CN111986828B - Sodalite-based ceramic-glass dual curing method for radioactive iodine waste - Google Patents
Sodalite-based ceramic-glass dual curing method for radioactive iodine waste Download PDFInfo
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- CN111986828B CN111986828B CN202010841089.XA CN202010841089A CN111986828B CN 111986828 B CN111986828 B CN 111986828B CN 202010841089 A CN202010841089 A CN 202010841089A CN 111986828 B CN111986828 B CN 111986828B
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- 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
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/28—Treating solids
- G21F9/30—Processing
- G21F9/301—Processing by fixation in stable solid media
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- 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
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/28—Treating solids
- G21F9/30—Processing
- G21F9/301—Processing by fixation in stable solid media
- G21F9/302—Processing by fixation in stable solid media in an inorganic matrix
- G21F9/304—Cement or cement-like matrix
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- 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
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/28—Treating solids
- G21F9/30—Processing
- G21F9/301—Processing by fixation in stable solid media
- G21F9/302—Processing by fixation in stable solid media in an inorganic matrix
- G21F9/305—Glass or glass like matrix
Abstract
The disclosure belongs to the technical field of radioactive waste treatment, and particularly relates to a sodalite-based ceramic-glass dual-curing method for radioactive iodine waste. The method comprises the following steps: (1) After ball milling, the 4A zeolite is mixed with silver nitrate solution and stirred under a heating state, so that the exchange reaction of silver ions and Na ions in the 4A zeolite is completed. (2) Mixing silver ion exchange zeolite, silver iodide containing radioactive iodine and glass powder, adding deionized water into the mixture, and grinding by a colloid mill; (3) And (3) putting the slurry ground by the colloid mill into a hydrolysis reaction container for hydrolysis reaction, and carrying out heat treatment on a hydrolysate to obtain the iodine-containing sodalite-based ceramic-glass solidified sintered body. The method has simple process, is safe and reliable, and can meet the requirement of long-term stable disposal of the radioactive iodine waste.
Description
Technical Field
The disclosure belongs to the technical field of radioactive waste treatment, and particularly relates to a sodalite-based ceramic-glass dual-curing method for radioactive iodine waste.
Background
The radioactive waste is inevitably generated in the processes of the front nuclear fuel circulation section, the reactor operation section, the rear nuclear fuel circulation section and the like, and the improper treatment of the radioactive waste can cause serious harm to the surrounding environment and the health of human bodies, so the treatment and disposal problems of the radioactive waste are more urgent. In a power reactor, the fission yield of radioactive iodine is high, and the radioactive iodine mainly exists in the form of radioactive nuclides such as iodine-129, iodine-131 and iodine-125, wherein the iodine-129 has a long half-life (t) 1/2 ＝1.57×10 7 a) And has the advantages of easy volatilizationThe characteristics of easy migration and easy enrichment in the thyroid of human body are widely concerned by the supervision department and the public. During spent fuel reprocessing, the vast majority of the iodine-129 is volatilized as a gas during fuel dissolution and as I 2 、I - 、IO 3 - 、IO - And CH 3 I, etc., and because of their chemical morphology, iodine-129 is difficult to trap in a single process and needs to be removed in combination with multiple processes, such as a first stage by washing and a second stage by an absorption tower. At present, post-treatment factories at home and abroad mainly adopt two methods of solution washing and solid adsorption for radioactive iodine treatment, wherein common iodine adsorbents comprise silver-coated silica gel, silver-coated zeolite, activated carbon and the like. The adsorption method of silver-coated zeolite has high iodine removal efficiency and wide application, the radioactive iodine adsorbed on the silver-coated zeolite exists mainly in the form of AgI, but the iodine-containing silver-coated zeolite has poor acid resistance, and Ag is used under the geological treatment condition + Is easily reduced into Ag to form I - And (4) releasing. Therefore, the iodine-containing silver-coated zeolite does not satisfy the requirement of long-term disposal, and needs to be converted into a cured body by some treatment process.
Sodalite is a natural aluminosilicate mineral with a theoretical chemical formula of Na 8 Al 6 Si 6 O 24 X 2 (X＝Cl - ，Br - ，I - ，OH - Etc.) have a chemical formula of [ AlO 4 ]And [ SiO ] 4 ]The clusters are connected into a cage structure, so that iodine atoms can be fixed in the cage structure to inhibit the diffusion of the iodine atoms, and the purpose of nuclide solidification is achieved. Previous studies have shown that sodalite is readily synthesized from clay minerals such as kaolin or certain chemical agents and has a low leaching rate of the core in aqueous solutions. Sodalite is considered suitable for curing radioactive iodine mineral substrates by comprehensively considering such factors as the curing process, the thermal conductivity of the cured body, the cost of the cured substrate and the leaching rate.
Disclosure of Invention
Object of the invention
In accordance with the problems of the prior art, the present disclosure provides a sodalite-based ceramic-glass dual-curing method that is simple in process, safe and reliable, and can meet the requirement of long-term stable disposal of radioactive iodine waste.
(II) technical scheme
In order to solve the problems existing in the prior art, the technical scheme provided by the disclosure is as follows:
a sodalite-based ceramic-glass dual curing method, comprising the steps of:
(1) Ball milling 4A zeolite, and making the particle diameter of 4A zeolite powder be less than 0.1mm, in which the molecular formula of 4A zeolite is Na 12 [Al 12 Si 12 O 48 ]·27H 2 O；
(2) Mixing the 4A zeolite powder obtained in the step (1) with a silver nitrate solution, stirring the mixture in a heating state, and drying the solution after silver ions completely react with Na ions in the 4A zeolite in an exchange manner to obtain silver ion exchange zeolite; wherein the reaction formula of the exchange reaction is:
(Na 12 [Al 12 Si 12 O 48 ]·27H 2 O+12AgNO 3 →Ag 12 [Al 12 Si 12 O 48 ]·27H 2 O+12NaNO 3 )；
(3) Mixing the silver ion exchange zeolite obtained in the step (2), silver iodide containing radioactive iodine and glass powder, adding deionized water into the mixture, and grinding by a colloid mill;
(4) And (3) putting the slurry after the colloid mill grinding into a hydrolysis reaction container for hydrolysis reaction at the temperature of 150-300 ℃ for 5-24 h, and drying the hydrolysis product during the hydrolysis reaction.
(5) And (4) carrying out heat treatment on the dried product in the step (4), wherein the temperature of the heat treatment is 550-900 ℃, and thus the iodine-containing sodalite-based ceramic-glass solidified sintered body can be obtained.
Preferably, the glass powder is borate glass powder, wherein the borate glass powder comprises, by mass, 40-70% of boron oxide, 22-48% of bismuth oxide and 8-12% of zinc oxide.
Preferably, the ball milling condition in the step (1) is 300-500 r/min, and the ball milling is carried out for 1-2 h.
Preferably, the concentration of the silver nitrate in the step (2) is 1-1.5 mol/L, and the amount of the silver nitrate substance exceeds the reaction stoichiometric ratio by 10%.
Preferably, in the step (2), the heating temperature is 80-90 ℃, the stirring time is 2-3 d, and the drying temperature is 120-300 ℃.
Preferably, the time of the colloid mill in the step (3) is 3-5 h.
Preferably, the mass ratios of the silver ion-exchanged zeolite, the silver iodide and the glass powder in the mixture in the step (3) are 66-78 wt.%, 14-17 wt.% and 5-20 wt.%, respectively.
Preferably, the slurry in step (4) is injected into the hydrolysis reaction vessel by a peristaltic pump.
Preferably, the heat treatment in step (5) is carried out in a muffle furnace and is divided into two steps, wherein the first step is preheating treatment at 550-600 ℃ for 15-18 h to promote AgI to enter the silver ion exchange zeolite lattice; the second step is sintering at 700-900 deg.c and normal pressure for 1-2 hr to obtain solidified sintered body of radioactive iodine waste with Ag as reaction principle 12 Al 12 Si 12 O 48 +4AgI→2Ag 8 Al 6 Si 6 O 24 I 2 。
Preferably, the solid-to-liquid ratio of the mixture to the deionized water in the step (3) is 1:4-1.
Preferably, the temperature is naturally reduced to room temperature after the heat treatment process in the step (5).
(III) advantageous effects
The sodalite-based ceramic-glass dual-curing method for radioactive iodine waste comprises the steps of firstly utilizing silver nitrate to react with 4A zeolite to obtain silver ion exchange zeolite, then utilizing the silver ion exchange zeolite to be mixed with silver iodide containing radioactive iodine and borate glass powder, then adding deionized water and carrying out rubber grinding, carrying out hydrolysis reaction on the obtained slurry, drying, and finally carrying out a series of heat treatments on the hydrolysate to obtain the iodine-containing sodalite-based ceramic-glass dual-curing sintered body. Compared with the simple ceramic solidification, the addition of the glass phase promotes the formation of sodalite, improves the mass fraction of the sodalite in a solidified crystal phase and reduces the leaching rate of iodine. The method has simple process, prepares the iodine-containing sodalite ceramic-glass dual-cured body by using the stable structure of the sodalite, and is suitable for treating radioactive iodine waste for a long time.
Detailed Description
The present application will be further described with reference to specific examples.
Example 1
A sodalite-based ceramic-glass dual curing method, comprising the steps of:
(1) And (3) putting the 4A zeolite into a ball mill for ball milling, wherein the ball milling condition is 400r/min, the ball milling is suspended for 6min every 20min, and the ball milling is carried out for 1.5h after the ball milling is restarted. The particle diameter of 4A zeolite powder after ball milling is 0.09mm, wherein the molecular formula of 4A zeolite is Na 12 [Al 12 Si 12 O 48 ]·27H 2 O; the ball mill is a PULVERISTET 6 ball mill sold by Beijing flying scientific instruments Co.
(2) Mixing the 4A zeolite powder obtained in the step (1) with a silver nitrate solution with the concentration of 1.2mol/L, wherein the amount of silver nitrate substances exceeds the reaction stoichiometric ratio by 10%. The 4A zeolite powder is mixed with silver nitrate solution and stirred for 2.5 days at 85 ℃. After the silver ions completely exchange and react with Na ions in the 4A zeolite, drying the solution at 150 ℃ to obtain silver ion exchange zeolite; wherein the exchange reaction has the formula: (Na) 12 [Al 12 Si 12 O 48 ]·27H 2 O+12AgNO 3 →Ag 12 [Al 12 Si 12 O 48 ]·27H 2 O+12NaNO 3 )；
(3) Mixing the silver ion exchange zeolite obtained in the step (2), silver iodide containing radioactive iodine and glass powder, and adding deionized water colloid mill for grinding for 4 hours, wherein the ratio of the mixture to the deionized water is 1:7; the glass powder is borate glass powder, wherein the borate glass powder comprises, by mass, 45% of boron oxide, 43% of bismuth oxide and 12% of zinc oxide. In the mixture, 66wt.% of silver ion-exchanged zeolite, 14wt.% of silver iodide, and 20wt.% of glass frit were present.
(4) Putting the slurry after colloid milling into a hydrolysis reaction container through a peristaltic pump for hydrolysis reaction at the temperature of 200 ℃ for 15h, and drying the slurry while performing the hydrolysis reaction to obtain an aluminosilicate precursor;
(5) Carrying out heat treatment on the product dried in the step (4), wherein the heat treatment is carried out in a muffle furnace and is divided into two steps, and the first step is preheating treatment for 16 hours at 580 ℃ to promote AgI to enter a silver ion exchange zeolite lattice; the second step is sintering at 800 deg.C for 1.5h under normal pressure to obtain solidified sintered body of radioactive iodine waste, and the reaction principle is Ag 12 Al 12 Si 12 O 48 +4AgI→2Ag 8 Al 6 Si 6 O 24 I 2 . And naturally cooling to room temperature after the heat treatment process.
XRD test shows that the solidified matter phase of the prepared iodine waste has main diffraction peak Ag 4 Al 3 Si 3 O 12 I, the extraction rate of radionuclide I under PCT standard (the extraction rate indicates the degree of extraction of the element to be extracted, i.e., the percentage of the element extracted; the extraction rate is determined by Sakuragi T, nishimura T, nasu Y, et al]MRS one Proceedings Library Archive,2008,1107.) was less than 3.1X 10 after 7 days -5 g·m -2 ·d -1 . Compared with the simple ceramic solidification, the content of sodalite in the crystal phase in the ceramic-glass dual solidified body is improved by 7wt.%, and the leaching rate of iodine element is reduced to 4.7 multiplied by 10 -6 g·m -2 ·d -1 。
Example 2
A sodalite-based ceramic-glass dual curing method, comprising the steps of:
(1) And (3) putting the 4A zeolite into a ball mill for ball milling, wherein the ball milling condition is 300r/min, the ball milling is suspended for 5min every 20min, and the ball milling is carried out for 2h after the ball milling is restarted. The particle diameter of 4A zeolite powder after ball milling is 0.096mm, wherein the molecular formula of 4A zeolite is Na 12 [Al 12 Si 12 O 48 ]·27H 2 O; the ball mill is a PULVERISTET 6 ball mill sold by Beijing flying scientific instruments Co.
(2) Mixing the 4A zeolite powder obtained in the step (1) with a silver nitrate solution with the concentration of 1mol/L, wherein the amount of silver nitrate substances exceeds the reaction stoichiometric ratio by 10%. Mixing the 4A zeolite powder with a silver nitrate solution, and stirring for 3d at 80 ℃. After the silver ions completely react with Na ions in the 4A zeolite in an exchange manner, drying the solution at 250 ℃ to obtain silver ion exchange zeolite; wherein the exchange reaction has the formula: (Na) 12 [Al 12 Si 12 O 48 ]·27H 2 O+12AgNO 3 →Ag 12 [Al 12 Si 12 O 48 ]·27H 2 O+12NaNO 3 )；
(3) Mixing the silver ion exchange zeolite obtained in the step (2), silver iodide containing radioactive iodine and glass powder, and adding deionized water colloid mill for grinding for 3h, wherein the ratio of the mixture to the deionized water is 1:4; the glass powder is borate glass powder, wherein the borate glass powder comprises 45% of boron oxide, 45% of bismuth oxide and 10% of zinc oxide in percentage by mass. In the mixture, 74wt.% of silver ion-exchanged zeolite, 16wt.% of silver iodide and 10wt.% of glass frit were present.
(4) Putting the slurry after colloid milling into a hydrolysis reaction container through a peristaltic pump for hydrolysis reaction at the temperature of 150 ℃ for 24 hours, and drying the slurry while performing the hydrolysis reaction to obtain an aluminosilicate precursor;
(5) Carrying out heat treatment on the dried product in the step (4), wherein the heat treatment is carried out in a muffle furnace and is divided into two steps, and the first step is preheating treatment for 18 hours at 550 ℃ to promote AgI to enter a silver ion exchange zeolite lattice; the second step is sintering at 700 ℃ for 2h under normal pressure to obtain a solidified sintered body of radioactive iodine waste, and the reaction principle is Ag 12 Al 12 Si 12 O 48 +4AgI→2Ag 8 Al 6 Si 6 O 24 I 2 . And naturally cooling to room temperature after the heat treatment process.
XRD tests show that the solidified body phase of the prepared iodine waste has a main diffraction peak Ag 4 Al 3 Si 3 O 12 I, leaching rate of radionuclide I under PCT standard (leaching rate indicates that the element to be extracted is leached outThe degree, i.e. the percentage of the element leached; the extraction rate can be determined by Sakuragi T, nishimura T, nasu Y, et al, mobility of radioactive iodine using AgI vision technique for the TRU waters disposa, evaluation of learning and surface properties [ J]MRS one Proceedings Library Archive,2008,1107.) below 2.3X 10 after 7 days -6 g·m -2 ·d -1 。
Example 3
A sodalite-based ceramic-glass dual curing method, comprising the steps of:
(1) And (3) putting the 4A zeolite into a ball mill for ball milling, wherein the ball milling condition is 500r/min, the ball milling is suspended for 8min every 20min, and the ball milling is carried out for 1h after the ball milling is restarted. The particle diameter of the 4A zeolite powder after ball milling is 0.08mm, wherein the molecular formula of the 4A zeolite is Na 12 [Al 12 Si 12 O 48 ]·27H 2 O; the ball mill model is MQG0909 sold by the cigarette Tai Jinpeng mining machinery Co.
(2) Mixing the 4A zeolite powder obtained in the step (1) with a silver nitrate solution with the concentration of 15mol/L, wherein the amount of silver nitrate substances exceeds the reaction stoichiometric ratio by 10%. The 4A zeolite powder is mixed with silver nitrate solution and stirred for 2 days at 90 ℃. After the silver ions completely react with Na ions in the 4A zeolite in an exchange manner, drying the solution at 300 ℃ to obtain silver ion exchange zeolite; wherein the exchange reaction has the formula: (Na) 12 [Al 12 Si 12 O 48 ]·27H 2 O+12AgNO 3 →Ag 12 [Al 12 Si 12 O 48 ]·27H 2 O+12NaNO 3 )；
(3) Mixing the silver ion exchange zeolite obtained in the step (2), silver iodide containing radioactive iodine and glass powder, wherein the ratio of the mixture to deionized water is 1; the glass powder is borate glass powder, wherein the borate glass powder comprises, by mass, 60% of boron oxide, 29% of bismuth oxide and 11% of zinc oxide. In the mixture, 78wt.% of silver ion-exchanged zeolite, 15wt.% of silver iodide and 7wt.% of glass frit were present.
(4) Putting the slurry after colloid milling into a hydrolysis reaction container through a peristaltic pump for hydrolysis reaction at the temperature of 200 ℃ for 15h, and drying the hydrolysate during the hydrolysis reaction;
(5) Carrying out heat treatment on the product dried in the step (4), wherein the heat treatment is carried out in a muffle furnace and is divided into two steps, and the first step is preheating treatment at 600 ℃ for 15 hours to promote AgI to enter a silver ion exchange zeolite lattice; the second step is sintering at 900 deg.C under normal pressure for 1h to obtain solidified sintered body of radioactive iodine waste, and the reaction principle is Ag 12 Al 12 Si 12 O 48 +4AgI→2Ag 8 Al 6 Si 6 O 24 I 2 . And naturally cooling to room temperature after the heat treatment process.
XRD tests show that the solidified body phase of the prepared iodine waste has a main diffraction peak Ag 4 Al 3 Si 3 O 12 I, the extraction rate of radionuclide I under PCT standard (the extraction rate indicates the degree of extraction of the element to be extracted, i.e., the percentage of the element extracted; the extraction rate is determined by Sakuragi T, nishimura T, nasu Y, et al]MRS one Proceedings Library Archive,2008,1107) is less than 3.1 × 10 after 7 days -6 g·m -2 ·d -1 。
Claims (11)
1. A sodalite-based ceramic-glass dual-curing method, characterized in that it comprises the steps of:
(1) Ball milling 4A zeolite, and making the particle diameter of 4A zeolite powder be less than 0.1mm, in which the molecular formula of 4A zeolite is Na 12 [Al 12 Si 12 O 48 ]·27H 2 O；
(2) Mixing the 4A zeolite powder obtained in the step (1) with a silver nitrate solution with the concentration of 1-1.5 mol/L, stirring the mixture in a heating state, and drying the solution after the silver ions completely exchange with Na ions in the 4A zeolite to obtain silver ion exchange zeolite; wherein the exchange reaction has the formula:
(Na 12 [Al 12 Si 12 O 48 ]·27H 2 O+12AgNO 3 →Ag 12 [Al 12 Si 12 O 48 ]·27H 2 O+12NaNO 3 )；
(3) Mixing the silver ion exchange zeolite obtained in the step (2), silver iodide containing radioactive iodine and borate glass powder, adding deionized water into the mixture, and grinding by a colloid mill;
(4) Putting the slurry ground by the colloid mill into a hydrolysis reaction container for hydrolysis reaction at the temperature of 150-300 ℃ for 5-24 h, and drying the hydrolysate during the hydrolysis reaction;
(5) And (3) carrying out two-step heat treatment on the dried product in the step (4), wherein the temperature of the heat treatment is 550-900 ℃, and thus the iodine-containing sodalite-based ceramic-glass solidified sintered body can be obtained.
2. The sodalite-based ceramic-glass dual-curing method according to claim 1, wherein the glass frit is a borate glass frit, wherein the borate glass frit comprises, by mass, 40-70% of boron oxide, 22-48% of bismuth oxide, and 8-12% of zinc oxide.
3. The sodalite-based ceramic-glass dual-curing method according to claim 1, wherein the ball milling conditions in step (1) are 300-500 r/min and 1-2 h.
4. The sodalite-based ceramic-glass dual curing method according to claim 1, wherein the amount of silver nitrate substance in step (2) exceeds the reaction stoichiometry by 10%.
5. The sodalite-based ceramic-glass dual curing method according to claim 1, wherein the heating temperature in step (2) is 80-90 ℃, the stirring time is 2-3 d, and the drying temperature is 120-300 ℃.
6. The sodalite-based ceramic-glass dual-curing method according to claim 1, wherein the colloid mill grinding time in step (3) is 3 to 5 hours.
7. The sodalite-based ceramic-glass dual curing method according to claim 1, wherein the mass ratios of the silver ion-exchanged zeolite, the silver iodide, and the glass frit in the mixture in step (3) are 66 to 78wt.%,14 to 17wt.%, and 5 to 20wt.%, respectively.
8. The sodalite-based ceramic-glass dual curing method according to claim 1, wherein the slurry in step (4) is injected into the hydrolysis reaction vessel by a peristaltic pump.
9. The dual sodalite-based ceramic-glass curing method according to claim 1, wherein the heat treatment in step (5) is performed in a muffle furnace and is divided into two steps, the first step is a preheating treatment at 550-600 ℃ for 15-18 h to drive AgI into the silver ion-exchanged zeolite lattice; the second step is sintering at 700-900 deg.c and normal pressure for 1-2 hr to obtain solidified sintered body of radioactive iodine waste with Ag as reaction principle 12 Al 12 Si 12 O 48 +4AgI→2Ag 8 Al 6 Si 6 O 24 I 2 。
10. The sodalite-based ceramic-glass dual curing method according to claim 1, wherein the solid-to-liquid ratio of the mixture to the deionized water in step (3) is 1:4-1.
11. The sodalite-based ceramic-glass dual-curing method according to claim 1, wherein the temperature is naturally decreased to room temperature after the heat treatment process in the step (5).
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| CN114550965B (en) * | 2021-12-27 | 2024-02-20 | 中国原子能科学研究院 | Method for curing sodium metaaluminate-silica gel system ceramic of radioactive cesium waste |
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