CN111161901B - Method for treating radioactive iodine waste - Google Patents
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- CN111161901B CN111161901B CN202010005477.4A CN202010005477A CN111161901B CN 111161901 B CN111161901 B CN 111161901B CN 202010005477 A CN202010005477 A CN 202010005477A CN 111161901 B CN111161901 B CN 111161901B
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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
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- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/28—Treating solids
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- G21F9/301—Processing by fixation in stable solid media
- G21F9/302—Processing by fixation in stable solid media in an inorganic matrix
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- 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
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Abstract
The invention discloses a method for treating radioactive iodine waste, which comprises the following steps: s1, reacting the radioactive iodine waste with sodium hydroxide to obtain radioactive iodine waste conversion product powder; s2, sintering boron oxide, bismuth oxide and zinc oxide into glass blocks, and preparing the glass blocks into glass powder; s3, mixing the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder with deionized water to prepare a mixture; and S4, hydrolyzing and evaporating the mixture to dryness, and sintering to obtain a solidified body of radioactive iodine waste.
Description
Technical Field
The embodiment of the invention relates to the technical field of radioactive waste treatment, in particular to a method for treating radioactive iodine waste.
Background
The rapid development of nuclear energy is accompanied by the production of large quantities of nuclear waste, in which iodine-129 etc. are usually expressed as I-、IO3 -、I2、IO-Or CH3I, and the like, and the volatilized waste not only causes pollution to the environment, but also harms human health. Therefore, the method has important significance for treating the nuclear waste.
In the early development of the nuclear industry, radioactive iodine is generally treated by marine treatment methods, but the amount of iodine accumulated in the sea gradually increases with the passage of time. Thus, the marine treatment method does not meet the requirement for long-term treatment of radioactive iodine-129.
The prior radioactive iodine treatment methods mainly comprise cement, plastic, asphalt curing methods and the like. These methods can treat radioactive iodine to some extent, but have problems such as poor stability of the cured product and easy secondary pollution, and the treatment effect is not satisfactory.
Disclosure of Invention
The main object of the present invention is to provide a method for treatment of radioactive iodine waste, solving at least one of the above technical problems.
According to one aspect of the present invention, there is provided a method of treating radioactive iodine waste, comprising the steps of: s1, reacting the radioactive iodine waste with sodium hydroxide to obtain radioactive iodine waste conversion product powder; s2, sintering boron oxide, bismuth oxide and zinc oxide into glass blocks, and preparing the glass blocks into glass powder; s3, mixing the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder with deionized water to prepare a mixture; and S4, hydrolyzing and evaporating the mixture to dryness, and sintering to obtain a solidified body of radioactive iodine waste.
According to some embodiments, in step S2, the mass ratio of boron oxide, bismuth oxide, and zinc oxide is 40-70: 22-48: 8-12.
According to some embodiments, in step S2, the sintering process includes: raising the temperature from room temperature to 900-1000 ℃ at the temperature raising rate of 5 ℃/min and keeping the temperature for 1 h.
According to some embodiments, in step S2, the average particle size of the glass frit is made to be 0.5 to 1 cm.
According to some embodiments, in step S3, the 4A zeolite, the radioactive iodine waste conversion powder, and the glass frit are mixed first, and then deionized water is added.
According to some embodiments, in step S3, the mass ratio of the 4A zeolite, radioactive iodine waste conversion powder and glass frit is 40-65: 30-40: 5-20.
According to some embodiments, the mass ratio of the mixture of the 4A zeolite, the radioactive iodine waste conversion powder and the glass frit to the deionized water in step S3 is 1:10 to 1: 20.
According to some embodiments, in step S3, the average particle size of the solidified substance in the mixture is 5 to 7 μm.
According to some embodiments, in step S3, after mixing, a milling refinement, homogenization treatment is performed to obtain the mixture.
According to some embodiments, the temperature for hydrolysis and evaporation to dryness in step S4 is 200 ℃ to 250 ℃ for 3-6 h.
According to some embodiments, in step S4, the sintering process includes: raising the temperature from room temperature to 600-1100 ℃ at the temperature raising rate of 5 ℃/min and keeping the temperature for 30 min.
According to some embodiments, in steps S2 and S4, the temperature reduction process of the sintering process is natural temperature reduction to room temperature.
In the method for treating radioactive iodine waste according to the embodiment of the present invention, the solidified body of radioactive iodine waste, which can double-solidify radioactive iodine waste and has good stability, can be obtained by hydrolyzing and evaporating the mixture of the 4A zeolite, the radioactive iodine waste conversion substance powder, the glass powder and the deionized water to dryness and then sintering the mixture.
Drawings
Other objects and advantages of the present invention will become apparent from the following description of the invention which refers to the accompanying drawings, and may assist in a comprehensive understanding of the invention.
Fig. 1 shows a flow chart of a method of treatment of radioactive iodine waste according to an exemplary embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings. Implementations not depicted or described in the drawings are of a form known to those of ordinary skill in the art. Additionally, while exemplifications of parameters including particular values may be provided herein, it is to be understood that the parameters need not be exactly equal to the respective values, but may be approximated to the respective values within acceptable error margins or design constraints.
Fig. 1 shows a flow chart of a method for treating radioactive iodine waste according to an exemplary embodiment of the present invention, and as shown in fig. 1, the method for treating radioactive iodine waste includes the steps of:
s1, reacting the radioactive iodine waste with sodium hydroxide to obtain radioactive iodine waste conversion product powder;
s2, sintering boron oxide, bismuth oxide and zinc oxide into glass blocks, and preparing the glass blocks into glass powder;
s3, mixing the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder with deionized water to prepare a mixture; and
and S4, hydrolyzing and evaporating the mixture to dryness, and sintering to obtain a solidified body of radioactive iodine waste.
In the method for treating radioactive iodine waste according to the embodiment of the present invention, the solidified body of radioactive iodine waste, which can double-solidify radioactive iodine waste and has good stability, can be obtained by hydrolyzing and evaporating the mixture of the 4A zeolite, the radioactive iodine waste conversion substance powder, the glass powder and the deionized water to dryness and then sintering the mixture. In the obtained cured product, iodine was present in Na4Al3Si3O12In the I crystal phase, the solidified body also comprises a glass phase, so that radioactive iodine waste can be doubly solidified.
In step S1, in gaseous state I2For example, the gaseous phase I emitted from nuclear waste2Reacting with solid sodium hydroxide to generate sodium iodide, sodium iodate and water, wherein the reaction equation is as follows:
3I2+6NaOH＝5NaI+NaIO3+3H2O
the solid obtained from the reaction can be ground and refined into radioactive iodine waste conversion substance powder. In step S1, the mass ratio of radioactive iodine waste to sodium hydroxide may be 70-80: 20-30.
In step S2, weighing boron oxide, bismuth oxide and zinc oxide in predetermined amount according to the proportion, maintaining the temperature for 1h in the temperature range of 900-1000 ℃, and sintering to obtain B2O3-Bi2O3-ZnO ternary glass. The mass ratio of boron oxide, bismuth oxide and zinc oxide can be 40-70: 22-48: 8-12. The temperature rise rate during sintering can be 5 ℃/min, and the temperature rise is started from room temperature. And after the heat preservation process is finished, naturally cooling to room temperature. Then the glass blocks are made into glass powder, and the average grain diameter of the glass powder can be 0.5-1 cm. The glass frit may be prepared by any method suitable for preparing powder, such as mechanical milling, air milling, etc.
In step S3, the 4A zeolite, the radioactive iodine waste conversion powder obtained in step S1, and the glass frit obtained in step S2 are mixed with deionized water. The 4A zeolite is usually in powder form and has the chemical formula Na12[Al12Si12O48]·27H2O is a three-dimensional skeleton structure compound consisting of silicon oxygen and aluminum tetrahedron, and has no pollution to the environment. In one embodiment, the preset amount of 4A zeolite, radioactive iodine waste conversion powder, glass powder and deionized water can be directly selected and mixed according to the proportion. Alternatively, the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder may be mixed uniformly, and then deionized water is added, in this embodiment, the mass ratio of the mixture of the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder to the deionized water may be 1:10 to 1:20, wherein the mass ratio of the 4A zeolite, the radioactive iodine waste conversion substance powder to the glass powder may be 40 to 65: 30-40: 5-20.
After mixing the 4A zeolite, radioactive iodine waste conversion substance powder, glass powder and deionized water, grinding, refining and homogenizing treatment can be carried out to prepare a wet and uniform mixture. In the embodiment of the invention, the grinding and refining treatment can be carried out by a colloid mill, and a stirring process exists in the grinding and refining process, so that the effect of homogenization treatment can be achieved. The average particle diameter of the solidified material in the uniformly wetted mixture can be set to 5 to 7 μm.
In step S4, the uniformly wet mixture is hydrolyzed and dried at a temperature of 200 ℃ to 250 ℃ for 3-6 h. Then, the temperature is kept within the temperature range of 600-1100 ℃ for 30min for sintering, and the solidified body of the radioactive iodine waste is obtained. The temperature rise rate during sintering can be 5 ℃/min, and the temperature rise is started from room temperature. And after the heat preservation process is finished, naturally cooling to room temperature.
The following description is based on specific examples.
Example 1
The radioactive iodine waste is treated according to the following steps:
step S11, discharging 280g of nuclear waste to obtain gaseous I2Reacting with 80g of sodium hydroxide to obtain radioactive iodine waste conversion substance powder;
step S12, uniformly mixing 40g of boron oxide powder, 48g of bismuth oxide powder and 12g of zinc oxide powder, placing the mixture in a muffle furnace (MFLC-7/12P type Tester instruments Co., Ltd., Tianjin) to raise the temperature from room temperature to 1000 ℃ at a heating rate of 5 ℃/min, preserving the temperature for 1h, and naturally cooling to room temperature to obtain B2O3-Bi2O3-a ZnO ternary glass block; then, grinding the obtained glass body until the average grain diameter of the glass powder is 0.5 cm;
step S13, mixing 40g of 4A zeolite, 40g of radioactive iodine waste conversion powder and 20g of glass powder, grinding in a colloid mill (JF-130 type, guantong mechanical ltd, corridor, city), and drying at 80 ℃ for 12 h; then adding deionized water into a mixture of 4A zeolite, radioactive iodine waste conversion substance powder and glass powder, wherein the mass ratio of solid to liquid is 1:10, and further carrying out grinding, refining and homogenization treatment to obtain a uniformly wet mixture, so that the average particle size of a cured substance in the mixture is 5 microns;
step S14, hydrolyzing the uniformly moistened mixture in a high-temperature physical and chemical box (DHG-9148A, Shanghai sperm macro experimental equipment Co., Ltd.) and evaporating to dryness at 200 ℃ for 3 h; then sintering is carried out, wherein the sintering process comprises the following steps: heating to 600 ℃ from room temperature at the heating rate of 5 ℃/min, preserving heat for 30min, and naturally cooling to room temperature to obtain the solidified body of the radioactive iodine waste.
The experimental results are as follows:
XRD test of the obtained solidified body of radioactive iodine waste shows that the main diffraction peak of the phase of the solidified body is Na4Al3Si3O12I, in addition to which a small amount of NaAlSi is present2O6While the glass frit is present in the form of a glass phase in the solidified body; the bulk density of the obtained cured product was 3.281g/cm3(ii) a The standardized extraction rate of radionuclide I under the Product Consistency Test (PCT) is less than 3.32X 10 after 42 days-3g·m-2·d-1. Wherein, the leaching rate indicates the leaching degree of the element to be extracted, namely the leaching percentage of the element, and the smaller the leaching rate, the better the stability of the solidified body; the extraction rate can be determined by the method described in (Sakuragi T, Nishimura T, Nasu Y, et al. immobilization of radioactive iodine using AgI vision technique for the TRU waters disposa: evaluation of learning and surface properties [ J].MRS Online Proceedings Library Archive,2008,1107.)。
Example 2
The radioactive iodine waste is treated according to the following steps:
step S21, discharging 280g of nuclear waste to obtain gaseous I2Reacting with 80g of sodium hydroxide to obtain radioactive iodine waste conversion substance powder;
step S22, uniformly mixing 40g of boron oxide powder, 48g of bismuth oxide powder and 12g of zinc oxide powder, placing the mixture in a muffle furnace (MFLC-7/12P type Tester instruments Co., Ltd., Tianjin) to raise the temperature from room temperature to 1000 ℃ at a heating rate of 5 ℃/min, preserving the temperature for 1h, and naturally cooling to room temperature to obtain B2O3-Bi2O3-a ZnO ternary glass block; then, grinding the obtained glass body until the average grain diameter of the glass powder is 0.5 cm;
step S23, mixing 40g of 4A zeolite, 40g of radioactive iodine waste conversion powder and 20g of glass powder, grinding in a colloid mill (JF-130 type, guantong mechanical ltd, corridor, city), and drying at 80 ℃ for 12 h; then adding deionized water into a mixture of 4A zeolite, radioactive iodine waste conversion substance powder and glass powder, wherein the mass ratio of solid to liquid is 1:10, and further carrying out grinding, refining and homogenization treatment to obtain a uniformly wet mixture, so that the average particle size of a cured substance in the mixture is 5 microns;
step S24, hydrolyzing the uniformly moistened mixture in a high-temperature physical and chemical box (DHG-9148A, Shanghai sperm macro experimental equipment Co., Ltd.) and evaporating to dryness at 200 ℃ for 3 h; then sintering is carried out, wherein the sintering process comprises the following steps: raising the temperature from room temperature to 1000 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 30min, and then naturally cooling to room temperature to obtain the solidified body of the radioactive iodine waste.
The experimental results are as follows:
XRD test of the obtained solidified body of radioactive iodine waste shows that the main diffraction peak of the phase of the solidified body is Na4Al3Si3O12I, in addition to which a small amount of NaAlSi is present2O6While the glass frit is present in the form of a glass phase in the solidified body; the bulk density of the obtained cured product was 3.862g/cm3(ii) a The standardized extraction rate of radionuclide I under the Product Consistency Test (PCT) is less than 6.62X 10 after 42 days-4g·m-2·d-1。
Example 3
The radioactive iodine waste is treated according to the following steps:
step S31, discharging 280g of nuclear waste to obtain gaseous I2Reacting with 80g of sodium hydroxide to obtain radioactive iodine waste conversion substance powder;
step S32, uniformly mixing 40g of boron oxide powder, 48g of bismuth oxide powder and 12g of zinc oxide powder, placing the mixture in a muffle furnace (MFLC-7/12P type) to heat the mixture from room temperature to 1000 ℃ at a heating rate of 5 ℃/min, preserving the heat for 1h, and naturally cooling the mixture to the temperature ofAt room temperature to obtain B2O3-Bi2O3-a ZnO ternary glass block; then, grinding the obtained glass body until the average grain diameter of the glass powder is 0.5 cm;
step S33, mixing 40g of 4A zeolite, 40g of radioactive iodine waste conversion powder and 20g of glass powder, grinding in a colloid mill (JF-130 type, guantong mechanical ltd, corridor, city), and drying at 80 ℃ for 12 h; then adding deionized water into a mixture of 4A zeolite, radioactive iodine waste conversion substance powder and glass powder, wherein the mass ratio of solid to liquid is 1:20, and further carrying out grinding, refining and homogenization treatment to obtain a uniformly wet mixture, so that the average particle size of a cured substance in the mixture is 5 microns;
step S34, hydrolyzing the uniformly moistened mixture in a high-temperature physical and chemical box (DHG-9148A, Shanghai sperm macro experimental equipment Co., Ltd.) and evaporating to dryness at 200 ℃ for 6 h; then sintering is carried out, wherein the sintering process comprises the following steps: raising the temperature from room temperature to 1000 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 30min, and then naturally cooling to room temperature to obtain the solidified body of the radioactive iodine waste.
The experimental results are as follows:
XRD test of the obtained solidified body of radioactive iodine waste revealed that the phase of the solidified body had a diffraction peak of Na4Al3Si3O12I, simultaneously, the glass powder exists in the solidified body in the form of a glass phase; the bulk density of the obtained cured product was 4.426g/cm3(ii) a The standardized leaching rate of radionuclide I under the Product Consistency Test (PCT) is less than 1.029X 10 after 42 days-4g·m-2·d-1。
The difference between comparative example 1 and example 2 is that the soaking temperature for sintering the solidified body in example 1 was 600 ℃ and the soaking temperature for sintering the solidified body in example 2 was 1000 ℃, and as a result, the leaching rate of example 2 was lower than that of example 1. It can be seen that, to some extent, the higher the holding temperature at which the cured body is sintered, the better the stability of the resulting cured body.
The method for treating radioactive iodine waste has the advantages of good stability of a solidified body, simple process, energy conservation, environmental protection, safety and reliability.
Although the present invention has been described in connection with the accompanying drawings, the embodiments disclosed in the drawings are intended to be illustrative of embodiments of the invention and should not be construed as limiting the invention.
It would be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the general inventive concept, the scope of which is defined in the claims and their equivalents.
Claims (12)
1. A method of treating radioactive iodine waste comprising the steps of:
s1, reacting the radioactive iodine waste with sodium hydroxide to obtain radioactive iodine waste conversion product powder;
s2, sintering boron oxide, bismuth oxide and zinc oxide into glass blocks, and preparing the glass blocks into glass powder;
s3, mixing the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder with deionized water to prepare a mixture; and
s4, hydrolyzing and evaporating the mixture to dryness, and sintering to obtain a solidified body of radioactive iodine waste;
in the step S2, weighing boron oxide, bismuth oxide and zinc oxide in preset amount according to the proportion, keeping the temperature for 1h in the temperature range of 900-1000 ℃, and sintering to obtain B2O3-Bi2O3-ZnO ternary glass.
2. The treatment method according to claim 1, wherein in step S2, the mass ratio of boron oxide, bismuth oxide and zinc oxide is 40-70: 22-48: 8-12.
3. The process of claim 1, wherein in step S2, the sintering process comprises: raising the temperature from room temperature to 900-1000 ℃ at the temperature raising rate of 5 ℃/min and keeping the temperature for 1 h.
4. The processing method according to claim 1, wherein in step S2, the average particle size of the glass frit is set to 0.5 to 1 cm.
5. The process of claim 1, wherein in step S3, the 4A zeolite, the radioactive iodine waste conversion powder and the glass frit are mixed, and then the deionized water is added.
6. The treatment method according to claim 5, wherein in step S3, the mass ratio of the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder is 40-65: 30-40: 5-20.
7. The treatment method of claim 5, wherein in the step S3, the mass ratio of the mixture of the 4A zeolite, the radioactive iodine waste conversion substance powder and the glass powder to the deionized water is 1:10 to 1: 20.
8. The method according to claim 1, wherein in step S3, the average particle size of the solidified material in the mixture is 5 to 7 μm.
9. The process of claim 1, wherein in step S3, after mixing, the mixture is ground to refine and homogenize.
10. The process as claimed in claim 1, wherein the temperature for hydrolysis and evaporation to dryness in step S4 is 200-250 ℃ for 3-6 h.
11. The process of claim 1, wherein in step S4, the sintering process comprises: raising the temperature from room temperature to 600-1100 ℃ at the temperature raising rate of 5 ℃/min and keeping the temperature for 30 min.
12. The processing method as claimed in claim 1, wherein in steps S2 and S4, the temperature of the sintering process is naturally reduced to room temperature.
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