Composition of extraction chromatographic material for selective separation of u(vi), th(iv), np(iv) and pu (iv) from nitric acid solutions

FIELD: chemistry.

SUBSTANCE: invention relates to field of recycling of radioactive solutions. Composition of extraction chromatographic material for selective separation of U(VI), Th(IV), Np(IV) and Pu(IV) from nitric acid solutions contains three components. As complexants composition contains 33% of methyltrioctylammonium nitrate (MTOAN) and 1-16% of phosphoryl podand. As matrix composition contains macroporous spherical granulated copolymer of styrene with divinylbenzene. As phosphoryl podand used are derivatives of 1,5-bis[2-(oxyethoxyphosphoryl)-4-(alkyl)phenoxy-3-oxapentane of general formula I , where Alk is alkyl C1-C12.

EFFECT: extension of spectrum of highly efficient selective sorbents for extraction of U(VI), Th(IV), Np(IV) and Pu(IV) from nitric acid solutions.

8 dwg

 

The high radioactivity of the solutions obtained in the processing of irradiated nuclear materials, puts forward a number of specific requirements to the methods of division and separation of their components. These methods should have a high selectivity and versatility, i.e., must be suitable for the separation of components of solutions with a wide variety of their composition, to vary the utmost simplicity and the possibility of application of remote technology for their implementation. To the greatest extent this can be achieved by a method of extraction chromatography using sorption materials of various types. As known sorbents do not always possess the necessary characteristics, the development of new compositions and highly efficient extraction chromatographic materials is of great interest.

The present invention relates to the field of chemical technologies for processing of radioactive solutions obtained in the processing of irradiated nuclear materials, namely, compositions extraction chromatographic materials obtained by applying (impregnation) organic ion-selective complexing compounds in organic and inorganic matrix.

The aim of the invention is to increase the selectivity of separation of U(VI), Th(IV), Np(IV) the Pu(IV) from nitric acid solutions, obtained by dissolution of irradiated nuclear materials in nitric acid.

The closest analogues of the properties to the proposed technical solution is the sorbent brand TEVA Resin" produced by the company "Eichrom Technologies, Inc", where as the complexing component is used methyltrioctylammonium nitrate (MEAN), and the matrix is a copolymer of styrene with divinylbenzene. [1. E. R. Horvitz, R. Chiarizia, M. L. Dietz, H. Diamond, and D. Nelson. "Separation and Preconcentration of Actinides from Acidic Media by Extraction Chromatography", Analytica Chimica Acta, 281 (1993) 361-372. 2 E. P. Horwitz and Maxell, Sherrod L. et al. "Separation and Preconcentration of Actinides by Extraction Chromatography Using a Supported Liquid Anion Exchanger: Application to the Characterization of High-Level Nuclear Waste Solutions", Analytica Chimica Acta, 310 (1995) 63-78.].

The disadvantages of sorbent TEVA Resin for the separation of U(VI), Th(IV), Np(IV) and Pu(IV) from nitric acid solutions include the low partition coefficients of these elements, solubility MEAN in nitric acid, which leads to its leaching from the surface of the sorbent, and, as a consequence of instability of the separation process of the target elements.

The task of improving the selectivity of separation of U(VI), Th(IV), Np(IV) and Pu(IV) from nitric acid solutions is solved in that the proposed composition of the new extraction chromatographic material impregnated type, including as a complexing component mixture MEAN, a constant percentage of 33% and strippedand - a derivative of 1,5-bis[2-(acetoxymethyl)-4-(alkyl)]phenoxy-3-oxapentane (I), where: R represents alkyl, C1-C12with the percentage from 1% to 16%, and the rest is a polymer matrix - macroporous spherical granular copolymer of styrene with divinylbenzene with a granule size of 40-200 microns.

The following examples illustrate the invention:

Synthesis of 1,5-bis[2-(acetoxymethyl)-4-ethyl]phenoxy-3-oxapentane, the structure of which is described by the formula I when R=Et, we have described previously [RF Patent №2391349 for the invention of the Russian Federation 1,5-Bis[2-(acetoxymethyl)-4-ethyl]epoxy-3-oxapentane as a ligand for selective extraction of Thorium(IV) in a series of Uranium(VI) and Lanthanum(III) from nitric acid media / Tsivadze A. Y., Baulin C. E., Baulin D. C., Tananaev, I., Safiulin A. M. Appl. 03.12.2008 published. 10.06.2010 (B. I. No. 16)].

The method for producing the inventive extraction-chromatographic material

A solution of 3.3 g MEAN and 1.6 g of 1,5-bis[2-(acetoxymethyl)-4-ethyl] phenoxy-3-oxapentane and 45 ml of chloroform is rapidly added to a suspension containing 5.1 g of a copolymer of styrene with divinylbenzene with the size of the spherical granules 100-150 μm and 50 ml of chloroform. The resulting mixture was stirred on a magnetic stirrer for 1 h, then transferred to a round bottom flask and remove the solvent in vacuo on a rotary is m evaporator. The residue is transferred into a porcelain Cup and dried to constant weight at room temperature. The sorbent yield 10.0 g (100%).

Sorption characteristics of the proposed sorbents with respect to U(VI), Th(IV), Np(IV) and Pu(IV) was investigated by the method of frontal extraction chromatography in different experimental conditions (composition of the sorbent, at various concentrations of HNO3and in the presence of oxalic acid as a Stripping component). To determine the dynamic distribution coefficients (Kd) analyze elements of the front output curves (Fig.1 - typical front output curves) were processed according to the method described in [brown t, Garcini, Extraction chromatography. M: Peace.: - 1978. 615 S.]. Dynamic distribution coefficients Kdfor each of the retrieved items was calculated by the formula:

Kd=V0,5With a0me

where V0,5- weight of the solution,

passed through the sorbent to half overshoot, g;

meis the mass of sorbent in the column,

Front output curves of U(VI) depending on the composition of the extraction chromatographic material shown in Fig.2, where 1 - is orbent, containing 33% MEAN; 2 - 15% of compound I; 3 - 33% MEAN and 3.2% of compound I; 4 - 33% MTOAH and 4.8% of compound I; 5 - 33% MEAN and 8.0% of compound I; 6 - 33% MEAN and 16.0% of compound I. In all experiments, the mass of the sorbent was 15 mg; the amount of sorbent granules 40-70 μm; concentration of U(VI) 20 mg/l; the concentration of HNO30,4 M Similar frontal according to Th(IV) shown in Fig.3; where 1 - sorbent, containing 33% MEAN; 2 - 15% of compound I; 3 -33% MEAN and 3.2% of compound I; 4 -33% MEAN and 8% of compound I; 5 -33% MEAN and 16% of compound I; in all experiments, the mass of the sorbent was 15 mg; granules size 40-70 μm; concentration of Th(IV) and HNO3accordingly amounted to 2 mg/l and 0.4 M In Fig.4 shows a front output curves of Np(IV) for sorbents with different composition, where 1-63 mg sorbent, containing 33% MEAN; 2 - 70 mg of sorbent, containing 33% MEAN and 1.5% of compound I; 3 -70 mg sorbent, containing 33% MEAN and 11% of compound I; 4 -77 mg sorbent, containing 33% of compound I and 16% of compound I. the Size of sorbent granules was 150-315 μm; the diameter of the column 4.6 mm; speed eluent, 1 ml/min; the concentration of Np(IV) and HNO3was 6.8 mg/l and 0.5 M, respectively. Front output curves of U(VI), Zr(IV), Th(IV), Np(IV) and Pu(IV), obtained on the sorbent, containing 33% MEAN, 1% phosphorylated I, at a flow rate of eluent, 1 ml/min, the concentration of U(VI), Th(IV), Np(IV) and Pu(IV), equal to 5 mg/l and the concentration of HNO3equal to 0.8 is shown in Fig.5. The analysis of these dependencies allows us to conclude that in the case of sorption of U(VI), Th(IV), Np(IV) and Pu(IV), the use of a mixture MEAN and phosphorylated I as components of the stationary phase sorbents leads to a significant synergistic effect, the maximum expression which occurs in the sorbent, containing 33% MEAN and 16% of compound I, which corresponds to the molar ratio of these components is equal to 2:1. For example, the minimum value of the distribution coefficient for Th(IV) at a concentration of CHNO3M for the proposed sorbent is 2700, and for the prototype (sorbent brand TEVA Resin") is similar to the value of Kd=90 (Fig.6, where 1 - sorbent, containing 20% MEAN; 2-21,6% of compound I; 3-20% MEAN and 21.6% of compound I, when the concentration of Th(IV) 20 mg/l).

Thus, the sorption capacity of the inventive sorbent 30 times sorbent brand TEVA Resin".

It should be noted that the dependence of the dynamic values of the distribution coefficients for U(VI) and Th(IV) on the concentration of HNO3(Fig.7, where U(VI)-1 and Th(IV)-2) when using sorbent containing 20% MEAN and 21.6% of compound I, unlike sorbents on the basis of individual MEAN and phosphorylated I (Fig.6) essentially depends on the concentration of HNO3that allows you to selectively implement the sorption-desorption of these actinides selection of the concentration of HNO3.

It is established that eSerbia U(VI), Th(IV), Np(IV) and Pu(IV) from the surface of the sorbent can be efficiently carried out by adding eluent ammonium oxalate (Fig.8 the dependence of the distribution coefficients of U(VI), Zr(IV), Th(IV), Np(IV) and Pu(IV) concentration of ammonium oxalate in eluent). The dependences obtained in the following experimental conditions: mass of sorbent 40 mg of the sorbent Composition: 33% MEAN and 1% phosphorylated I. the flow Rate of eluent, 1 ml/min, the Concentration of U(VI), Th(IV), Np(IV) and Pu(IV) in all experiments was 5 mg/L. Concentration of HNO30.8 M Concentration of ammonium oxalate: 1-100 mg/l; 2-50 mg/l; 3-25 mg/l; 4-0 mg/L.

Thus, on the basis of the presented data we can conclude that differences in the dynamic values of the distribution coefficients of U(VI), Th(IV), Np(IV) and Pu(IV) allow selective separation of these elements in the inventive sorbent.

The composition of the extraction chromatographic material impregnated type for the selective extraction of U(VI), Th(IV), Np(IV) and Pu(IV) from nitric acid solutions containing three components with the following content (wt.%): methyltrioctylammonium nitrate (MEAN) - 33, phosphorylated is a derivative of 1,5-bis[2-(acetoxyphenyl)-4-(alkyl)]phenoxy-3-oxapentane General formula I, where R represents alkyl, C1-C12, - 1÷16, macroporous spherical granular copolymer of styrene with divinylbenzene with the size of g is anal 40-400 µm - the rest of it.



 

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