SU866416A1 - Method of chromatographic separating of scandium - Google Patents

Description

(54) METHOD OF CHROMATOGRAPHY DEDICATION OF DKANDIUM

 The invention relates to the field of separation of scondi from perchloric acid solutions by the method of extraction chromatography during chemical analysis of natural objects of complex composition containing zirconium, iron, aluminum, rare-earth elements (REE, titanium, chromium, silicon, alkaline and alkaline-earth elements. The invention can be used for metallurgical and machine-building enterprises in the implementation of chemical control of rare elements, as well as the products of enrichment and processing of ores. Small amounts of scandium from complex natures of objects containing Fe, A1, Zr REE, Tf, Cr 2. The method involves the sequential separation of the accompanying elements by sedimentation, extraction, separation chromotogram and. First, scandium along with other metals is separated from alkaline , alkaline earth elements and magnesium by precipitation with ammonia. Then alkali is separated from atmospheric hydroxides, for example, aluminum and chromium, the precipitate of non-amphoteric hydroxides together with fcp is dissolved with hydrochloric acid, kupferon is introduced and kstragirukp; chloroform Fe, Ti, Zr and some other elements. Scandium is then concentrated by coprecipitation with yttrium ammonium tartrate. In this case, separation from a small number of elements remaining from the previous operations is achieved. The separation of the scandium from the carrier is carried out by distribution chromatography or extraction with tenoyl trifluorocenton. In the final solution, scandium is quantitatively determined by the photometric method with xylenone orange GP. The disadvantage of this method is the use of time consuming and lengthy operations, as well as the need for a strictly maintained separation condition. The closest to the invention to the technical essence and the achieved result is a method of separating scandium from natural objects containing Zr, REE, Fe, A1, Ti, Cr, Cu, etc., using ion-exchange chromatography, Dp of sequential separation of scandium from accompanying elements three ion exchange columns are used. First, scandium together with other metals is condemned by ammonia, separated from alkaline and alkaline-earth elements. The hydroxides are dissolved in 3M HC 1 and the solution is passed through a column with a Dowex 50 W x 8 cation in the N form at a rate of 0.7 MP / min. At the same time, A1,. REE, Zr. and Sc is sorbed, and Cr, Cu, Fe and T1 are passed with the eluate. Scanning is carried out with a mixture of 0, 3M ammonium sulphate and 0.025 M sulfuric acid B. the eluate containing So partially transforms Fe ° H Al, from which a Daux 1x8 anion exchanger in a sulphate form is used. Fe and A1 impurities are removed by washing the sorbent with a certain volume of a mixture of 0.1 M ammonium sulfate and 0.025 M Nl 50 Scandi-desorb with another portion of the same solution. Dp concentrated NINS Sc is added to the last eluate and Fe is precipitated with Sc and Fe with a miak solution. Hydroxide is dissolved in 6 M HC and the solution is passed through a Dowex 1x8 anion exchange resin in C1 form. At the same time, iron is retained on the column, and scandium passes into the eluate. The eluate is evaporated and scandium is quantitatively determined by the photometric method with arsenazo 1 G23.

The disadvantage of this method is the low selectivity of Sc, the use of three ion-exchange columns, as well as large quantities of washing solutions, which necessitates an additional step of concentrating scandium before quantifying

The purpose of the invention is to increase the segmentation of scandium and simplify the method.

The goal is achieved by the fact that in the known method of chromatographic scandium separation from waste of zirconium production, including sorption and subsequent desorption, sorption is carried out from

Example 1. A hydrochloric acid process solution, obtained from wastes of zirconium production, containing 0.01–15 mg, is evaporated to wet salts, which are dissolved in 10 ml of 5 M HCW when heated in a water bath, and passed through a column with a sorbent ( 2 g of siliconized silica gel and 1.2 ml of TBP), prewashed with 10 ml of 5M .. Accompanying scandium Zr, Fe, Al, REE, Ti, Cr, alkaline and alkaline earth elements elute 10 ml of the same acid. Scandium is drawn from a sorbent of 10 ml of 0.01 M H1. Elc) At sc with Sc collected in a volumetric flask with a capacity of 50 ml and quantitative determination of Sc by the photometric method., With xylenol orange by a known method. of tributyl phosphate solution, deposited on siliconized silica gel, and desorption - on dilute hydrochloric acid. The separation of Sc from Zr, P33, Fe, Al, Or, Ca, etc. was carried out in a glass column with a diameter of 10 mm and a height of 100 mm, into which 3.2 g of sorbent were placed (2 g of siliconized KSK silica gel and 1.2 ml of tributyl phosphate (TBP). The rate of passage of the solutions was 2 ml / min. A solution of 5 M perchloric acid, containing the elements to be separated, was passed through a layer of sorbent, which was washed with elution solutions: 5 M HC104 and 0.01-0.5 M HC1. As it was established, since the distribution coefficients of Zr, REE A1, Fe, Cr, Ti, alkaline and alkaline-earth elements in the TBP system C10 0, 5, a, the latter is firmly held by the sorbent, while the accompanying elements are washed out of the column with small volumes of the eluate. Separation was carried out in 5M NSPO. Ca, etc., requires about 10 ml of L M CH10. 10 ml of 0.01 — 0.5 M CH1 is sufficient for elution of sorbed scandi. The content of concomitant elements in the isolated concentrate Sc does not exceed the allowable values for the quantitative determination of So by reagents arsenose 1 and xylenol orange. Example 2. Technological sulphate or nitrate solution obtained from waste of zirconium production, containing 0,0115, 0 mg, heated to 70-80 ° C, ammonia precipitated hydroxides Sc, Zr, Fe, Al, REE, Ti, Cg, which is washed hot water to remove NOJ and 50 ions. The precipitate is dissolved in 10 ml of 6M HC10 when heated in a water bath and passed through a sorbent bottle (2 g of condensed silica gel and 1.2 mp TBP) previously washed with 10 MP 5M HC. Od. Accompanying scandium Zr, Te, A1, REE, Ti, Cr eluted 10 MP of the same acid. Scandium is eluted with 10 ml of 0.5 M HC1. The eluate is collected in a 50 MP volumetric flask and quantitated by the photometric method. xylenol orange by a known technique. The proposed method is different. . due to the large capacity of the extractant and the ability of the siliconized silica gel to hold the extractant firmly, in particular tributyl phosphate, a small column can be used

Pass the eluate through Dowex 1x8 in SO form

Washing with a mixture of 0.1 M (NH4) S04 + 0.025 M

Sorbate 20

30 A1, REE, Zr, Sc.He adsorb Cg, Cu, Fe, Ti

Eluate: Sc20

thirty

(partially Fe, Al) yyyy Al, REE sorbed

thirty

65 186 66 to produce a large number of separations without replacing the sorbent. The proposed method is much easier known. It uses only one ion exchange column and two washings. Instead of eight operations in the well-known in the proposed method, three are used, the duration of the operations is 25 times less than in the well-known one. Since it is expensive (the price of I kg Zs Och is 2.5 thousand rubles) and an indispensable metal for the development of new technology, the presence of such a simple and selective method of scandium separation from complex chemical components of technological solutions opens up great opportunities for the radiation of its behavior during the processing of various Sc - containing concentrates and the cure of numerous dump products. Table 1 shows the ion-exchange separation of scandium from natural objects containing Zr, Fe, Al, REE, C g, - Ti, Cu, alkaline and alkaline-earth elements. Table 2 shows the extradio-photographic scandium extraction from technological solutions containing Zr, Fe, Al, PZE, Cr, TI, alkaline and alkaline-earth elements. Table 1

Addition of 10 mg Fe Fa Sc Sc

C. eloatu with Sc and NNDON precipitation

Sc + Fe solution

PacTBOperaie sediment in 6M HCI

Passing the solution Sorbed Fe, Yu 15 (6) through a Dowex 1x8 Sc eluate in a C1 form

Continued table. I

15

ten

15

table 2

Claims (2)

Claim , 1. The method of chromatographic isolation of scandium from technological solutions, including sorption of scandium and its selective desorption, except that in order to increase the selectivity of scandium isolation and simplify the method, sorption is carried out from 5-6 molar perchloric acid solution on silica-coated silica gel with tributyl phosphate * deposited on it, and desorption is carried out with dilute hydrochloric acid / VNIIPI Order 8060/64 ._____ Total 15 minutes ________ 2. The method according to claim ₀ 1, which is based on the fact that the desorption of scandium is carried out with a 0.01-0.5 M hydrochloric acid solution.