CN117700077A - Glass and glass beads with high composition consistency for curing high radioactive waste liquid and preparation method thereof - Google Patents
Glass and glass beads with high composition consistency for curing high radioactive waste liquid and preparation method thereof Download PDFInfo
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- CN117700077A CN117700077A CN202311730399.4A CN202311730399A CN117700077A CN 117700077 A CN117700077 A CN 117700077A CN 202311730399 A CN202311730399 A CN 202311730399A CN 117700077 A CN117700077 A CN 117700077A
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- 239000011521 glass Substances 0.000 title claims abstract description 96
- 239000007788 liquid Substances 0.000 title claims abstract description 33
- 239000011324 bead Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000203 mixture Substances 0.000 title claims description 19
- 239000002901 radioactive waste Substances 0.000 title claims description 3
- 239000002927 high level radioactive waste Substances 0.000 claims abstract description 33
- 239000013067 intermediate product Substances 0.000 claims abstract description 33
- 238000002844 melting Methods 0.000 claims abstract description 31
- 230000008018 melting Effects 0.000 claims abstract description 31
- 238000004458 analytical method Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 21
- 238000009472 formulation Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 238000004846 x-ray emission Methods 0.000 claims description 9
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 abstract description 8
- 238000007711 solidification Methods 0.000 abstract description 4
- 230000008023 solidification Effects 0.000 abstract description 4
- 235000013350 formula milk Nutrition 0.000 description 13
- 229910010413 TiO 2 Inorganic materials 0.000 description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 229910018068 Li 2 O Inorganic materials 0.000 description 4
- 239000005388 borosilicate glass Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 229910052770 Uranium Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000002915 spent fuel radioactive waste Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052778 Plutonium Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002925 low-level radioactive waste Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 235000020610 powder formula Nutrition 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011268 retreatment Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
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- Glass Compositions (AREA)
Abstract
The invention belongs to the technical field of high-level waste liquid treatment, and particularly relates to glass and glass beads with high consistency of components for curing high-level waste liquid and a preparation method thereof. The invention determines the recipe and allowable setting error of the glass; according to the formula of the glass, mixing raw materials, and then carrying out high-temperature melting to obtain an intermediate product; carrying out component analysis on the intermediate product to obtain the content of each component; comparing the obtained component contents with the corresponding component contents in the glass formula to obtain a difference value, and re-determining the formula according to the difference value; and (3) until the absolute value of the difference value of the contents of all the components is smaller than 50% of the set error, obtaining the glass with high consistency of the components for curing the high-level waste liquid. The preparation method provided by the invention can be used for rapidly obtaining the glass with high ingredient consistency, and further, the glass bead with high ingredient consistency can be obtained by taking the glass as a raw material, so that the solidification treatment of the high-level waste liquid can be better realized.
Description
Technical Field
The invention belongs to the technical field of high-level waste liquid treatment, and particularly relates to glass and glass beads with high consistency of components for curing high-level waste liquid and a preparation method thereof.
Background
The closed nuclear fuel circulation treatment technology mainly carries out retreatment on Spent Nuclear Fuel (SNF) through different processes so as to recycle residual Transuranics (TRUs), such as uranium (U) and plutonium (Pu), which fully and repeatedly recycle the nuclear fuel, thereby achieving the purposes of thoroughly incinerating U, pu and TRUs in a nuclear energy system and minimizing the generation amount of nuclear waste.
The post-treatment process produces high level waste streams, including fission products, unrecovered TRUs and post-treatment additives. At present, the glass curing technology is the only industrialized application technology for fixing the high-level waste liquid.
Borosilicate glass is widely considered as a suitable glass substrate, borosilicate glass formulations of different waste components are systematically developed by national laboratories in the united states of america, the pacific northwest, and a borosilicate cured glass database is established, the feasibility of curing high level waste by joule heating ceramic furnace glass is verified, and a valley glass curing demonstration device, a national defense waste treatment device and a heftir glass curing facility are sequentially established for curing medium and low level waste and high level waste. Because borosilicate glass has a relatively high glass transition temperature and high capacity for different radionuclides, long-term stability of the cured body can be ensured.
The high-level waste liquid glass solidification is the process of forming a glass solidified body by high-temperature melting of the high-level waste liquid and the borosilicate glass substrate together. Because the power stack high-level discharge waste liquid has complex components and usually contains indissolvable elements and noble metals (Ru, rh and Pd), wherein the indissolvable elements Mo and S have limited solubility in a glass solidified body, are easy to be separated out in a yellow phase form (containing radioactive elements Sr and Cs) to cause rapid reduction of chemical stability, and the noble metal elements are easy to be settled at the furnace bottom to generate great harm to a discharging process due to relatively larger specific gravity.
Disclosure of Invention
The invention aims to provide glass and glass beads with high ingredient consistency for curing high-level waste liquid and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of glass powder with high consistency of components for curing high-level radioactive waste liquid, which comprises the following steps:
(1) Determining the recipe and allowable setting errors of the glass;
(2) According to the formula of the glass, mixing raw materials, and then carrying out high-temperature melting to obtain an intermediate product;
(3) Carrying out component analysis on the intermediate product to obtain the content of each component;
(4) Comparing the obtained component contents with the corresponding component contents in the glass formula to obtain a difference value; if the absolute value of the difference is greater than or equal to 50% of the set error, subtracting the difference from the corresponding component content in the glass formulation, and re-determining the formulation of the glass;
(5) Repeating the steps (2) - (4) until the absolute value of the difference value of all the component contents is less than 50% of the set error, and obtaining the glass with high consistency of the components for curing the high-level waste liquid.
Preferably, the absolute value of the setting error is 20 to 75%.
Preferably, the high temperature melting temperature is 1300-1520 ℃.
Preferably, the process of component analysis includes:
mixing the intermediate product with lithium tetraborate for the first time, and carrying out first melting to obtain a first sample to be tested; analyzing the first sample to be detected by using an X-ray fluorescence spectrometry to obtain the content of oxide corresponding to the element with the atomic number less than or equal to 11;
secondly mixing the intermediate product with potassium hydroxide, carrying out second melting, and extracting the obtained melt by using hydrochloric acid solution to obtain a second sample to be detected; and analyzing the second sample to be tested by utilizing an ICP-AES method to obtain the content of the oxide corresponding to the element with the atomic number more than 11.
Preferably, the mass ratio of the intermediate product to the lithium tetraborate is 1:9.8 to 10.2; the temperature of the first melting is 1090-1110 ℃, and the heat preservation time is 19-21 min.
Preferably, the mass ratio of the intermediate product to the potassium hydroxide is 1:15; the temperature of the second melting is 600 ℃, and the heat preservation time is 10min.
The invention also provides the glass with high consistency of the components for curing the high-level waste liquid prepared by the preparation method.
The invention also provides a glass bead which is prepared by taking the glass with high consistency of the components for curing the high-level waste liquid as a raw material.
The invention also provides a preparation method of the glass beads, which comprises the following steps: and (3) sequentially carrying out high-temperature melting, mould pressing, crushing, fire polishing and screening on the glass with high ingredient consistency for curing the high-level waste liquid to obtain the glass beads.
The invention provides a preparation method of glass powder with high consistency of components for curing high-level radioactive waste liquid, which comprises the following steps: (1) determining the recipe and allowable setting errors of the glass; (2) According to the formula of the glass, mixing raw materials, and then carrying out high-temperature melting to obtain an intermediate product; (3) Carrying out component analysis on the intermediate product to obtain the content of each component; (4) Comparing the obtained component contents with the corresponding component contents in the glass formula to obtain a difference value; if the absolute value of the difference is greater than or equal to 50% of the set error, subtracting the difference from the corresponding component content in the glass formulation, and re-determining the formulation of the glass; (5) Repeating the steps (2) - (4) until the absolute value of the difference value of all the component contents is less than 50% of the set error, and obtaining the glass with high consistency of the components for curing the high-level waste liquid. The preparation method provided by the invention can be used for rapidly obtaining the glass with high ingredient consistency, and further, the glass bead with high ingredient consistency can be obtained by taking the glass as a raw material, and the obtained glass bead can better realize the solidification treatment of the high-level waste liquid.
Detailed Description
The invention provides a preparation method of glass powder with high consistency of components for curing high-level radioactive waste liquid, which comprises the following steps:
(1) Determining the recipe and allowable setting errors of the glass;
(2) According to the formula of the glass, mixing raw materials, and then carrying out high-temperature melting to obtain an intermediate product;
(3) Carrying out component analysis on the intermediate product to obtain the content of each component;
(4) Comparing the obtained component contents with the corresponding component contents in the glass formula to obtain a difference value; if the absolute value of the difference is greater than or equal to 50% of the set error, subtracting the difference from the corresponding component content in the glass formulation, and re-determining the formulation of the glass;
(5) Repeating the steps (2) - (4) until the absolute value of the difference value of all the component contents is less than 50% of the set error, and obtaining the glass with high consistency of the components for curing the high-level waste liquid.
In the present invention, all raw materials are commercially available products well known to those skilled in the art unless specified otherwise.
The present invention determines the recipe and allowable setting errors for the glass. In a specific embodiment of the present invention, the formulation of the glass frit preferably comprises SiO 2 、B 2 O 3 、Na 2 O、Li 2 O、Al 2 O 3 、CaO、TiO 2 MgO and Fe 2 O 3 . In the present invention, the absolute value of the setting error is preferably 20 to 75%.
After the glass formula is obtained, the invention mixes the raw materials according to the glass formula and then melts the raw materials at high temperature to obtain an intermediate product.
The mixing process is not particularly limited and may be employed as is well known to those skilled in the art. In the present invention, the high-temperature melting temperature is preferably 1300 to 1520 ℃. In the present invention, the intermediate product has a particle size of less than 75 μm.
After the intermediate product is obtained, the invention carries out component analysis on the intermediate product to obtain the content of each component.
In the present invention, the process of component analysis preferably includes:
mixing the intermediate product with lithium tetraborate for the first time, and carrying out first melting to obtain a first sample to be tested; analyzing the first sample to be detected by using an X-ray fluorescence spectrometry to obtain the content of oxide corresponding to the element with the atomic number less than or equal to 11;
secondly mixing the intermediate product with potassium hydroxide, carrying out second melting, and extracting the obtained melt by using hydrochloric acid solution to obtain a second sample to be detected; and analyzing the second sample to be tested by utilizing an ICP-AES method to obtain the content of the oxide corresponding to the element with the atomic number more than 11.
In the present invention, the mass ratio of the intermediate product to lithium tetraborate is preferably 1:9.8 to 10.2, more preferably 1:10. in the present invention, the temperature of the first melting is preferably 1090 to 1110 ℃, and more preferably 1100 ℃; the holding time is preferably 19 to 21 minutes, more preferably 20 minutes. The specific process of the X-ray fluorescence spectrometry (XRF) is not particularly limited, and may be employed as is well known to those skilled in the art. In a specific embodiment of the invention, the intermediate product is preferably tested for SiO by X-ray fluorescence spectroscopy 2 、Na 2 O、Al 2 O 3 、CaO、TiO 2 MgO and Fe 2 O 3 Is contained in the composition.
In the present invention, the mass ratio of the intermediate product to potassium hydroxide is preferably 1:15. in the present invention, the temperature of the second melting is preferably 600℃and the holding time is preferably 10 minutes. The process of extraction of the hydrochloric acid solution is not particularly limited, and may be known to those skilled in the art. The specific process of the ICP-AES method is not particularly limited, and may be known to those skilled in the art. In a particular embodiment of the invention, the intermediate product is preferably tested for B by the ICP-AES method 2 O 3 And Li (lithium) 2 O content.
In the present invention, the total time for performing one component analysis is preferably 3 hours or less.
After the contents of the components are obtained, the obtained contents of the components are compared with the contents of the corresponding components in the glass formula to obtain a difference value; and if the absolute value of the difference is greater than or equal to 50% of the set error, subtracting the difference from the corresponding component content in the glass powder formula, and re-determining the formula of the glass powder.
In the present invention, when the absolute value of the difference is greater than or equal to 50% of the component content of the setting error, fine adjustment of the unadjusted element is preferably further included so as to satisfy the total amount of each component in the formulation as 100%. In the present invention, the absolute value of the fine tuning range is preferably less than 0.1.
The steps (2) to (4) are repeated until the absolute value of the difference value of the contents of all the components is less than 50% of the set error, and the glass with high consistency of the components for curing the high-level waste liquid is obtained.
The invention also provides the glass with high consistency of the components for curing the high-level waste liquid prepared by the preparation method.
The invention also provides a glass bead which is prepared by taking the glass with high consistency of the components for curing the high-level waste liquid as a raw material.
The invention also provides a preparation method of the glass beads, which comprises the following steps: and (3) sequentially carrying out high-temperature melting, mould pressing, crushing, fire polishing and screening on the glass with high ingredient consistency for curing the high-level waste liquid to obtain the glass beads. The process of high temperature melting, molding, crushing, fire polishing and sieving is not particularly limited, and can be adopted by those skilled in the art.
In order to further illustrate the present invention, the following examples are provided to describe in detail a glass and glass bead having high consistency of ingredients for curing a high level waste liquid and a method for producing the same, but they should not be construed as limiting the scope of the present invention.
Example 1
Determining the recipe and allowable setting errors for the glass as shown in table 1;
TABLE 1 glass formulation (wt%)
Mixing the raw materials according to a formula, and then carrying out high-temperature melting at 1350 ℃ to obtain an intermediate product 1, wherein the particle size of the intermediate product is less than 75 mu m;
component analysis was performed on intermediate 1:
uniformly mixing 0.2g of intermediate product 1 and 2g of lithium tetraborate, and melting at 1100 ℃ for 20min to prepare a glass sheet, and using XRF to perform XRF on SiO in the glass sheet 2 、Na 2 O、Al 2 O 3 、CaO、TiO 2 MgO and Fe 2 O 3 Quantitative analysis is carried out;
mixing 0.2g of intermediate 1 and 3g of potassium hydroxide, melting at 600 ℃ for 10min, extracting with hydrochloric acid solution, and determining the volume to 250mL, and measuring the B in the sample by ICP-AES 2 O 3 And Li (lithium) 2 O content, total analysis time 1h; the analysis results obtained are shown in Table 2;
TABLE 2 analysis of intermediate 1 composition (wt%)
| Oxide compound | SiO 2 | B 2 O 3 | Na 2 O | Li 2 O | Al 2 O 3 | CaO | TiO 2 | MgO | Fe 2 O 3 |
| Analysis result 1 | 54.72 | 16.51 | 13.75 | 1.86 | 4.62 | 3.64 | 0.70 | 0.93 | 3.24 |
| Difference value | -0.38 | 0.30 | 0.25 | 0.00 | 0.02 | -0.08 | -0.15 | -0.02 | 0.03 |
As can be seen from Table 2, wherein SiO 2 、B 2 O 3 、Na 2 O、TiO 2 The absolute value of the difference is greater than 50% of the set error, so the residual components are adjusted according to the difference, and the residual components are fine-tuned to obtain a redetermined formula, as shown in table 3;
table 3 redefined glass formulation (wt%)
| Oxide compound | SiO 2 | B 2 O 3 | Na 2 O | Li 2 O | Al 2 O 3 | CaO | TiO 2 | MgO | Fe 2 O 3 | Totalizing |
| Design composition | 55.48 | 15.91 | 13.25 | 1.86 | 4.60 | 3.74 | 1.00 | 0.95 | 3.21 | 100 |
Mixing the raw materials according to the redetermined formula, and then carrying out high-temperature melting at 1350 ℃ to obtain an intermediate product 2, wherein the grain diameter of the intermediate product is smaller than 75 mu m;
component analysis was performed on intermediate 2:
0.2g of intermediate 12 and 2g of lithium tetraborate are mixed uniformly and melted at 1100 ℃ for 20min to form glass sheets, and the SiO in the glass sheets is subjected to XRF 2 、Na 2 O、Al 2 O 3 、CaO、TiO 2 MgO and Fe 2 O 3 Quantitative analysis is carried out;
mixing 0.2g of intermediate 12 and 3g of potassium hydroxide, melting at 600 ℃ for 10min, extracting with hydrochloric acid solution, and determining the volume to 250mL, and measuring the B in the sample by ICP-AES 2 O 3 And Li (lithium) 2 O content, total analysis time 1h; the analysis results obtained are shown in Table 4:
TABLE 4 analysis of intermediate 2 composition (wt%)
| Oxide compound | SiO 2 | B 2 O 3 | Na 2 O | Li 2 O | Al 2 O 3 | CaO | TiO 2 | MgO | Fe 2 O 3 |
| Analysis result 2 | 55.00 | 16.19 | 13.40 | 1.85 | 4.61 | 3.69 | 0.82 | 0.93 | 3.19 |
| Difference value | -0.10 | -0.02 | -0.10 | -0.01 | 0.01 | -0.03 | -0.03 | -0.02 | -0.02 |
As can be seen from Table 4, the absolute value of the difference of the contents of each component is less than 50% of the setting error, and the glass with high consistency of the components is obtained;
the glass beads are prepared by taking the obtained glass as a raw material and sequentially carrying out high-temperature melting, mould pressing, crushing, fire polishing and screening, and the obtained glass beads can better realize the solidification of high-level waste liquid.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (9)
1. The preparation method of the glass with high consistency of the components for curing the high radioactive waste liquid is characterized by comprising the following steps:
(1) Determining the recipe and allowable setting errors of the glass;
(2) According to the formula of the glass, mixing raw materials, and then carrying out high-temperature melting to obtain an intermediate product;
(3) Carrying out component analysis on the intermediate product to obtain the content of each component;
(4) Comparing the obtained component contents with the corresponding component contents in the glass formula to obtain a difference value; if the absolute value of the difference is greater than or equal to 50% of the set error, subtracting the difference from the corresponding component content in the glass formulation, and re-determining the formulation of the glass;
(5) Repeating the steps (2) - (4) until the absolute value of the difference value of all the component contents is less than 50% of the set error, and obtaining the glass with high consistency of the components for curing the high-level waste liquid.
2. The method according to claim 1, wherein the absolute value of the setting error is 20 to 75%.
3. The method according to claim 1, wherein the high-temperature melting temperature is 1300 to 1520 ℃.
4. The method of claim 1, wherein the process of component analysis comprises:
mixing the intermediate product with lithium tetraborate for the first time, and carrying out first melting to obtain a first sample to be tested; analyzing the first sample to be detected by using an X-ray fluorescence spectrometry to obtain the content of oxide corresponding to the element with the atomic number less than or equal to 11;
secondly mixing the intermediate product with potassium hydroxide, carrying out second melting, and extracting the obtained melt by using hydrochloric acid solution to obtain a second sample to be detected; and analyzing the second sample to be tested by utilizing an ICP-AES method to obtain the content of the oxide corresponding to the element with the atomic number more than 11.
5. The preparation method according to claim 4, wherein the mass ratio of the intermediate product to lithium tetraborate is 1:9.8 to 10.2; the temperature of the first melting is 1090-1110 ℃, and the heat preservation time is 19-21 min.
6. The preparation method according to claim 4, wherein the mass ratio of the intermediate product to potassium hydroxide is 1:15; the temperature of the second melting is 600 ℃, and the heat preservation time is 10min.
7. The glass for curing a high-level waste liquid produced by the production method according to any one of claims 1 to 6, which has high consistency of components.
8. A glass bead prepared from the glass with high consistency of the components for curing the high-level waste liquid according to claim 7.
9. The method for preparing glass beads according to claim 8, comprising the steps of: the glass beads are obtained by sequentially melting, molding, crushing, fire polishing and sieving the glass with high consistency of the components for curing the high-level waste liquid according to claim 7.
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