CN109036612B - TiO with anatase structure2Method for treating technetium-containing waste liquid - Google Patents

TiO with anatase structure2Method for treating technetium-containing waste liquid Download PDF

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CN109036612B
CN109036612B CN201810758857.8A CN201810758857A CN109036612B CN 109036612 B CN109036612 B CN 109036612B CN 201810758857 A CN201810758857 A CN 201810758857A CN 109036612 B CN109036612 B CN 109036612B
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technetium
tio
waste liquid
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CN109036612A (en
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张武
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Shandong Xinrongde New Materials Co ltd
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Shenyang Ligong University
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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
    • G21F9/04—Treating liquids
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Abstract

一种利用锐钛矿结构TiO2处理含锝废液的方法，属于核废物处理领域；方法：1)稀释含锝废液；2)将钛粉与氟化铵混合均匀；3)将混合粉末加入含锝溶液中，加热至沸腾；4)将得到的固液混合物离心，获得Tc掺杂锐钛矿结构和无色液体；发明中的方案充分利用了钛粉氧化过程中锐钛矿相TiO2结构的形成过程，在其形成过程中可以使大量TC组分进入其结构，从而大大提高固化效果，固定率高达99.99％以上，而且工艺过程温度低，只需将含锝溶液加热至沸腾，无需加热至高温，有效避免了高温过程中锝组分的挥发。A method for treating waste liquid containing technetium by utilizing anatase structure TiO 2 belongs to the field of nuclear waste treatment; the method: 1) dilute the waste liquid containing technetium; 2) mix titanium powder and ammonium fluoride uniformly; Add the technetium-containing solution and heat it to boiling; 4) Centrifuge the obtained solid-liquid mixture to obtain a Tc-doped anatase structure and a colorless liquid; the solution in the invention makes full use of anatase-phase TiO in the oxidation process of titanium powder 2 The formation process of the structure, in the process of its formation, a large amount of TC components can be entered into its structure, thereby greatly improving the curing effect, the fixation rate is as high as 99.99%, and the process temperature is low, only need to heat the technetium-containing solution to boiling. , without heating to high temperature, effectively avoiding the volatilization of technetium components in the high temperature process.

Description

TiO with anatase structure2Method for treating technetium-containing waste liquid
Technical Field
The invention belongs to the field of nuclear waste treatment, and particularly relates to a method for treating nuclear waste by utilizing TiO with an anatase structure2A method for treating technetium-containing waste liquid.
Background
Technetium-99 (Tc) is a common nuclear fission product due to its long half-life (2.1X 10)5Year), high cracking rate (6%), high environmental mobility, and complicated long-term disposal of nuclear waste. At present, it is widely believed that "separation-solidification-deep geological" disposal is a viable high-emissivity waste liquid treatment disposal scheme. The method separates radionuclides with long half-life period, high radioactivity level and high biotoxicity from the high-level radioactive liquid waste, classifies the radionuclides according to nuclide types and radioactivity levels, performs cement curing on the large-volume low-level radioactive waste obtained after separation, and can perform glass curing or artificial rock curing on the small-volume high-level radioactive waste, so that the treatment burden is greatly reduced, and the treatment safety is improved. According to the "separation-solidification-deep geological disposal" protocol described above, technetium-containing waste is usually fixed in the form of borosilicate glass, but some of the volatile technetium-containing material is lost during vitrification, thereby greatly reducing the effectiveness of the protocol.
Disclosure of Invention
TiO with anatase structure2The method for treating the technetium-containing waste liquid comprises the following steps in sequence:
(1) diluting the technetium-containing waste liquid into a technetium-containing solution with the concentration of 1.8-2.3 mu g/mL by using deionized water;
(2) uniformly mixing titanium powder and ammonium fluoride to obtain mixed powder;
(3) adding the mixed powder into the technetium-containing solution according to the liquid-solid ratio (15-20) to 1 of the technetium-containing solution to the mixed powder, and heating the mixed powder to boiling from room temperature to obtain a solid-liquid mixture;
(4) centrifuging the solid-liquid mixture to obtain Tc-doped anatase structure TiO2And a colorless liquid.
The method for treating the technetium-containing waste liquid by using the anatase structure comprises the following steps:
in the step 2, the mass percentage of the metal titanium in the titanium powder is not less than 99.8%, and the granularity is 300-325 meshes; the ammonium fluoride is powdery, the purity is more than 99.5 percent (mass percentage content), and the granularity is 200-300 meshes.
In the step 2, the mass ratio of the titanium powder to the ammonium fluoride is (1-1.2) to 1.
In the step 2, mixing materials in a glass container provided with a reflux device.
In the step 3, the liquid-solid ratio refers to the ratio of the volume (unit: ml) of the solution to the mass (unit: g) of the mixture.
In the step 3, the technetium-containing solution and the mixed powder are heated to boiling (100 ℃) for 10-16 hours.
In the step 4, Tc is doped with Ti0 with anatase structure2As a brown-grey powder.
The prepared Tc-doped anatase-structure TiO2Leaching with water, and testing the Tc concentration in the leachate to be less than or equal to 0.0028% after 30-210 days.
TiO with anatase structure2The method for treating the technetium-containing waste liquid has the main design idea of the technical scheme that:
in the invention, the base is based on TCO2And anatase phase TiO2High similarity of structure, preparing technetium doped anatase phase TiO by direct oxidation of titanium powder2The structure of the anatase structure is such that technetium in the waste is permanently fixed to the anatase structure, thereby eliminating the risk of technetium-containing waste.
TiO with anatase structure2Compared with the prior art, the method for treating the technetium-containing waste liquid has the beneficial effects that:
(1) the temperature of the process is low, only the technetium-containing solution is required to be heated to boiling, and the technetium-containing solution is not required to be heated to high temperature (the existing process usually needs more than 600 ℃), so that the volatilization of technetium components in the high-temperature process is effectively avoided.
(2) The process is simple and efficient, and the technetium has a fixing rate of over 99.99 percent through the steps.
(3) The scheme of the invention makes full use of anatase phase TiO in the titanium powder oxidation process2Formation of structures during which a large number of T's can be madeCThe components enter the structure of the curing agent, thereby greatly improving the curing effect.
Drawings
FIG. 1 Tc-doped anatase TiO obtained according to example 1 of the invention2X-ray diffraction pattern of the powder.
FIG. 2 Tc-doped anatase TiO obtained in example 4 of the invention2Time-dependent curve of Tc extraction from the powder.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1
TiO with anatase structure2The method for treating the technetium-containing waste liquid comprises the following steps in sequence:
(1) diluting the technetium-containing waste liquid into a technetium-containing solution with the concentration of 1.8 mu g/mL by using deionized water;
(2) uniformly mixing 24g of titanium powder with the purity of 99.9 percent and the granularity of 300 meshes with 24g of ammonium fluoride with the purity of 99.6 percent and the granularity of 200 meshes according to the mass ratio of the titanium powder to the ammonium fluoride of 1: 1 to obtain mixed powder;
(3) adding the mixed powder into the technetium-containing solution according to the liquid-solid ratio of the technetium-containing solution to the mixed powder of 15: 1, and heating to boil for 10 hours at room temperature to obtain a solid-liquid mixture;
(4) centrifuging the solid-liquid mixture to obtain TiO with brown-gray Tc doped anatase structure2Powder and colorless liquid.
The supernatant colorless liquid was taken to assay for the concentration of Tc, and the presence of Tc in the supernatant was not detected, indicating that Tc was successfully doped into the anatase powder. Taking dried Tc doped TiO2For powdersAnd (3) leaching with water, wherein the Tc concentration in the test leaching solution is 0.001% after 30 days, which shows that the fixation effect is good.
Tc-doped anatase TiO prepared in this example2The X-ray diffraction pattern of the powder is shown in FIG. 1.
Example 2
TiO with anatase structure2The method for treating the technetium-containing waste liquid comprises the following steps in sequence:
(1) diluting the technetium-containing waste liquid into a technetium-containing solution with the concentration of 2.0 mu g/mL by using deionized water;
(2) uniformly mixing 24g of titanium powder with the purity of 99.9 percent and the granularity of 300 meshes with 20g of ammonium fluoride with the purity of 99.6 percent and the granularity of 200 meshes according to the mass ratio of the titanium powder to the ammonium fluoride of 1.2: 1 to obtain mixed powder;
(3) adding the mixed powder into the technetium-containing solution according to the liquid-solid ratio of the technetium-containing solution to the mixed powder of 15: 1, and heating to boil for 12 hours at room temperature to obtain a solid-liquid mixture;
(4) centrifuging the solid-liquid mixture to obtain TiO with brown-gray Tc doped anatase structure2Powder and colorless liquid.
The supernatant was taken as a colorless liquid and assayed for Tc concentration and the presence of Tc in the supernatant was not detected, indicating that Tc was successfully incorporated into the anatase powder. Taking dried Tc doped TiO2The powder was leached with water and after 60 days the Tc concentration in the leachate was assayed to be 0.002%, indicating a good fixing effect.
Example 3
TiO with anatase structure2The method for treating the technetium-containing waste liquid comprises the following steps in sequence:
(1) diluting the technetium-containing waste liquid into a technetium-containing solution with the concentration of 2.3 mu g/mL by using deionized water;
(2) uniformly mixing 24g of titanium powder with the purity of 99.9 percent and the granularity of 325 meshes with 20g of ammonium fluoride with the purity of 99.7 percent and the granularity of 200 meshes according to the mass ratio of the titanium powder to the ammonium fluoride of 1.2: 1 to obtain mixed powder;
(3) adding the mixed powder into the technetium-containing solution according to the liquid-solid ratio of the technetium-containing solution to the mixed powder of 20: 1, and heating to boil for 15h at room temperature to obtain a solid-liquid mixture;
(4) centrifuging the solid-liquid mixture to obtain TiO with brown-gray Tc doped anatase structure2Powder and colorless liquid.
The supernatant was taken as a colorless liquid and assayed for Tc concentration and the presence of Tc in the supernatant was not detected, indicating that Tc was successfully incorporated into the anatase powder. Taking dried Tc doped TiO2The powder was leached with water and after 90 days the Tc concentration in the leachate was assayed to 0.0025%, indicating good fixing.
Example 4
TiO with anatase structure2The method for treating the technetium-containing waste liquid comprises the following steps in sequence:
(1) diluting the technetium-containing waste liquid into a technetium-containing solution with the concentration of 2.3 mu g/mL by using deionized water;
(2) uniformly mixing 24g of titanium powder with the purity of 99.8 percent and the granularity of 325 meshes with 24g of ammonium fluoride with the purity of 99.7 percent and the granularity of 300 meshes according to the mass ratio of the titanium powder to the ammonium fluoride of 1: 1 to obtain mixed powder;
(3) adding the mixed powder into the technetium-containing solution according to the liquid-solid ratio of the technetium-containing solution to the mixed powder of 20: 1, and heating to boil for 16h at room temperature to obtain a solid-liquid mixture;
(4) centrifuging the solid-liquid mixture to obtain TiO with brown-gray Tc doped anatase structure2Powder and colorless liquid.
The supernatant was taken as a colorless liquid and assayed for Tc concentration and the presence of Tc in the supernatant was not detected, indicating that Tc was successfully incorporated into the anatase powder. Taking dried Tc doped TiO2The powder was leached with water, and after 210 days, the Tc concentration in the test leachate was 0.0023%, and the Tc leaching rate was shown as a time-dependent curve in fig. 2, indicating that the fixation effect was good.
Tc-doped anatase TiO prepared in this example2The time-dependent curve of the Tc extraction rate of the powder is shown in FIG. 2.
Example 5
Use ofAnatase structure TiO2The method for treating the technetium-containing waste liquid comprises the following steps in sequence:
(1) diluting the technetium-containing waste liquid into a technetium-containing solution with the concentration of 2.3 mu g/mL by using deionized water;
(2) uniformly mixing 22g of titanium powder with the purity of 99.9 percent and the granularity of 325 meshes with 20g of ammonium fluoride with the purity of 99.7 percent and the granularity of 300 meshes according to the mass ratio of the titanium powder to the ammonium fluoride of 1.1: 1 to obtain mixed powder;
(3) adding the mixed powder into the technetium-containing solution according to the liquid-solid ratio of the technetium-containing solution to the mixed powder of 18: 1, and heating to boil for 16h at room temperature to obtain a solid-liquid mixture;
(4) centrifuging the solid-liquid mixture to obtain TiO with brown-gray Tc doped anatase structure2Powder and colorless liquid.
The supernatant was taken as a colorless liquid and assayed for Tc concentration and the presence of Tc in the supernatant was not detected, indicating that Tc was successfully incorporated into the anatase powder. Taking the dried TiO2The powder was leached with water and the Tc concentration in the leachate was assayed at 210 days to 0.0028%, indicating good fixation.

Claims (4)

1.一种利用锐钛矿结构TiO2处理含锝废液的方法，其特征在于，实施过程依次按以下步骤进行：1. utilizes anatase structure TiO 2 the method for processing technetium-containing waste liquid, is characterized in that, implementation process is carried out successively according to the following steps: (1)使用去离子水将含锝废液稀释成浓度为1.8～2.3μg/mL的含锝溶液；(1) Use deionized water to dilute the technetium-containing waste liquid into a technetium-containing solution with a concentration of 1.8-2.3 μg/mL; (2)将钛粉与氟化铵以质量比(1～1.2)：1混合均匀，得到混合粉末；(2) uniformly mixing titanium powder and ammonium fluoride in a mass ratio (1-1.2): 1 to obtain mixed powder; (3)按照含锝溶液与混合粉末的液固比(15～20):1将混合粉末加入含锝溶液中，从室温加热至沸腾，获得固液混合物；(3) adding the mixed powder to the technetium-containing solution according to the liquid-solid ratio of the technetium-containing solution to the mixed powder (15-20): 1, and heating to boiling from room temperature to obtain a solid-liquid mixture; (4)将固液混合物离心，获得Tc掺杂锐钛矿结构的TiO2和无色液体。(4) Centrifuge the solid-liquid mixture to obtain Tc-doped anatase-structured TiO2 and a colorless liquid. 2.根据权利要求1所述的一种利用锐钛矿结构TiO2处理含锝废液的方法，其特征在于，所述步骤2中，钛粉中金属钛质量百分比不小于99.8％，粒度为300～325目；氟化铵为粉末状，纯度大于99.5％(质量百分含量)，粒度为200～300目。2. a kind of utilizing anatase structure TiO according to claim 1 the method for processing technetium-containing waste liquid, is characterized in that, in described step 2, in the titanium powder, the mass percentage of metallic titanium is not less than 99.8%, and the particle size is 300-325 mesh; ammonium fluoride is in powder form, the purity is more than 99.5% (mass percentage), and the particle size is 200-300 mesh. 3.根据权利要求1所述的一种利用锐钛矿结构TiO2处理含锝废液的方法，其特征在于，所述步骤3中，含锝溶液与混合粉末加热至沸腾，沸腾时间为10～16h。3. a kind of utilizing anatase structure TiO according to claim 1 The method for processing technetium-containing waste liquid is characterized in that, in described step 3, technetium-containing solution and mixed powder are heated to boiling, and the boiling time is 10 ~16h. 4.根据权利要求1所述的一种利用锐钛矿结构TiO2处理含锝废液的方法，其特征在于，通过所述方法制得的Tc掺杂锐钛矿结构的TiO2用水浸出，30～210日后化验浸出液中的Tc浓度≤0.0028％。4. a kind of utilizing anatase structure TiO according to claim 1 The method for processing technetium-containing waste liquid is characterized in that, the TiO of Tc-doped anatase structure obtained by the method is leached with water, After 30 to 210 days, the Tc concentration in the leaching solution should be ≤0.0028%.
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