back into the production process, the purified solution with the ratio of Al2About3/Fe2About3not less than 3500 serves for further processing.

2. The method according to claim 1, characterized in that the temperature of the solutions of nitrate salts containing aluminum in contact with the cation exchange resin, does not exceed 70°C.

3. The method according to claim 1, characterized in that the desorption relesaes cation exchanger is conducted with a solution of nitric acid of a concentration of 8-12%.



 

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1 tbl, 1 ex

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