CN112908508A - Method for treating radioactive analysis waste liquid by one-step method - Google Patents
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- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
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Abstract
The invention discloses a method for treating radioactive analysis waste liquid by a one-step method, solves the problems that an effective treatment method aiming at the radioactive analysis waste liquid is not available in the prior art, and the conventional Fenton-ferrite method can increase the secondary waste amount and increase the difficulty of radioactive operation and is difficult to implement, and belongs to the technical field of nuclear industry waste liquid treatment. The method of the invention comprises the following steps: adjusting the pH value of the radioactive analysis waste liquid to be treated to acidity, and sequentially adding Fe2+、H2O2Stirring and mixing to start Fenton reaction; adjusting the pH value of the system after the reaction is finished to be alkaline, and starting ferrite coprecipitation; and (5) carrying out liquid-solid separation to finish treatment. The invention does not need two steps of processes, avoids the steps of adding reagents for many times, separating liquid from solid and the like, simplifies the treatment process, improves the treatment efficiency and has important significance for improving the efficiency and the effect of treating the radioactive analysis waste liquid.
Description
Technical Field
The invention belongs to the technical field of nuclear industry waste liquid treatment, relates to radioactive waste liquid generated in a sample analysis process, and particularly relates to a method for treating radioactive analysis waste liquid by a one-step method.
Background
In the sample analysis process in the nuclear industry field, a large amount of organic media such as an extractant, a complexing agent and the like are used to generate radiationThe composition of sexual waste liquid is more and more complex. The radioactive nuclide in the radioactive analysis waste liquid mainly comprises actinide nuclide, the radioactive species mainly comprises alpha radioactivity, and the total alpha specific activity of the radioactive nuclide is widely distributed and can be distributed from low level to medium level. Organic substances such as extractants, complexing agents and the like and actinides form relatively stable complexes, and are difficult to form by the traditional flocculation sedimentation method (Fe (OH) is generated under alkaline conditions)3Colloid carrying nuclide) is completely removed; while Fe (OH)3The density of the settled slurry is low, the water content of the slurry separated by gravity settling can reach more than 80%, the settling speed is low, the treatment efficiency is low, more chemical slurry type secondary wastes are easily generated, and the principle of waste minimization is not met.
At present, no report is published about an effective treatment method of the radioactive analysis waste liquid. For the treatment of other heavy metal ions in coordination state, there are reports related to the treatment by a Fenton (Fenton) -ferrite method two-step process, and the first step process comprises: carrying out decomplexing by utilizing the oxidation of Fenton reaction; the second step of the process: and then removing heavy metal ions by adopting a ferrite coprecipitation method.
Wherein the Fenton oxidation mechanism is that a Fenton reagent (FeSO) is added under an acidic condition4、H2O2)，H2O2In Fe2+OH with strong oxidation capacity is generated under the catalysis, the OH can play a role of breaking the complex, and Fe2+Is oxidized into Fe3+After the oxidation process is finished, the reaction system is adjusted to be alkaline to terminate the reaction to generate Fe3+And (5) flocculent precipitation, carrying out liquid-solid separation, and ending the Fenton process.
Adding Fe into the supernatant after Fenton reaction according to a certain proportion2+Reagent and Fe3+Reagent for producing ferrite (Fe) under alkaline conditions3O4) And (4) precipitating, carrying nuclide while the ferrite is settled, and performing liquid-solid separation to finish the treatment process.
If the method is used for treating the radioactive analysis waste liquid for reference, the two-step process of taking supernatant after Fenton oxidation and liquid-solid separation and then adding a reagent for ferrite coprecipitation can generate iron mud precipitation twice in sequence, so that the secondary waste amount is increased, and the principle of waste minimization in radioactive waste treatment is not met. Meanwhile, the two-step process needs operations such as reagent addition for multiple times, liquid-solid separation for two times and the like, increases the difficulty of radioactive operation, and is not beneficial to implementation of the treatment process.
Therefore, it is an urgent need to provide a method for treating a radioactive analysis waste solution, which can treat a complex actinide nuclide, is simple to operate and easy to implement, and does not increase the amount of secondary waste.
Disclosure of Invention
The technical problem solved by the invention is as follows: provides a method for treating radioactive analysis waste liquid by a one-step method, and solves the problems that no effective treatment method aiming at the radioactive analysis waste liquid exists in the prior art, and the conventional Fenton-ferrite method can increase the secondary waste amount and increase the difficulty of radioactive operation and is not easy to implement.
The technical scheme adopted by the invention is as follows:
the method for treating the radioactive analysis waste liquid by the one-step method comprises the following steps:
s1.Fenton reaction: adjusting the pH value of the radioactive analysis waste liquid to be treated to acidity, and sequentially adding Fe2+、H2O2Stirring and mixing to start Fenton reaction;
s2, ferrite coprecipitation: adjusting the pH value of the system after the S1 reaction is finished to be alkaline, and starting ferrite coprecipitation;
s3, liquid-solid separation: and (3) carrying out liquid-solid separation on the system which is subjected to the step 2 to finish the treatment.
In some embodiments of the present invention, in the step S1, the radioactive analysis waste liquid to be treated is mixed with Fe2+The mass ratio is 5000-6000: 1, preferably 5200: 1.
In some embodiments of the present invention, in S1, Fe2+Derived from FeSO4Preferably, FeSO is added4And H2O2Is 3: 1.
The invention generates ferrite by one-step method, and carries nuclide while the ferrite is settledAnd then the liquid-solid separation is carried out to complete the treatment process. Fe3O4The chemical formula of ferrite can also be written as FeO2O3I.e. 1 of the 3 Fe atoms is +2 valent and the remaining 2 are +3 valent. And H2O2The O atom in (A) is a valence of-1 and becomes a valence of-2 after being reduced by divalent iron. To produce Fe3O4Ferrite, FeSO4 and H2O2The theoretical molar ratio of (1) should be 3:1, so as to ensure Fe after Fenton reaction2+With Fe3+In a ratio of 2: 1.
In some embodiments of the present invention, in S1, the pH of the radioactive analysis waste liquid to be treated is adjusted to 2 to 4.
In some embodiments of the invention, the pH of the radioactive assay waste to be treated is adjusted with an inorganic acid; the inorganic acid is preferably HCl or H2SO4、HNO3Any one or more of them.
In some embodiments of the invention, in the S1, the Fenton reaction time is 0.5 to 4 hours; preferably 0.5-2 h.
In some embodiments of the invention, in the step S2, the pH of the system after the completion of the S1 reaction is adjusted to 10 to 11.
In some embodiments of the present invention, in S2, the pH is adjusted by using an inorganic base, and the inorganic base is preferably one of NaOH and KOH.
In some embodiments of the invention, in the S2, the ferrite co-precipitation time is 2-8 h.
In some embodiments of the invention, the radioactive assay waste comprises a radioactive waste contaminated with actinides.
Compared with the prior art, the invention has the following beneficial effects:
the invention has scientific design and simple operation. The invention creatively controls the FeSO in the Fenton reagent4And H2O2The proportion, the reaction step, the reaction time and other parameters of the Fe in the system after the Fenton reaction2+With Fe3+In a desired molar ratio (2: 1) so as to enable direct basification to Fe3O4FerriteFurther completing the complex breaking and nuclide removal. The invention does not need two steps of processes, avoids the steps of adding reagents for many times, separating liquid from solid and the like, simplifies the treatment process, improves the treatment efficiency and has important significance for improving the efficiency and the effect of treating the radioactive analysis waste liquid.
The final product generated by the invention is Fe3O4Ferrite precipitates, has good magnetism, and provides convenience for liquid-solid separation after waste liquid treatment; meanwhile, the density is high, and the sedimentation speed is much higher than that of Fe (OH)3The colloid sedimentation speed improves the treatment efficiency; fe3O4The ferrite precipitate has small total volume, reduces the yield of final secondary waste and simplifies the difficulty of further treatment of subsequent precipitates.
The invention has reference significance for treating the non-radioactive heavy metal ion wastewater, and can simplify the process flow of treating the non-radioactive heavy metal ion wastewater.
Drawings
FIG. 1 is a diagram showing the state in which ferrite precipitates obtained in example 1 are attracted to a magnet.
FIG. 2 shows Fe (OH) obtained in comparative example 13Colloidal sediment.
FIG. 3 is a comparison between the radioactive waste liquid of example 2 before and after treatment, wherein the left is a waste liquid sample after treatment and the right is a waste liquid sample before treatment.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Example 1
The embodiment discloses a method for treating radioactive analysis waste liquid, which specifically comprises the following steps:
a certain total alpha specific activity of 100Bq/L level, resulting from contamination of radioactive waste liquid with actinides in the sample analysis process, with H2SO4Adjusting the pH value to 3; according to radioactive waste liquid and Fe2+Adding FeSO with the mass ratio of 5200:14·7H2O, according to Fe2+And H2O2H is added in a molar ratio of 3:12O2Stirring and mixing, reacting for 0.5h, adding NaOH to adjust the pH value of the system to 10.5, precipitating to complete liquid-solid separation, and measuring the total alpha specific activity of the supernatant to be 0.17Bq/L, which meets the discharge requirement of the total alpha specific activity in Integrated wastewater discharge Standard (GB 8978-1996). The state diagram of the ferrite precipitate obtained in this example being attracted by a magnet is shown in FIG. 1.
Comparative example 1
The comparative example adopts the traditional flocculation sedimentation method to treat the radioactive analysis waste liquid, and specifically comprises the following steps:
the actinoid in example 1 was used to contaminate the radioactive waste liquid with the radioactive waste liquid, Fe2+Mass ratio, KMnO4Mixing according to the mass ratio of 5200:1:1, reacting for 0.5h, adding NaOH to adjust the pH of the system to 10.5, settling to complete liquid-solid separation, wherein the sediment is loose Fe (OH)3And (3) colloid. Repeating the process for more than 3 times, and determining that the total alpha specific activity of the supernatant is still 100Bq/L order of magnitude. Fe (OH) obtained in this comparative example3The colloidal sediment is shown in figure 2.
Compared with the traditional flocculation sedimentation method adopted in the comparative example 1, the example 1 has the advantages that the Fenton oxidation is introduced to play a role in breaking the complex, so that the removal capability of actinides in the waste liquid is greatly improved, and meanwhile, the actinides are precipitated into magnetic Fe3O4Ferrite, which is easier to realize liquid-solid separation. The volume of the sediment is only about 1/3 of the traditional flocculation method of the embodiment 1, the settling time is about 1/3 of the embodiment 1, and the secondary waste amount is greatly reduced and the treatment efficiency is improved.
Example 2
The embodiment discloses a method for treating radioactive analysis waste liquid, which specifically comprises the following steps:
a certain total alpha specific activity of 105Of Bq/L order, resulting from actinides during sample analysisContamination of radioactive waste liquid with nuclides, with H2SO4Adjusting the pH value to 3 according to the ratio of radioactive waste liquid to Fe2+Adding FeSO with the mass ratio of 5200:14·7H2O, according to Fe2+And H2O2H is added in a molar ratio of 3:12O2Stirring and mixing, reacting for 0.5h, adding NaOH to adjust the pH of the system to 10.5, precipitating to complete liquid-solid separation, and measuring the total alpha specific activity of the supernatant to be 103Bq/L order, and processing efficiency>99％。
The comparative figures before and after the radioactive waste liquid treatment in this example are shown in FIG. 3, in which the left part is the waste liquid sample after the treatment and the right part is the waste liquid sample before the treatment.
Comparative example 2
The comparative example adopts the traditional flocculation sedimentation method to treat the radioactive analysis waste liquid, and specifically comprises the following steps:
the actinoid in example 2 was used to contaminate the radioactive waste liquid with the radioactive waste liquid, Fe2+Mass ratio, KMnO4Mixing according to the mass ratio of 5200:1:1, reacting for 0.5h, adding NaOH to adjust the pH of the system to 10.5, and precipitating to complete liquid-solid separation. Repeating the process for more than 3 times, and determining that the total alpha specific activity of the supernatant is still 105Bq/L order of magnitude.
Compared with the traditional flocculation sedimentation method adopted in the comparative example 2, the example 2 has the advantages that the Fenton oxidation is introduced to play a role in breaking the complex, so that the removal capability of actinides in the waste liquid is greatly improved, and meanwhile, the actinides are precipitated into magnetic Fe3O4Ferrite, which is easier to realize liquid-solid separation.
Example 3
The embodiment discloses a method for treating radioactive analysis waste liquid, which specifically comprises the following steps:
a certain total alpha specific activity of 107Bq/L level, resulting from contamination of radioactive waste liquid with actinides in the sample analysis process, with H2SO4Adjusting the pH to 3 according to the ratio of radioactive waste liquid to Fe2+Adding FeSO with the mass ratio of 5200:14·7H2O, according to Fe2+And H2O2H is added in a molar ratio of 3:12O2After reacting for 0.5h, NaOH is added to adjust the pH value of the system to 10.5, and the reaction is finishedSeparating liquid and solid, and measuring the total alpha specific activity of the supernatant to be 104Of the Bq/L order, i.e. the efficiency of the treatment>99.9％。
Examples 4 to 8
Examples 4 to 8 disclose methods for treating a radioactive assay waste liquid according to the present invention, which are different from example 3 in the amount of fenton reagent used or the reaction parameters, and the remaining conditions are the same.
Example 4
In this example, compared to example 3, the radioactive waste liquid was mixed with Fe2+The mass ratio was 5000:1, and the other conditions were the same, and the results showed that the total alpha ratio of the supernatant treated in this example was 104Bq/L order, processing efficiency>99.9％。
Example 5
In this example, compared to example 3, the radioactive waste liquid was mixed with Fe2+The mass ratio was 6000:1, and the other conditions were the same, and the results showed that the total alpha ratio of the supernatant treated in this example was 104Bq/L order, processing efficiency>99.9％。
Example 6
This example compares with example 3 with H2SO4The pH of the radioactive waste liquid was adjusted to 2, and the rest conditions were the same, and the results showed that the total α specific activity of the supernatant treated in this example was 104Bq/L order, processing efficiency>99.9％。
Example 7
This example compares with example 3 with H2SO4The pH of the radioactive waste liquid was adjusted to 4, and the rest conditions were the same, and the results showed that the total α specific activity of the supernatant treated in this example was 104Bq/L order, processing efficiency>99.9％。
Example 8
In this example, compared with example 3, after 4 hours of fenton reaction, NaOH was added to adjust the pH of the system to 10.5, and the other conditions are the same, and the result shows that the total α specific activity of the supernatant treated in this example is 104Bq/L order, processing efficiency>99.9％。
Finally, it should be noted that: the above embodiments are only preferred embodiments of the present invention to illustrate the technical solutions of the present invention, but not to limit the technical solutions, and certainly not to limit the patent scope of the present invention; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; that is, the technical problems to be solved by the present invention, which are not substantially changed or supplemented by the spirit and the concept of the main body of the present invention, are still consistent with the present invention and shall be included in the scope of the present invention; in addition, the technical scheme of the invention is directly or indirectly applied to other related technical fields, and the technical scheme is included in the patent protection scope of the invention.
Claims (10)
1. A method for treating a radioactive assay waste stream in a one-step process, comprising the steps of:
s1.Fenton reaction: adjusting the pH value of the radioactive analysis waste liquid to be treated to acidity, and sequentially adding Fe2+、H2O2Stirring and mixing to start Fenton reaction;
s2, ferrite coprecipitation: adjusting the pH value of the system after the S1 reaction is finished to be alkaline, and starting ferrite coprecipitation;
s3, liquid-solid separation: and (3) carrying out liquid-solid separation on the system which is subjected to the step 2 to finish the treatment.
2. The method according to claim 1, wherein in S1, the radioactive analysis waste liquid to be treated is mixed with Fe2+The mass ratio is 5000-6000: 1, preferably 5200: 1.
3. The method according to claim 1, wherein in S1, Fe2+Derived from FeSO4Preferably, FeSO is added4And H2O2Is 3: 1.
4. The method according to claim 1, wherein in S1, the pH of the radioactive analysis waste liquid to be treated is adjusted to 2 to 4.
5. The method according to claim 4, wherein the pH of the radioactive assay waste liquid to be treated is adjusted with an inorganic acid; the inorganic acid is preferably HCl or H2SO4、HNO3Any one or more of them.
6. The method according to claim 1, wherein in S1, the Fenton reaction time is 0.5-4 h; preferably 0.5-2 h.
7. The method according to claim 1, wherein in S2, the pH of the system after completion of the S1 reaction is adjusted to 10 to 11.
8. The method according to claim 7, wherein in S2, the pH value is adjusted by using an inorganic base, preferably one of NaOH and KOH.
9. The method according to claim 1, wherein in S2, the ferrite co-precipitates for 2-8 h.
10. The method of claim 1, wherein the radioactive assay waste comprises actinide-contaminated radioactive waste.
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