CN109273130B - Preparation method of high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body - Google Patents
Preparation method of high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body, which is characterized by comprising the following steps of: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution of SO4 2‒And Ba2+The molar ratio of the heavy metal ions to the heavy metal ions is 1: 1-1.5, so as to obtain high-sulfur high-sodium high-level radioactive waste liquid containing barite; taking raw material SiO2、B2O3、Na2O、CaO、Al2O3、MgO、TiO2And high-sulfur high-sodium high-level radioactive waste liquid containing barite; the raw materials are mixed and then placed in a furnace to be calcined for 1-2 hours at the temperature of 800-850 ℃, then are melted for 2-3 hours at the temperature of 1000-1150 ℃, and then are annealed for 1-2 hours at the temperature of 450-500 ℃ and then are naturally cooled to room temperature, so that the high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body is prepared. The invention has low melting temperature, and the prepared glass ceramic solidified body has high content of high-sulfur high-sodium high-emission waste liquid, good chemical stability and strong practicability.
Description
Technical Field
The invention belongs to the treatment and disposal of radioactive wastes, and relates to a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body. The invention is particularly suitable for the solidification treatment of high-level radioactive waste liquid with high contents of sulfur and sodium.
Background
The high-level radioactive waste liquid (high-level radioactive waste liquid for short) mainly comes from raffinate generated by uranium-plutonium co-decontamination circulation in a spent fuel (also called irradiated nuclear fuel, namely used nuclear fuel) post-treatment process accumulated in nuclear power generation, has the characteristics of complex chemical components, high radioactive level, high biological toxicity and the like, and the safe treatment and disposal of the high-level radioactive waste liquid become one of key factors influencing the sustainable development of nuclear energy. At present, high-level radioactive waste liquid left over in the history of China urgently needs to be properly disposed, and in the future, the spent fuel accumulated in nuclear power generation generates more and more high-level radioactive waste liquid in the post-treatment process and also needs to be safely treated. Glass curing is the only treatment method of high-level radioactive liquid waste which is applied internationally at present. Borosilicate glass is a preferred glass curing material for curing high-level radioactive waste liquid in many countries including China due to good radiation resistance, chemical stability, water resistance and the like.
High-level radioactive waste liquid with high contents of sulfur and sodium, i.e. high-sulfur high-sodium high-level radioactive waste liquid, such as: SO in high level radioactive waste liquid in China3The content of Na is 4.6 percent (mass percentage content, the same is applied later)2The O content reaches 45.4% (Liulijun et al, nuclear and radiochemistry, 2014, vol 36, P163-168). Due to the low solubility of sulfate in borosilicate glass (SO)3Less than or equal to 1 percent) and the problem of 'yellow phase' which is generated during the glass melting process and separated from yellow second phase (the main component is Na) in many countries when borosilicate glass is used for curing high-sulfur high-sodium high-radioactive waste liquid2SO4). Yellow phase is easy to adsorb90Sr、137Cs and other nuclides are easily dissolved in water, so that the leaching resistance of the glass solidified body is remarkably reduced. Therefore, the generation of a yellow phase during the glass curing process must be avoided.
China requires that the package capacity of waste oxides (waste oxides, namely oxides obtained by concentrating and calcining high-sulfur high-sodium high-emission waste liquid) of a glass solidified body is 16 +/-3%, and when the package capacity reaches the upper limit (19%), sulfur in the glass solidified body is close to the solubility of the glass solidified body, and a yellow phase is likely to be generated in the actual production process. In the prior art, aiming at the problem of 'yellow phase' at home and abroad, sulfate is mainly decomposed into gas (SO) by adding reducing agents such as carbon powder, cane sugar and the like2) Volatilization, but increases the burden of tail gas treatment and secondary waste liquid treatment, and nitrate in the waste liquid can be reduced and decomposed; by increasing the melting temperature and prolonging the melting time, SO can be increased2But the volatilization amount can shorten the service life of the furnace, increase the volatilization amount of volatile radioactive elements (such as Ru) and reduce the production capacity of the furnace; avoiding the generation of yellow phases at the expense of reducing the packet capacity, both in terms of improving the capacity reduction ratio and reducing the costIs not advisable; the sulfate-containing capacity of the glass can be improved to a certain extent by optimizing the formula of the borosilicate base glass or adopting measures such as bubbling, mechanical stirring and the like, but the improvement capacity is limited. The problem of 'yellow phase' is a difficult problem in treating high-sulfur high-sodium high-level radioactive waste liquid in many countries, and no good method for eliminating the yellow phase exists at present.
Because the sulfur in the high-level radioactive waste liquid is sulfate radical ion (SO)4 2-) The sulfur element exists in a form of Na in the glass solidification research aiming at sulfur-containing high-level radioactive waste liquid at home and abroad at present2SO4And introducing the mixture in a form. Although Na is present2SO4The crystal itself has a high decomposition temperature (1200 ℃ C.), but Na2SO4With SiO2When the Na exists at the same time, the temperature (850 ℃) for the decomposition reaction is obviously reduced2SO4After melting, it will decompose rapidly. Liulijun et al (Liulijun et al, atomic energy science and technology, 2015, volume 49, P1551-1556) by analyzing the sulfur content in borosilicate glass, yellow phase and tail gas at different temperatures, found that the sulfate starts to decompose at 800 ℃, at 900-1150 ℃, it was observed that more yellow phase is gathered on the surface of the glass melt, but the yellow phase disappeared after 2h of heat preservation at 1150 ℃, and finally the sulfur contained in the glass body was only about half of the total amount initially added. Therefore, part of the sulfur inevitably volatilizes during the glass melting process, resulting in a lower content of sulfur fixed in the glass body.
The more yellow phase in the smelting furnace is accumulated because the tail gas absorption liquid returns to the feed tank regularly during the operation of the engineering scale. Therefore, how to effectively inhibit the decomposition of sulfate at high temperature and fix sulfur in a solidified body to the maximum is a technical difficulty encountered when borosilicate glass is used for solidifying high-sulfur high-sodium high-emission waste liquid.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body. Thereby providing an effective way for solving the problem of 'yellow phase' of borosilicate glass solidified high-sulfur high-sodium high-emission waste liquid.
The invention adds a proper amount of Ba (NO) into the high-sulfur high-sodium high-level radioactive waste liquid3)2Solution, chemical precipitation to form barite (BaSO)4) Precipitating (i.e. fixing sulfur in high-sulfur high-sodium high-radioactivity waste liquid in barite crystals with excellent thermal stability and chemical stability), and preparing borosilicate glass ceramic solidified body containing barite phase by adopting melting method widely applied in industry to solve Na problem2SO4Easily decomposed and volatilized at high temperature and low sulfur content in the glass solidified body. In practical application, a material delivery pipe can be designed between the material supply tank and the melting furnace for delivering a proper amount of Ba (NO)3)2The solution is added into the high-level radioactive waste liquid, and because the high-sulfur high-sodium high-level radioactive waste liquid has a certain flow velocity, a small amount of precipitate can not be attached to the wall of the conveying pipeline, and the normal operation of equipment can be ensured.
The content of the invention is as follows: a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body is characterized by comprising the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution of SO in high-sulfur high-sodium high-level radioactive waste liquid4 2-And Ba2+The molar ratio of the heavy metal ions to the heavy metal ions is 1: 1-1.5, namely the prepared high-sulfur high-sodium high-level radioactive waste liquid containing barite;
b. preparing materials: according to SiO2 36.0～54.0％，B2O3 13.5～20.0％，Na2O 3.0～4.5％，CaO 3.3～5.0％，Al2O3 2.2～3.5％，MgO 1.0～1.5％，TiO21.0-1.5 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid and 10-40 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid in terms of waste oxides;
the waste oxide is an oxide obtained by concentrating and calcining high-sulfur high-sodium high-level radioactive waste liquid;
c. mixing and reacting: mixing the raw materials of each component, placing the mixture in a furnace (such as a muffle furnace or a glass furnace) for heat preservation and calcination for 1-2 h at the calcination temperature of 800-850 ℃ (so as to decompose carbonate); then melting for 2-3 h at the melting temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 1-2 h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body (or called a borosilicate glass ceramic solidified body containing barite phase).
The invention comprises the following steps: in the high-sulfur high-sodium high-level radioactive waste liquid containing barite in step b, the main chemical composition and mass percentage content of the waste oxide can be as follows: SO (SO)34.623％，Na2O 45.405％，CeO2 0.346％，Cr2O3 2.023％，Cs2O 0.092％，K2O 0.606％，La2O3 11.625％，Fe2O321.460％，Al2O3 8.767％，BaO 0.129％，MoO3 0.777％，Nd2O3 0.693％，NiO 2.556％，P2O50.444％，SrO 0.047％，TiO20.316%, and Y2O30.091%, wherein SO3With barite (BaSO)4) The form exists.
The invention comprises the following steps: said component B in step B2O3、Na2H can be used for O, CaO and MgO3BO3、Na2CO3、CaCO3、MgCO3Is used as a raw material.
The invention comprises the following steps: said component SO3、Na2O、CeO2、Cr2O3、Cs2O、K2O、La2O3、Fe2O3、Al2O3、BaO、MoO3、Nd2O3、NiO、P2O5、SrO、TiO2、Y2O3BaSO can be respectively adopted correspondingly4、NaNO3、Ce(NO3)3·6H2O、Cr(NO3)3·9H2O、CsNO3、KNO3、La(NO3)3·6H2O、Fe(NO3)3·9H2O、Al(NO3)3·9H2O、Ba(NO3)2、Na2MoO4·2H2O、Nd2O3、Ni(NO3)2、Na3PO4、Sr(NO3)2、TiO2、Y(NO3)3·6H2O is taken as a raw material; when in use, the raw materials of each component are taken and dissolved by nitric acid, and the simulated high-sulfur high-sodium high-level radioactive waste liquid is obtained.
The invention comprises the following steps: the furnace in step c may be a muffle furnace or a glass furnace or the like.
The invention comprises the following steps: in the step c, different specific calcining temperature, melting temperature and annealing temperature can be selected according to the result of differential thermal analysis (DTA for short) when the composition is different.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) by adopting the invention, sulfate ions (SO) in the high-sulfur high-sodium high-radioactivity waste liquid4 2-) Is fixed on barite (BaSO) with excellent thermal stability and chemical stability4) The chemical reaction equation is as follows:
Na2SO4+Ba(NO3)2→BaSO4↓+2NaNO3；
then adopting a melting method to prepare a borosilicate glass ceramic solidified body containing a barite phase, thereby solving the problem of Na2SO4The problems of easy decomposition and volatilization at high temperature and low sulfur content in the glass solidified body;
(2) by adopting the method, the prepared borosilicate glass ceramic solidified body containing the barite phase, namely the high-sulfur high-sodium high-level radioactive waste liquid glass ceramic solidified body, has good chemical stability, does not have a yellow phase in the glass melting process when the packing capacity of waste oxides (namely the oxides of the high-sulfur high-sodium high-level radioactive waste liquid after concentration and calcination) reaches 20 percent, and has the normalized leaching rates of 10 after 28d of Na, B and Si elements-2、10-2And 10-3g·m2·d-1Are all lower than the requirement of 'characteristic identification of radioactive waste and waste package' of the national nuclear industry standard EJ 1186-2·d-1)；
(3) The simulated high-sulfur high-sodium high-level radioactive waste liquid is prepared according to the components of the real high-sulfur high-sodium high-level radioactive waste liquid, and elements with similar chemical properties are used for simulating radioactive elements, such as lanthanide neodymium (Nd), cerium (Ce) and lanthanum (La) for simulating actinides (such as U, Am, Eu and the like), so that the treatment method for simulating the high-sulfur high-sodium high-level radioactive waste liquid can be used for treating the real high-sulfur high-sodium high-level radioactive waste liquid;
(4) the invention tightly buckles the engineering application background, and the melting temperature is low; the prepared glass ceramic solidified body has high content of high-sulfur high-sodium high-radioactive waste liquid, good chemical stability, good treatment and disposal effects on radioactive waste and strong practicability.
Drawings
FIG. 1 is an X-ray diffraction (XRD for short) pattern of the precipitate of example 2;
FIG. 2 is an X-ray diffraction (XRD for short) pattern of the precipitate of example 3;
FIG. 3 is a graph showing the appearance of samples of the glass-ceramic solidified bodies of example 6 melted at different temperatures;
FIG. 4 is a graph showing the appearance of samples of the glass-ceramic solidified bodies of example 7 melted at different temperatures.
Detailed Description
The following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
Example 1:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 54.0％，B2O3 20.0％，Na2O 4.5％，CaO 5.0％，Al2O3 3.5％，MgO 1.5％，TiO21.5 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid, and taking the components according to the mass percentage of 10 percent of the components;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 850 deg.C for 1h (to decompose carbonate); then melting for 2h at 1150 ℃; then annealing at the annealing temperature of 500 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein no yellow phase appears in the glass melting process.
Example 2:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal and the catalyst is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained (XRD of the precipitate is shown as figure 1);
b. preparing materials: according to SiO2 52.8％，B2O3 19.6％，Na2O 4.4％，CaO 4.9％，Al2O3 3.4％，MgO 1.45％，TiO21.45 percent, and taking each component according to the composition and mass percentage of 12 percent of high-sulfur high-sodium high-level radioactive waste liquid containing barite calculated by waste oxides;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 850 deg.C for 1h (to decompose carbonate); then melting for 2h at 1150 ℃; then annealing at the annealing temperature of 500 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein no yellow phase appears in the glass melting process.
Example 3:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal and the barium nitrate is 1:1.4, and high-sulfur high-sodium high-level radioactive waste liquid containing the heavy spar and the barium nitrate is obtained (XRD of the precipitate is shown as an attached figure 2);
b. preparing materials: according to SiO2 51.6％，B2O3 19.1％，Na2O 4.3％，CaO 4.8％，Al2O3 3.36％，MgO 1.42％，TiO21.42 percent, and taking each component according to the composition and mass percentage of 14 percent of high-sulfur high-sodium high-level radioactive waste liquid containing barite calculated by waste oxides;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 850 deg.C for 1h (to decompose carbonate); then melting for 2h at 1120 ℃; then annealing at the annealing temperature of 490 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein no yellow phase appears in the glass melting process.
Example 4:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 50.4％，B2O3 18.6％，Na2O 4.2％，CaO 4.7％，Al2O3 3.3％，MgO 1.40％，TiO21.40 percent, and taking each component according to the composition and mass percentage of 16 percent of high-sulfur high-sodium high-level radioactive waste liquid containing barite calculated by waste oxides;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 850 deg.C for 1h (to decompose carbonate); melting for 2h at 1100 ℃; then annealing at the annealing temperature of 480 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein no yellow phase appears in the glass melting process.
Example 5:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: preparing materials: according to SiO2 49.2％，B2O3 18.3％，Na2O 4.1％，CaO 4.52％，Al2O33.18％，MgO 1.35％，TiO21.35 percent, and taking each component according to the component composition and mass percentage of 18 percent of high-sulfur high-sodium high-level radioactive waste liquid containing barite calculated by waste oxides;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 850 deg.C for 1h (to decompose carbonate); melting for 2h at 1100 ℃; then annealing at the annealing temperature of 480 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein no yellow phase appears in the glass melting process.
Example 6:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 48.0％，B2O3 17.8％，Na2O 4.0％，CaO 4.45％，Al2O3 3.11％，MgO 1.32％，TiO21.32 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid, and taking the components with the mass percent of 20 percent of the components;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 850 deg.C for 1h (to decompose carbonate); melting for 2h at 1100 ℃; then annealing at the annealing temperature of 480 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein no yellow phase appears in the glass melting process, as shown in figure 3.
Example 7:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 45.0％，B2O3 16.7％，Na2O 3.75％，CaO 4.15％，Al2O3 2.90％，MgO 1.25％，TiO21.25 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid, and taking the components according to the mass percent, wherein the components are calculated by waste oxides and 25 percent;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 850 deg.C for 1h (to decompose carbonate); melting for 2h at 1100 ℃; then annealing at the annealing temperature of 470 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein a yellow phase appears in the glass melting process, as shown in figure 4.
Example 8:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 42.0％，B2O3 15.6％，Na2O 3.50％，CaO 3.86％，Al2O3 2.72％，MgO 1.16％，TiO21.16 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid, and taking the components according to the mass percentage, wherein the components are calculated by waste oxides and 30 percent;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 800 deg.C for 1h (to decompose carbonate); melting at 1050 ℃ for 2 h; then annealing at the annealing temperature of 460 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein a yellow phase appears in the glass melting process, and the finally obtained glass solidified body also has a yellow phase.
Example 9:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 39.0％，B2O3 14.5％，Na2O 3.22％，CaO 3.60％，Al2O3 2.52％，MgO 1.08％，TiO21.08 percent, and taking each component according to the mass percentage, wherein the components are calculated by waste oxides and comprise 35 percent of high-sulfur high-sodium high-level radioactive waste liquid containing barite;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 800 deg.C for 1h (to decompose carbonate); then melting for 2h at 1020 ℃; then annealing at the annealing temperature of 450 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein a yellow phase appears in the glass melting process, and the finally obtained glass solidified body also has a yellow phase.
Example 10:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 36.0％，B2O3 13.5％，Na2O 3.0％，CaO 3.3％，Al2O3 2.2％，MgO 1.0％，TiO21.0 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid, and taking the components according to the mass percentage of the components, wherein the components are calculated by waste oxides and 40 percent;
c. mixing and reacting: mixing the raw materials, placing in a furnace (such as a muffle furnace or a glass furnace) for calcining at 800 deg.C for 1h (to decompose carbonate); then melting for 2 hours at the temperature of 1000 ℃; then annealing at the annealing temperature of 450 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body, wherein a yellow phase appears in the glass melting process, and the finally obtained glass solidified body also has a yellow phase.
Examples 11 to 17:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: according to SiO2 36.0～54.0％，B2O3 13.5～20.0％，Na2O 3.0～4.5％，CaO 3.3～5.0％，Al2O3 2.2～3.5％，MgO 1.0～1.5％，TiO21.0-1.5 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid, and taking the components according to the mass percentage, wherein the components are calculated by waste oxides and 10-40 percent of the high-sulfur high-sodium high-level radioactive waste liquid; the specific mass percentage of each component is as follows:
c. mixing and reacting: mixing the raw materials, placing the mixture in a furnace (such as a muffle furnace or a glass furnace) and calcining the mixture for 1h at the temperature of 800-850 ℃ (so as to decompose carbonate); then melting for 2 hours at the temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body.
Example 18:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.2, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: the specific mass percentage usage of each component is the same as that in any one of embodiments 11-17, and is omitted;
c. mixing and reacting: mixing and grinding the raw materials, and then placing the mixture into a furnace to be calcined for 2 hours at the temperature of 800-850 ℃ (so as to decompose carbonate); then melting for 3 hours at the temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 2h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body.
Example 19:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.4, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: the specific mass percentage usage of each component is the same as that in any one of embodiments 11-17, and is omitted;
c. mixing and reacting: mixing and grinding the raw materials, and then placing the mixture into a furnace to be calcined for 1.5h at the temperature of 800-850 ℃ (so as to decompose carbonate); then melting for 2.5h at the temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 1.5h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body.
Example 20:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the heavy metal is 1:1.1, and high-sulfur high-sodium high-level radioactive waste liquid containing barite is obtained;
b. preparing materials: the specific mass percentage usage of each component is the same as that in any one of embodiments 11-17, and is omitted;
c. mixing and reacting: mixing and grinding the raw materials, and then placing the mixture into a furnace to be calcined for 1h at the temperature of 800-850 ℃ (so as to decompose carbonate); then melting for 2 hours at the temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body.
Example 21:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a, preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the barium nitrate is 1:1.3, and high-sulfur high-sodium high-level radioactive waste liquid containing the barite and the barium nitrate is obtained;
b. preparing materials: the specific mass percentage usage of each component is the same as that in any one of embodiments 11-17, and is omitted;
c. mixing and reacting: mixing and grinding the raw materials, and then placing the mixture into a furnace to be calcined for 1h at the temperature of 800-850 ℃ (so as to decompose carbonate); then melting for 2 hours at the temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body.
Example 22:
a preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body comprises the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution, control of SO4 2-And Ba2+The molar ratio of the heavy metal to the barium nitrate is 1:1.5, and high-sulfur high-sodium high-level radioactive waste liquid containing the barite and the barium nitrate is obtained;
b. preparing materials: the specific mass percentage usage of each component is the same as that in any one of embodiments 11-17, and is omitted;
c. mixing and reacting: mixing and grinding the raw materials, and then placing the mixture into a furnace to be calcined for 1h at the temperature of 800-850 ℃ (so as to decompose carbonate); then melting for 2 hours at the temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 1h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body.
In the above embodiment:
in the high-sulfur high-sodium high-level radioactive waste liquid containing barite in step b, the main chemical composition and mass percentage content of the waste oxide can be as follows: SO (SO)3 4.623％，Na2O45.405％，CeO2 0.346％，Cr2O32.023％，Cs2O 0.092％，K2O 0.606％，La2O3 11.625％，Fe2O3 21.460％，Al2O3 8.767％，BaO 0.129％，MoO3 0.777％，Nd2O3 0.693％，NiO2.556％，P2O5 0.444％，SrO 0.047％，TiO20.316%, and Y2O30.091%, wherein SO3With barite (BaSO)4) The form exists;
said component B in step B2O3、Na2H can be used for O, CaO and MgO3BO3、Na2CO3、CaCO3、MgCO3Is taken as a raw material;
said component SO in step b3、Na2O、CeO2、Cr2O3、Cs2O、K2O、La2O3、Fe2O3、Al2O3、BaO、MoO3、Nd2O3、NiO、P2O5、SrO、TiO2、Y2O3BaSO can be respectively adopted correspondingly4、NaNO3、Ce(NO3)3·6H2O、Cr(NO3)3·9H2O、CsNO3、KNO3、La(NO3)3·6H2O、Fe(NO3)3·9H2O、Al(NO3)3·9H2O、Ba(NO3)2、Na2MoO4·2H2O、Nd2O3、Ni(NO3)2、Na3PO4、Sr(NO3)2、TiO2、Y(NO3)3·6H2O is taken as a raw material; when in use, the raw materials of each component are taken and dissolved by nitric acid, and the simulated high-sulfur high-sodium high-level radioactive waste liquid is obtained.
In the above embodiments 11 to 22: in the step c, different specific calcining temperature, melting temperature and annealing temperature can be selected according to the result of differential thermal analysis (DTA for short) when the composition is different.
In the above embodiment: all the raw materials are commercially available products.
In the above embodiment: the percentages used, not specifically indicated, are percentages by weight or known to those skilled in the art; the parts by mass (by weight) may all be grams or kilograms.
In the above embodiment: the process parameters (temperature, time, etc.) and the numerical values of the components in each step are in the range, and any point can be applicable.
The present invention and the technical contents not specifically described in the above embodiments are the same as the prior art.
The present invention is not limited to the above-described embodiments, and the present invention can be implemented with the above-described advantageous effects.
Claims (4)
1. A preparation method of a high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body is characterized by comprising the following steps:
a. preparing high-sulfur high-sodium high-radioactivity waste liquid containing barite: adding Ba (NO) into high-sulfur high-sodium high-level waste liquid3)2Solution of SO in high-sulfur high-sodium high-level radioactive waste liquid4 2-And Ba2+The molar ratio of the heavy metal ions to the heavy metal ions is 1: 1-1.5, namely the prepared high-sulfur high-sodium high-level radioactive waste liquid containing barite;
b. preparing materials: according to SiO2 36.0～54.0%，B2O3 13.5～20.0%，Na2O 3.0～4.5%，CaO 3.3～5.0%，Al2O3 2.2～3.5%，MgO 1.0～1.5%，TiO21.0-1.5 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid and 10-40 percent of barite-containing high-sulfur high-sodium high-level radioactive waste liquid in terms of waste oxides;
in the high-sulfur high-sodium high-level radioactive waste liquid containing barite calculated by waste oxides, the main chemical compositions and mass percentage contents of the waste oxides are as follows: SO (SO)3 4.623%，Na2O 45.405%，CeO2 0.346%，Cr2O3 2.023%，Cs2O 0.092%，K2O 0.606%，La2O3 11.625%，Fe2O3 21.460%，Al2O3 8.767%，BaO 0.129%，MoO30.777%，Nd2O3 0.693%，NiO 2.556%，P2O5 0.444%，SrO 0.047%，TiO20.316%, and Y2O30.091%；
c. Mixing and reacting: mixing the raw materials of each component, and then placing the mixture into a furnace to perform heat preservation and calcination for 1-2 hours at the calcination temperature of 800-850 ℃; then melting for 2-3 h at the melting temperature of 1000-1150 ℃; then annealing at the annealing temperature of 450-500 ℃ for 1-2 h, and naturally cooling to room temperature to obtain the high-sulfur high-sodium high-radioactivity waste liquid glass ceramic solidified body.
2. According to claimThe preparation method of the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body is characterized by comprising the following steps of: said component B in step B2O3、Na2H is adopted for O, CaO and MgO respectively3BO3、Na2CO3、CaCO3、MgCO3Is used as a raw material.
3. The method for preparing the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body according to claim 1, which is characterized by comprising the following steps of: said component SO3、Na2O、CeO2、Cr2O3 、Cs2O、K2O、La2O3、Fe2O3、Al2O3、BaO、MoO3、Nd2O3、NiO、P2O5、SrO、TiO2、Y2O3Respectively correspondingly adopts BaSO4、NaNO3、Ce(NO3)3·6H2O、Cr(NO3)3·9H2O、CsNO3、KNO3、La(NO3)3 ·6H2O、Fe(NO3)3·9H2O、Al(NO3)3·9H2O、Ba(NO3)2、Na2MoO4·2H2O、Nd2O3、Ni(NO3)2、Na3PO4、Sr(NO3)2、TiO2、Y(NO3)3·6H2O is taken as a raw material.
4. The method for preparing the high-sulfur high-sodium high-emission waste liquid glass ceramic solidified body according to claim 1, which is characterized by comprising the following steps of: the furnace in step c is a muffle furnace or a glass furnace.
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