Method of extracting radionuclides and microelements

FIELD: chemistry.

SUBSTANCE: invention relates to the field of the sorption technology for the extraction of radionuclides and microelements in processing of various liquid and solid objects of radio-chemical enterprises. The claimed method includes a contact with a sorbent based on transitional metal cyanoferrate, with the contact being realised in a medium of a suspension, which contains humic acid in an amount of 0.15-0.25 g/l relative to the volume of the processed solution or 0.15-0.25 g/dm2 relative to the surface of the processed object, with the ratio Ssorb:L not less than 0.001 kg/l.

EFFECT: possibility to increase the degree of purifying polluted objects of the radio-chemical industry from radionuclides and microelements.

1 tbl

 

The invention relates to the field of sorption technology of extraction of radionuclides and trace elements in the processing of various liquid and solid objects radiochemical industries.

The known method of extraction of radionuclides from aqueous solutions in a dynamic mode using inorganic composite sorbent containing non-magnetic fraction product processing metallurgical slag having the following composition: calcium silicate Ca2SiO4; iron oxide-lithium Li0,28Fe21/34O32; coasit SiO2; glandular grossular Ca3Al1,332Fe0,668Si3O12; ringwoodite Fe2SiO4; a sodium aluminum silicate of Na14,88Al15,26Si32,74O96; wherein the process is carried out at an initial pH value of not less than 2 and the final pH value of not more than 14 (patent RU 2330340, IPC G21F 9/12, 2008).

The disadvantages of this method are not sufficiently high degree of purification from radionuclides waste water solutions radiochemical production, and not a wide range of sorbed elements.

The known method of purification from radionuclides of water environment technology at nuclear facilities by filtering water through granular load ferrosilicomanganese sorbent containing 0.2 to 2 wt.% hydrazine; 35-48 wt.% water and 20-35 wt.% ferrocyanides composition Me(I) 4-2x[NixFe(CN)6where Me(I)-Li+, Na+, K+NH4+or their mixture; the rest is zirconium hydroxide (patent RU 2399974, IPC G21F 9/12, 2010) (prototype).

The disadvantages of the known method include the possibility of its application only to clean the radionuclides of cesium, as well as insufficiently high degree of purification (1,9·104-5,8·105).

Thus, the authors task was to develop a method of extraction of radionuclides and trace elements from both liquid and solid objects radiochemical industries, providing a wide range of items retrieved, along with a high degree of extraction.

The task is solved in the method of extraction of radionuclides and trace elements, including contacting the sorbent on the basis of cyanoferrate transition metal, in which the contacting is carried out in the environment of a suspension containing humic acid in the amount of 0.15-0.25 g/l in relation to the volume of the treated solution or 0.15-0.25 g/DM2in relation to the surface of the object to be processed, at a ratio of TSorb:Not less than 0.001 kg/L.

At the present time of patent and technical literature is not a method of extraction of radionuclides and trace elements from contaminated solid and liquid objects radiochemical industries using Sorb�NTA in the medium of suspension, containing humic acid in the amount of 0.15-0.25 g/l, at a ratio of TSorb:Not less than 0.001 kg/L.

Conducted by the authors of the study has allowed to establish that the use of a suspension of powder cyanoferrate transition metal in a solution of humic acid leads to the simultaneous sorption extraction not only of cesium and strontium, but additionally a large number of ions other trace elements is often found in radioactive waste as a result of getting fission products and activation (Co, Mn, Fe, Zr, Nb, U, Th, Y, La, rare earth).

The proposed technical solution is discovered by the authors of the intensification of sorption specificity (affinity) of cyanoferrate transition metal cations to the s-, p-, d - and f-elements at the trace level under the action of humic acid. This is because in the presence of humic acid distribution coefficient Kd (mg/g) of these trace elements in relation to cyanoferrate transition metals increases by 1-3 order of magnitude due to the fact that trace elements are sorbed not in plain Aqua-ions, and in the form of complexes with humic acid. And herself humic acid is practically not retained on cyanoferrate transition metal. This is a feature of humic acids as a representative of natural organic INR�funkcionalnych connections: as a complexing agent for all ions of chemical elements in aqueous solutions, humic acid however is not suppressed (as the majority of known ligands), and enhances the sorption affinity complexes formed with cyanoferrate.

Experimentally, the authors found quantitative limits of the content of humic acids, providing an increase of the distribution coefficient. So, by reducing the content of humic acid is less than 0.15 g/l, the decrease of the distribution coefficient, due to the suppression of complexation of trace elements with humic acid and, as a consequence, the suppression of their sorption. With increasing humic acid content of more than 0.25 g/l and a decrease of the distribution coefficient due to the formation of strong complexes with micronutrients dimeric form of humic acid, which suppresses their sorption.

Fig.1 shows the dependence of the distribution coefficient (Kd) for sorption of trace elements Mg, Al, Si, Ca, Ti, V, Cr, Mn, Co, Ni, Sr, Zr, Cs, Ce, Nd, Th, and U from the sample of river water of Beloyarsk reservoir (Sverdlovsk region) powder of Prussian blue Fe4[Fe(CN)6]3with an average particle size of 200 μm depending on the concentration of humic acid in water (pH=7,6; 23°C; mass of sorbent - 0.20 g; volume of solution is 300 ml).

The proposed method can be implemented as follows. Prepare a suspension by adding in �Astor humic acid at a concentration of 0.15-0.25 g/l in relation to the volume of the treated solution or 0.15-0.25 g/DM 2in relation to the surface of the object to be processed cyanoferrate transition metal in an amount that provides a ratio of TSorb:Not less than 0.001 kg/L. Then brought into contact with the object being processed: pour the treated solution or brought into contact with the surface of the object. The proposed technical solution can be implemented in a confined space (static sorption in the reactor) or in a flow system (dynamics of sorption in the filtration column). In the first case, in the reactor with the purified solution was added a suspension of the proposed composition, after mixing, provide exposure to sediment deposition, the purified solution with residues of humic acid is drained for further processing or discharge to the soil or river system. The precipitate, concentrate the target radionuclides and trace elements sent for drying and conditioning for subsequent burial.

In the second case in the pipeline with a clearing solution serves a suspension containing humic acid and cyanoferrate transition metal. The solution, stir the slurry is fed to the input column with filter powder from the same cyanoferrate transition metal. As a result of passing through the filter the filtrate solution with residues of humic acid is drained for further processing or discharge to p�CWU or river system. The precipitate from the filter column sent for drying and conditioning for subsequent burial.

The proposed method can be used for desorption of radionuclides and trace elements from the surface of solid objects, for example, from the walls of the reactor. In this case, the surface brought into contact with a suspension containing humic acid and cyanoferrate transition metal. After surface treatment, the suspension was decanted and passed through a column with filter bottom. The filtrate residues of humic acid is drained for further processing, discharge to soil or river system. The precipitate, concentrate the target radionuclides and trace elements sent for drying and conditioning for subsequent burial.

The proposed method relates to green chemistry because humic acids are natural-compatible chemicals, capable of plugging into the natural biochemical reactions in soils and hydrological systems. That is why the filtrates with residues of humic acid can be moved directly into the environment, for example, be poured into the ground or river water.

The proposed method is illustrated by the following examples.

Example 1. Take a sample of river water volume of 300 ml To control the content of cesium ions injected into the water sample additionally p�the target cesium chloride in a quantity to the initial concentration of cesium was 0,83 g/L. Then prepare the slurry using a 45 ml solution of humic acid selected from an underground well # 36 - re Salekhard, Tyumen region, containing humic acid 0,99 g/l Dilution of this volume in the sample corresponds to the concentration of 0.15 g/l humic acid when adding solution to the sample of river water. To a solution of humic acid is added 0.20 g of cyanoferrate (II) iron (III), which corresponds to the ratio of TSorb:L=4,4:1 (kg/l). The suspension is added to the sample of river water and can stand up to the establishment of empirical equilibrium at 22°C. the Separated precipitate and the solution filtered through a filter of "blue ribbon". After separation of the precipitate from the solution determine the concentration of cesium and other elements in the sediment composition analysis of the separated solution by the method of mass spectroscopy with inductively coupled plasma instrument Elan 9000 (Perkin Elmer) in a quantitative mode. According to the measurement results calculate the distribution coefficient Kd (mg/g) characterizing the affinity of the sorbent for cesium ions and other elements by the formula (1):

,

where Coand C are the initial and equilibrium (after adsorption) concentrations of trace elements in solution; V - 300 ml, m - 0,200 g.

Example 2. Take a sample of river water volume of 300 ml To control the content of cesium ions injected into PR�BU water is additionally a solution of cesium chloride in a quantity to the initial concentration of cesium was 0,83 g/L. Then prepare a suspension using 75 ml of a solution of humic acid selected from an underground well # 36 - re Salekhard, Tyumen region, containing humic acid 0,99 g/l. Enter this amount humic acids in a river water sample, which corresponds to a concentration of 0.25 g/l humic acid when adding solution to the sample of river water. To a solution of humic acid is added 0.20 g of cyanoferrate (II) iron (III), which corresponds to the ratio of TSorb:W=2,7:1 (kg/l). The suspension is added to the sample of river water and can stand up to the establishment of empirical equilibrium at 22°C. the Separated precipitate and the solution filtered through a filter of "blue ribbon". After separation of the precipitate from the solution determine the concentration of cesium and other elements in the sludge by the method of mass spectroscopy with inductively coupled plasma instrument Elan 9000 (Perkin Elmer) in a quantitative mode. According to the measurement results calculate the distribution coefficient (Kd(mg/g) characterizing the affinity of the sorbent for cesium ions and other elements by the formula (1):

,

where Coand C are the initial and equilibrium (after adsorption) concentrations of trace elements in solution; V - 300 ml, m - 0,200 g.

The table shows the comparative distribution coefficients (Kdobtained when using� of the proposed method and the prototype method.

Table
Kd (the proposed method)Kd (method - prototype)Kd (the proposed method)
Kd(prototype) Rel. EDN.
Li80<1>80
Be4500<1>4500
Mg22003007
Al1100037030
Si2500<1>2500
Ca24005005
Sc1900<1>1900
Ti4000/td> <1>4000
V38000<1>38000
Cr11000<1>11000
Mn1900070003
Co410012034
Ni770010077
Sr4700<60>70
Y4500<1>4500
Zr5200<1>5200
Cs420000058000000,7
Ba29100<10>2900
Ce30000<10>3000
Nd30500<10>3000
Th31000<10>3100
U770015005

Thus, the proposed method allows to significantly increase the degree of purification from radionuclides and trace elements contaminated sites radiochemical industry.

Method of extraction of radionuclides and trace elements, including contacting the sorbent on the basis of cyanoferrate transition metal, characterized in that the contacting is carried out in the environment of a suspension containing humic acid in the amount of 0.15-0.25 g/l in relation to the volume of the treated solution or 0.15-0.25 g/DM2in relation to the surface of the object to be processed, at a ratio of TSorb:Not less than 0.001 kg/L.



 

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