Method for heterogenic catalytic decomposition of oxalate ions, complexing agents and surfactants in process mediums of radiochemical plants

FIELD: chemistry.

SUBSTANCE: what is provided is heterogenic catalytic decomposition of process media containing oxalate ions having the concentration of 16-18 g/l (complexing agents (up to 2 g/l), surfactant (up to 50 mg/l)) and nitric acid (up to 60 g/l) on a platinum catalyst applied on anion exchange resin VP-1AP (0.05-2 wt % of platinum). The effect is achieving a degree of decomposition of oxalate ions, complexing agents, surfactants up to 99.9%, in the residual concentrations - less than 10 mg/l in oxalate ions and less than 1 mg/l in complexing agent (EDTA, Trilon B) and surfactant (sulphonol).

EFFECT: improving the characteristics.

3 cl, 1 dwg

 

The invention relates to radiochemical technology and can be used in technology of processing of liquid radioactive waste (LRW) radiochemical production facilities and nuclear power plants.

An important task in ensuring radiation safety during operation of nuclear power plants and radiochemical productions is the solution to the problem of cleaning and processing of liquid radioactive waste generated during the conduct of various technological operations with solutions containing radionuclides, as well as decontamination of equipment and operating power plants.

One of the main components of technological solutions radiochemical plants are sequestering agent, which form stable soluble complexes with radionuclides134Cs,137Cs,60Co, etc. as these substances are used polyphosphates, aminopolycarboxylates acid, citric, hydrofluoric acid and their salts - citrate and fluoride. It is worth noting oxalate compounds, whose role has increased in recent time due to the increased production of nuclear fuel and reprocessing of spent nuclear fuel (SNF). Organic complexing agents of the type aminoalkanoic acids, usually called complexions and used in nuclear power plants (NPP) and radio�chemical industries, most important is ethylenediaminetetraacetic acid (EDTA) and its disodium salt (Trilon B).

It follows that processing of LRW is greatly simplified after the removal or destruction of the contained organic anions (oxalate, complexones) and surfactants that bind radionuclides and hamper their selection of traditional physico-chemical methods, and also affect the extraction and sorption behavior of uranium, neptunium, plutonium in the further processing.

From the current level of technology known oxidative [Lagunova J. A., Seliverstov A. F., B. G. Ershov,. Basiev, A. G. // Oxidative decomposition of oxalate ions in aqueous solutions of concentrated ozone. Atomic energy, 2012. Vol 111, No. 5. S. 31-35] and fotoatelier method of decomposition of the oxalate ion and complexing [Lagunova J. A., Seliverstov A. F., B. G. Ershov, P. A. Morozov, Komrakov A. S., Angelize sh.. // Fotoatelier the destruction of Trilon B in alkaline solutions. Materials of the 5th international scientific-technical conference: "radioactive waste management". M.: "VNIIAES", 2006, Pp. 39-40], among the disadvantages which, primarily, is to provide the duration of the decomposition process (100-150 min), increased consumption of the oxidant (ozone) to achieve the decomposition of 99% or more of the oxalate ion (chelating agent), narrow working range of pH (~10) when razlo�attachment, as well as the extreme nature of the influence of process temperature on the efficiency of decomposition of the oxalate ion, chelating agent.

The known method of oxidation and electrochemical degradation of surfactants by ozone, in particular sulphonole [Grinevich V. I., A. A. Gushchin, Plastinina N. And. Degradation of phenol and synthetic surfactants dissolved in water, in electrochemical effects in conjunction with ozonation // Izvestiya vuzov. Chemistry and chemical technology. 2009. - Vol. 52 - Vol.2. - P. 130-134]. Also known a method of decomposition of synthetic surfactant by plasma-catalytic degradation [Grinevich V. I., Plastinina N. And. Plasma-catalytic treatment of waste water from organic compounds // proceedings of V international Symposium on theoretical and applied plasma chemistry, Ivanovo, 2008. - T. 1. - P. 95-98]. The main disadvantages of these methods is the duration of the decomposition process, the complexity of hardware design process, as well as the significant influence of the initial concentration of surfactant and the nature of the catalysts on the efficiency of decomposition.

The closest to the claimed method is a method of decomposition of complexing in nitrate solutions when heated to 50-90°C. the Process is conducted in the presence of a catalyst - activated carbon or platinum supported on silica gel (0,86 wt.% platinum) in termostatica�Noah chromatographic column with a volume of 9 ml. Shows the decomposition of the chelating agent to 99.9% at contact time of 20 min. [Patent SU 1214607A, C02F 1/72, 28.02.86] (prototype). The disadvantage of this method is the prolonged contact time of the solution with catalyst - to 20 minutes. The contact time of the proposed method is 50-55 seconds. An advantage of the claimed invention in hardware design is to rapidly change the volume of the catalyst, the height of its layer in the column, i.e. in simpler installation service unlike chromatographic column prototype. Moreover, as a carrier of platinum in the present invention (method) is used anion-exchange resin EP-AP, unlike silica gel (prototype), which significantly increases the resistance of the catalyst, both in alkaline and in acidic media. Differences in favour of the invention also exist in the amount of deposited platinum on the carrier - the minimum amount is 0.05 wt.%. platinum in the developed method against 0,86 wt.% in the prior art. Also, unlike the prototype, according to the developed method is possible heterogeneous catalytic decomposition of complexing at lower temperatures (37-52°C) when introduced into the hydrogen peroxide solution.

The problem to be solved by the claimed invention is the decomposition of organic anions such as oxalate ions, chelating agents, surface treatments�-active substances, in the technological solutions and liquid radioactive waste of radiochemical production facilities and nuclear power plants to waste the concentrations at which these substances do not complicate further processing containing solutions or waste.

The problem is solved by the developed method of heterogeneous catalytic decomposition of the oxalate ions, complexing and surfactants in technological solutions radiochemical production on the platinum catalyst deposited on an anion exchange resin EP-AP (0.05 to 2 wt.% platinum).

The technical result of the invention is to achieve the degree of decomposition of more than 99% and residual concentrations of less than 10 mg/l of the oxalate ion and less than 1 mg/l of the chelating agent (EDTA, Trilon B) and a surfactant (sulphonole).

The feasibility of the proposed method is confirmed by researches at the laboratory apparatus shown in Fig.1, which comprises: a catalytic column with shirt (1), thermostat (2), peristaltic pump (3), the capacity with the initial solution (4), a receiving vessel (5), measuring cylinder (6); In-01, In-02, In-03 - the needle valves to regulate the flow rate.

The proposed method is implemented in the following sequence: a catalyst was prepared by impregnating resin VP-AP alkaline solution of platinum, put cooked catalysate� in the column, connect thermostat. With peristaltic pump serves the original solution of the catalyst column, carry out the decomposition process. The solution after catalytic columns are collecting portions and analyze the content of H2C2O4(of chelating agent, surfactant) and HNO3(pH). The total acidity of the solution and the concentration of HNO3determined by potentiometric titration using an automatic titrator.

Example 1.

Preparing a platinum catalyst source and the solution of the following composition: oxalate-ion - 16-18 g/l, nitric acid is 60 g/L.

The contact time of the feed solution with catalyst - 55-75 C. the process Temperature is 70-80°C. the Flow rate of the feed solution - 7 colon.about./h. the Experiment was conducted in the above sequence.

Residual concentration of the oxalate ion was less than 10 mg/l, the degree of decomposition of 99.88-99,90%.

Example 2.

The process of heterogeneous catalytic decomposition of the chelating agent of Trilon B was carried out similarly to example 1. The composition of the initial solution: Trilon B - 1,1-1,5 g/l, nitric acid - 12-25 g/L.

The process temperature is 75-80°C. the contact Time of the feed solution with catalyst - 55-75 C. the Flow rate of the feed solution - 7 colon.about./p.m.

Residual concentration of the chelating agent of Trilon B was less than 1 mg/l, the degree of decomposition of 99.91 per cent.

Example 3.

The process was carried out� analogously to example 2, however, the introduction of hydrogen peroxide (9 g/l) improves the efficiency of decomposition of the chelating agent (Trilon B) at a lower temperature and to reduce the content of nitric acid in the initial solution. The composition of the initial solution: Trilon B - 1,1-1,5 g/l, nitric acid and 0.2-0.3 g/l, hydrogen peroxide - 9 g/L.

The process temperature is 65-70°C. the contact Time of the feed solution with catalyst - 55-75 C. the Flow rate of the feed solution - 7 colon.about./p.m.

Residual concentration of the chelating agent of Trilon B was less than 1 mg/l, the degree of decomposition of 99.91 per cent.

Example 4.

The process was carried out analogously to example 2, however, instead of complexone spent the decomposition of surfactants sulphonole. The composition of the initial solution: sulphonole up to 50 mg/l, nitric acid and 0.2 g/l, hydrogen peroxide - 9 g/L.

The process temperature is 65-70°C. the contact Time of the feed solution with catalyst - 55-75 C. the Flow rate of the feed solution - 7 colon.about./p.m.

Residual concentration sulphonole (surfactant) was less than 1 mg/l, the degree of decomposition of 99.9%.

Example 5.

The process was carried out analogously to example 3, however, conducted a joint decomposition of the chelating agent of Trilon B and surfactant sulphonole. The composition of the initial solution: Trilon B - 1,1-1,5 g/l, sulphonole up to 50 mg/l, nitric acid and 0.2 g/l, hydrogen peroxide - 9 g/L.

The temperature of the process� - 65-70°C. the contact Time of the feed solution with catalyst - 55-75 C. the Flow rate of the feed solution - 7 colon.about./p.m.

Residual concentration of Trilon B (complex) and sulphonole (surfactant) was less than 1 mg/l, the degree of decomposition of 99.9%.

Example 6.

The experiment was carried out according to example 1. The composition of the initial solution: carbonate-ion - 2 g/l, nitric acid is 60 g/L.

The process temperature is 70-80°C. the contact Time of the feed solution with catalyst - 55-75 C. the Flow rate of the feed solution - 7 colon.about./p.m.

The residual concentration of carbonate ion was less than 1 mg/l, the degree of decomposition of 99.9%.

The technical result of the invention, namely the achievement of the degree of decomposition of less than 10 mg/l of the oxalate ion and less than 1 mg/l of the chelating agent (EDTA, Trilon B) and surfactant (sulphonole), gives an indication of the potential implementation of the present invention (method) in the technology of processing of liquid radioactive waste, in particular decontaminating solutions (containing oxalate ions, chelating agents, surfactants) radiochemical production facilities and nuclear power plants. Moreover, the heterogeneous catalytic decomposition of the oxalate ion can be embedded in the design of catalytic decomposition of oxalate ions the mother liquors after the precipitation of plutonium oxalate in the technology of purification of plutonium dioxide.

1. Method of heterogeneous catalytic decomposition of the oxalate ions.�sonow and surfactants in technological solutions radiochemical productions characterized in that the catalyst is platinum deposited on an anion exchange resin EP-UP with weight platinum content of 0.05-2%.

2. A method according to claim 1, characterized in that the technological solution was added hydrogen peroxide to increase the efficiency of heterogeneous catalytic decomposition and reduction of the process temperature.

3. A method according to claim 1, characterized in that the leach solution contains a carbonate ion to 2 g/L.



 

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