CN110727022A - Application of 4A molecular sieve in rapid enrichment of artificial radionuclide zirconium in ocean - Google Patents

Application of 4A molecular sieve in rapid enrichment of artificial radionuclide zirconium in ocean Download PDF

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CN110727022A
CN110727022A CN201910968550.5A CN201910968550A CN110727022A CN 110727022 A CN110727022 A CN 110727022A CN 201910968550 A CN201910968550 A CN 201910968550A CN 110727022 A CN110727022 A CN 110727022A
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zirconium
molecular sieve
enrichment
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seawater
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黄勇
王婷
李金培
吴敏
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Technical Institute of Physics and Chemistry of CAS
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    • G—PHYSICS
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    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T7/00—Details of radiation-measuring instruments
    • G01T7/02—Collecting means for receiving or storing samples to be investigated and possibly directly transporting the samples to the measuring arrangement; particularly for investigating radioactive fluids
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
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Abstract

The invention discloses an application of a 4A molecular sieve in rapidly enriching artificial radionuclide zirconium in ocean, which is to mix the 4A molecular sieve with seawater containing the artificial radionuclide zirconium, and the artificial radionuclide zirconium in the seawater is rapidly enriched by the molecular sieve. The 4A molecular sieve can quickly and efficiently selectively enrich the artificial radionuclide zirconium in seawater, and can quickly enrich trace zirconium nuclide in the polluted sea through the 4A molecular sieve in the case of sudden nuclear accidents or nuclear pollution, so that the pollution condition of the zirconium nuclide in the sea can be quickly monitored.

Description

Application of 4A molecular sieve in rapid enrichment of artificial radionuclide zirconium in ocean
Technical Field
The invention belongs to the field of radionuclide enrichment, and particularly relates to application of a 4A molecular sieve in rapid enrichment of artificial radionuclide zirconium in ocean.
Background
At this stage, nuclear energy industry is rapidly developed, and potential nuclear accidents increasingly increase the nuclear pollution pressure in offshore areas. The water body in the ocean is huge, the diffusion of the artificial radioactive nuclide is fast, and the concentration of the artificial radioactive nuclide is relatively low, so that the enrichment of the artificial radioactive nuclide in the ocean becomes a difficult problem. There are two major difficulties in monitoring artificial radionuclide contamination in the ocean during sudden nuclear accidents: firstly, nuclides are difficult to enrich in seawater; secondly, the enrichment time is too long, which requires about three to four days, and the requirement of rapid monitoring is difficult to meet when the nuclear leakage accident really occurs.
In the prior art, the concentration of potassium nuclide in seawater can be directly analyzed, radium nuclide can be quickly enriched, and due to the influence of high salt concentration of seawater, the quick enrichment and monitoring of other nuclides are still difficult, particularly for artificial radionuclide zirconium, research is few, and which material can quickly enrich the artificial radionuclide zirconium in the sea is not reported.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the application of the 4A molecular sieve in the rapid enrichment of the artificial radionuclide zirconium in the ocean.
The inventor creatively discovers that the 4A molecular sieve can selectively and quickly realize the quick enrichment of the artificial radionuclide zirconium nuclide in the seawater, reduces the time cost, can be further applied to the conventional monitoring of the zirconium nuclide pollution in the offshore area or the emergency monitoring of nuclear accidents, and quickly enriches the artificial radionuclide zirconium in the seawater under the condition of sudden nuclear pollution so as to monitor the pollution degree of the artificial radionuclide zirconium in the seawater.
Specifically, the present invention provides the following technical solutions.
The application of the 4A molecular sieve in rapidly enriching the artificial radionuclide zirconium in the ocean is to mix the 4A molecular sieve with seawater containing artificial radionuclides, and the artificial radionuclide zirconium in the seawater is enriched by the molecular sieve.
Preferably, in the above application, the concentration of the artificial radionuclide zirconium in the seawater is less than 100 ppm.
Preferably, in the application, the 4A molecular sieve is mixed with seawater according to the mass-to-volume ratio of 1-10g: 1L.
Preferably, in the above application, the enrichment time is 1-30 min.
Preferably, in the above application, the pH of the seawater is 7.5 to 8.5.
Preferably, in the above application, the 4A molecular sieve is mixed with seawater for enrichment at room temperature.
Preferably, in the above application, the 4A molecular sieve is in a powder form.
The invention has the following beneficial effects:
the molecular sieve can be used for quickly and efficiently selectively enriching the artificial radionuclide zirconium in seawater, and can be used for quickly enriching trace zirconium nuclides in polluted sea in the case of sudden nuclear accidents or nuclear pollution, so that the pollution condition of the zirconium nuclides in the sea can be quickly monitored. The molecular sieve can be artificially synthesized or naturally formed, and is cheap and easy to obtain.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited thereto.
In the following examples, information on each reagent and apparatus used is shown in Table 1.
TABLE 1 reagent and Instrument information Table used in the examples
Figure BDA0002231312290000031
Preparation of simulated seawater: 25.6g of sodium chloride and 198mg of sodium bicarbonate are dissolved in 1L of deionized water and stirred until the sodium chloride and the sodium bicarbonate are completely dissolved, and the pH value of the prepared simulated seawater is 8.1.
Example 1
Weighing 118mg Zr (NO)3)4·5H2Dissolving O in simulated seawater, and metering to 250mL, wherein the concentration of zirconium ions in the prepared solution is 100 ppm. 10mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 20 ppm. Adding 0.22g of 4A molecular sieve (powder), magnetically stirring for 30min, filtering the reacted solution with a 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (2) is reduced from 19.47ppm before enrichment to 1.54ppm after enrichment, and the enrichment efficiency is 92.07 percent.
The enrichment efficiency calculation method comprises the following steps: enrichment efficiency ═ (concentration before enrichment-concentration after enrichment)/concentration before enrichment × 100%.
Example 2
Weighing 118mg Zr (NO)3)4·5H2Dissolving O in simulated seawater, and metering to 250mL, wherein the concentration of zirconium ions in the prepared solution is 100 ppm. 10mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 20 ppm. Adding 0.05g of 4A molecular sieve (powder), magnetically stirring for 30min, filtering the reacted solution with a 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (A) is reduced from 19.47ppm before enrichment to 1.66ppm after enrichment, and the enrichment efficiency is 91.48%.
Example 3
Weighing 118mg Zr (NO)3)4·5H2Dissolving O in simulated seawater, and metering to 250mL, wherein the concentration of zirconium ions in the prepared solution is 100 ppm. 10mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 20 ppm. Adding 0.1g of 4A molecular sieve (powder), magnetically stirring for 30min, filtering the reacted solution with a 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (2) is reduced from 19.47ppm before enrichment to 1.56ppm after enrichment, and the enrichment efficiency is 91.98%.
Example 4
Weighing 118mg Zr (NO)3)4·5H2Dissolving O in simulated seawater, and metering to 250mL, wherein the concentration of zirconium ions in the prepared solution is 100 ppm. 4mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 8 ppm. Adding 0.05g of 4A molecular sieve (powder), magnetically stirring for 6min, filtering the reacted solution with a 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (2) is reduced from 8.05ppm before enrichment to 1.07ppm after enrichment, and the enrichment efficiency is 87%.
Example 5
Weighing 118mg Zr (NO)3)4·5H2O is dissolved inAnd (3) in simulated seawater, the volume is fixed to 250mL, and the concentration of zirconium ions in the prepared solution is 100 ppm. 4mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 8 ppm. Adding 0.05g of 4A molecular sieve (powder), magnetically stirring for 30min, filtering the reacted solution with a 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (2) is reduced from 8.68ppm before enrichment to 0.73ppm after enrichment, and the enrichment efficiency is 91.6%.
Example 6
Weighing 118mg Zr (NO)3)4·5H2Dissolving O in simulated seawater, and metering to 250mL, wherein the concentration of zirconium ions in the prepared solution is 100 ppm. 5mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 10 ppm. Adding 0.5g of 4A molecular sieve (spherical), magnetically stirring for 30min, filtering the reacted solution with 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (A) is reduced from 10.88ppm before enrichment to 7.32ppm after enrichment, and the enrichment efficiency is 32.7%.
Comparative example 1
Weighing 118mg Zr (NO)3)4·5H2Dissolving O in simulated seawater, and metering to 250mL, wherein the concentration of zirconium ions in the prepared solution is 100 ppm. 10mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 20 ppm. Adding 0.25g of 3A molecular sieve (powder), magnetically stirring for 30min, filtering the reacted solution with a 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (A) is reduced from 19.47ppm before enrichment to 7.76ppm after enrichment, and the enrichment efficiency is 60.14%.
Deionized water is used as a solvent to prepare 50mL of Zr-containing solution4+Adding 0.25g of 3A molecular sieve (powder), magnetically stirring for 30min, filtering the sample with a 0.22um filter membrane after the reaction is finished, and generating plasma by inductive couplingThe concentration of the solution before and after enrichment was measured by a spectrometer. Zr4+The concentration of (A) is reduced from 18.52ppm before enrichment to 0.02ppm after enrichment, and the enrichment efficiency is 99.9%.
Comparing the measurement results of the 3A molecular sieve (powder) in simulated seawater and deionized water shows that the enrichment efficiency of the 3A molecular sieve (powder) on the radionuclide zirconium is obviously reduced under the influence of high salt concentration of seawater.
Comparative example 2
Weighing 118mg Zr (NO)3)4·5H2Dissolving O in simulated seawater, and metering to 250mL, wherein the concentration of zirconium ions in the prepared solution is 100 ppm. 10mL of a solution having a zirconium ion concentration of 100ppm was diluted to 50mL, and the zirconium ion concentration after dilution was approximately 20 ppm. Adding 0.29g of 13X molecular sieve (powder), magnetically stirring for 30min, filtering the reacted solution with a 0.22um filter membrane, and performing inductively coupled plasma emission spectrometer on Zr in the solution before and after enrichment4+Is measured. Zr4+The concentration of (2) is reduced from 19.47ppm before enrichment to 13.818ppm after enrichment, and the enrichment efficiency is 29.03%.
Deionized water is used as a solvent to prepare 50mL of Zr-containing solution4+Adding 0.29g of 13X molecular sieve (powder), magnetically stirring for 30min, filtering a sample by using a 0.22um filter membrane after the reaction is finished, and measuring the concentration of the solution before and after enrichment by using an inductively coupled plasma emission spectrometer. Zr4+The concentration of (A) is reduced from 18.52ppm before enrichment to 4.03ppm after enrichment, and the enrichment efficiency is 78.3%.
Comparing the measurement results of the 13X molecular sieve (powder) in simulated seawater and deionized water shows that the enrichment efficiency of the 13X molecular sieve (powder) on the radionuclide zirconium is obviously reduced under the influence of high salt concentration of seawater.
Comparative example 3
Deionized water is used as a solvent to prepare 50mL of Ag-containing solution+、Zn2+、Fe3+、Zr4+、Ce4+Adding 0.05g of 4A molecular sieve (powder), magnetically stirring for 30min, filtering the sample with a 0.22um filter membrane after the reaction is finished, and using inductively coupled plasmaAnd (4) measuring the concentration of the solution before and after enrichment by a bulk emission spectrometer.
Ag+From 4.53ppm before enrichment to 0.004ppm after enrichment; zn2+The concentration of (A) is reduced from 5.07ppm before enrichment to 0.10ppm after enrichment; fe3+From 4.11ppm before enrichment to 0.14ppm after enrichment; zr4+The concentration of (A) is reduced from 5.02ppm before enrichment to 0.57ppm after enrichment; ce4+From 3.98ppm before enrichment to 0.11ppm after enrichment. So 4A molecular sieve is added to Ag in deionized water+、Zn2+、Fe3+、Zr4+、Ce4+Has obvious enriching effect.
Comparative example 4
Uses simulated seawater as solvent to prepare the solution containing Ag+The initial concentration of the solution is about 10ppm, the solution is magnetically stirred for 30min, a 0.22um filter membrane is used for filtering, 100mL of filtrate is taken, 0.1g of 4A molecular sieve (powder) is added, the solution is magnetically stirred for 30min, after the reaction is finished, a sample is filtered by the 0.22um filter membrane, and the concentration of the solution before and after enrichment is measured by using an inductively coupled plasma emission spectrometer.
The initial concentration of the preparation is 10ppm, the concentration of the residual silver ions is only 1.5ppm after the silver ions in the seawater react with the sodium chloride, and the enrichment experiment is carried out on the residual silver ions. Ag before enrichment+The concentration of (A) is 1.58ppm, Ag is enriched+The concentration of the silver ion is 1.55ppm, and the concentration of the silver ion is not changed before and after enrichment, so that the 4A molecular sieve has no enrichment effect on the silver ion in the simulated seawater.
Comparative example 5
Preparing 50mL of Zn-containing solution by using simulated seawater as a solvent2+、Fe3+、Ce4+Adding 0.05g of 4A molecular sieve (powder), magnetically stirring for 30min, filtering a sample by using a 0.22um filter membrane after the reaction is finished, and measuring the concentration of the solution before and after enrichment by using an inductively coupled plasma emission spectrometer.
Zn before enrichment2+Has a concentration of 7.88ppm and is enriched with Zn2+The concentration of (A) is 7.8ppm, and the concentration of zinc ions before and after enrichment is not changed, so that the molecular sieve is used for simulating seaThe zinc ions in the water have no enrichment effect; fe before enrichment3+Has a concentration of 12.96ppm and is enriched in Fe3+The concentration of the molecular sieve is 12.8ppm, and the concentration of iron ions is not changed before and after enrichment, so that the molecular sieve has no enrichment effect on the iron ions in the simulated seawater; ce before enrichment4+Has a concentration of 6.66ppm and is enriched with Ce4+The concentration of (2) is 6.64ppm, and the concentration of cerium ions is not changed before and after enrichment, so that the molecular sieve has no enrichment effect on the cerium ions in the simulated seawater.
According to the measurement results of the examples and the comparative examples, under the influence of high salt concentration of seawater, the enrichment efficiency of the 3A molecular sieve and the 13X molecular sieve on the radionuclide zirconium is obviously reduced, and the enrichment efficiency of the 4A molecular sieve on the radionuclide zirconium is still kept as high as that of pure water. Meanwhile, the 4A molecular sieve is influenced by the high salt concentration of seawater to Ag+、Zn2+、Fe3+、Ce4+The enrichment efficiency of the molecular sieve is reduced to almost zero from more than 95% in pure water, which shows that the 4A molecular sieve can selectively and quickly realize the quick enrichment of the artificial radionuclide zirconium nuclide in the seawater, can be further applied to conventional monitoring of zirconium nuclide pollution in offshore areas or emergency monitoring of nuclear accidents, and quickly enrich the artificial radionuclide zirconium in the seawater under the condition of sudden nuclear pollution so as to monitor the pollution degree of the artificial radionuclide zirconium in the seawater.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (7)

  1. The application of the 4A molecular sieve in the rapid enrichment of the artificial radionuclide zirconium in the ocean is characterized in that the 4A molecular sieve is mixed with seawater containing the artificial radionuclide zirconium, and the artificial radionuclide zirconium in the seawater is rapidly enriched by the molecular sieve.
  2. 2. The use of the 4A molecular sieve of claim 1 for the rapid enrichment of the marine artificial radionuclide zirconium, wherein the concentration of the marine artificial radionuclide zirconium is below 100 ppm.
  3. 3. The use of the molecular sieve of claim 1 or 2 for rapid enrichment of the marine artificial radionuclide zirconium, wherein the 4A molecular sieve is mixed with seawater in a mass-to-volume ratio of 1-10g: 1L.
  4. 4. Use of a molecular sieve according to any one of claims 1-3 for the rapid enrichment of the marine artificial radionuclide zirconium, wherein the time of the enrichment is 1-30 min.
  5. 5. Use of a molecular sieve according to any one of claims 1-4 for the rapid enrichment of the artificial radionuclide zirconium in the ocean, wherein the seawater has a pH of 7.5-8.5.
  6. 6. Use of the molecular sieve of any one of claims 1 to 5 for the rapid enrichment of the artificial radionuclide zirconium in the ocean, wherein the 4A molecular sieve is enriched by mixing with seawater at room temperature.
  7. 7. Use of the 4A molecular sieve according to any one of claims 1-6 for the rapid enrichment of the marine artificial radionuclide zirconium, wherein the 4A molecular sieve is in powder form.
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Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013142573A (en) * 2012-01-10 2013-07-22 Japan Atomic Energy Agency Method for separating/removing radioactive element from liquid
CN104014360A (en) * 2014-06-12 2014-09-03 东南大学 Multi-metal oxygen-group catalyst for unsymmetrical dimethylhydrazine degradation and preparation method and application thereof
CN207337948U (en) * 2017-08-18 2018-05-08 华北电力大学 A kind of radioactivity seawater treatment apparatus
CN207611618U (en) * 2017-09-14 2018-07-13 华北电力大学 Radionuclide collection device in a kind of ocean
CN110124641A (en) * 2019-04-29 2019-08-16 华中科技大学 A kind of radionuclide adsorbent material and its preparation method and application

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