CN113368809B - Preparation method of bismuth-based silicon dioxide material and application of bismuth-based silicon dioxide material in radioactive iodine trapping - Google Patents
Preparation method of bismuth-based silicon dioxide material and application of bismuth-based silicon dioxide material in radioactive iodine trapping Download PDFInfo
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- CN113368809B CN113368809B CN202110679798.7A CN202110679798A CN113368809B CN 113368809 B CN113368809 B CN 113368809B CN 202110679798 A CN202110679798 A CN 202110679798A CN 113368809 B CN113368809 B CN 113368809B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
Abstract
The invention discloses a preparation method of a bismuth-based silicon dioxide material and application thereof in trapping radioactive iodine, comprising the following steps: dissolving bismuth nitrate in a nitric acid solution to obtain a bismuth nitrate solution; adding nano SiO into bismuth nitrate solution2Stirring for 30-45 min to obtain a solution I; dissolving stannous chloride in a sodium hydroxide solution to obtain a solution II; mixing the solution I and the solution II, stirring for 5-10 min, washing, and filtering to obtain a solid; and sintering the solid obtained in the fourth step for 5.5-6.5 hours at 350-450 ℃ in an argon-hydrogen reduction protective atmosphere to obtain the bismuth-based silicon dioxide material. The bismuth-based silicon dioxide material can be simply and efficiently synthesized in a short time by adopting a simple dipping reduction method and taking bismuth nitrate as a bismuth source and stannous chloride as a reducing agent, and has high iodine adsorption capacity which is far higher than that of other similar materials.
Description
Technical Field
The invention relates to the field of material technology and radioactive waste treatment, in particular to a preparation method of a bismuth-based silicon dioxide material and application of the bismuth-based silicon dioxide material in radioactive iodine capture.
Background
Along with the rapid development of the nuclear energy industry in China, the safe treatment of radioactive wastes becomes the focus of increasing attention of people, and particularly, the leakage of the nuclear power station in Fudao of Japan causes the existence of a large amount of radioactive gas iodine and inorganic iodine in the environment of the surrounding area, namely radioactive iodine (A), (B), (C) and (C)129I) Is one of the main sources of radioactive waste hazard due to its long half-life (1.57X 10)7Years) poses a serious threat to humans, and adsorption removal treatment thereof is considered as one of good strategies. Therefore, removal of radioactive gaseous iodine from the environment is essential. At present, the adsorption material for radioactive gaseous iodine mainly comprises zeolite, activated carbon, COFS, MOFS and the like, has a large specific surface area and a microporous structure, has a strong adsorption effect on gaseous iodine, but is limited by factors such as complex preparation process, poor stability, low cyclic utilization rate, difficulty in post-treatment, high practical application cost and the like, so that an alternative adsorption material is urgently needed to be found.
Bismuth-containing composite materials are considered to be a good radioactive iodine (129I) An adsorbent material. The existing bismuth-based material often has the problems of difficult synthesis, high cost and the like, so a simple and efficient method for preparing the bismuth-based silicon dioxide (Bi-SiO) with low cost is developed2) The iodine trapping material is applied to trapping radioactive iodine steam, and has important significance.
Disclosure of Invention
The invention aims to provide a method for synthesizing bismuth-based silicon dioxide (Bi-SiO) with simplicity, high efficiency and low cost2) The iodine trapping material realizes efficient trapping of radioactive iodine. Aiming at the problems of complex operation, high cost, poor iodine adsorption capacity and the like of the existing synthesis method, the invention takes bismuth nitrate as a bismuth source, stannous chloride as a reducing agent and commercial nano-silica as a carrier,simple and efficient synthesis of bismuth-based silicon dioxide (Bi-SiO) by adopting impregnation method2) The material was iodine-capturing, and its adsorption performance for iodine was evaluated. The obtained material has the characteristics of low cost, large iodine adsorption amount and the like, and the method has the advantages of simplicity, high efficiency and the like.
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a bismuth-based silica material, comprising the steps of:
dissolving bismuth nitrate in a nitric acid solution to obtain a bismuth nitrate solution;
step two, adding nano SiO into bismuth nitrate solution2Stirring for 30-45 min to obtain a solution I;
dissolving stannous chloride in a sodium hydroxide solution to obtain a solution II;
step four, mixing the solution I and the solution II, stirring for 5-10 min, washing, and filtering to obtain a solid;
and fifthly, sintering the solid obtained in the fourth step for 5.5-6.5 hours at 350-450 ℃ in an argon-hydrogen reduction protective atmosphere to obtain the bismuth-based silicon dioxide material.
Preferably, the mass volume ratio of the bismuth nitrate to the nitric acid solution is 2-8 g:100 mL; the concentration of the nitric acid solution is 0.5-1.5 mol/L.
Preferably, the bismuth nitrate and the nano SiO2The mass ratio of (A) to (B) is 2-8: 1.5.
Preferably, the mass volume ratio of the stannous chloride to the sodium hydroxide solution is 1.5-5.5 g: 70-120 mL; the concentration of the sodium hydroxide solution is 1.5-2.5 mol/L.
Preferably, in the fourth step, while stirring, the mixed reaction solution of the solution I and the solution II is irradiated intermittently by using an infrared lamp.
Preferably, the power of the infrared lamp is 240-300W; the distance between the infrared lamp and the mixed reaction liquid is 5-10 cm; the intermittent irradiation is 1min, and the irradiation is stopped for 30s, so that the circulation is realized.
Preferably, in the fifth step, the bismuth-based silica material is reprocessed, and the process comprises: and (3) placing the bismuth-based silicon dioxide material in a low-temperature plasma treatment instrument, and introducing gas into the low-temperature plasma treatment instrument to form plasma to treat the bismuth-based silicon dioxide material for 1-3 min.
Preferably, the gas introduced into the low-temperature plasma treatment instrument is SF6And ethanol; the frequency of the low-temperature plasma treatment instrument is 10-30 KHz, the power is 30-60W, and the treatment temperature is 30-45 ℃; wherein ethanol is gasified and then mixed with SF6Mixing and introducing into a low-temperature plasma processor.
The invention also provides an application of the bismuth-based silicon dioxide material in trapping radioactive iodine.
The invention at least comprises the following beneficial effects: (1) the cost is low: the traditional similar Bi-based composite material usually takes mesoporous silica as a carrier, the price of the mesoporous silica is about 1500 yuan/kg, and the commercial common nano silica used in the invention has the price of about 75 yuan/kg. Therefore, the bismuth-based silicon dioxide (Bi-SiO) prepared by the invention2) The cost of the iodine trapping material can be reduced by one twentieth. (2) Large iodine adsorption: the bismuth-based silica material (Bi-SiO) of the present invention2) The iodine adsorption capacity of the material is high and is far higher than that of other similar materials. (3) The operation is simple and efficient: the bismuth-based silicon dioxide material can be synthesized simply and efficiently in a short time by adopting a simple dipping reduction method and taking bismuth nitrate as a bismuth source and stannous chloride as a reducing agent.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is an XRD pattern of the material prepared in example 3 of the present invention and nano-silica;
FIG. 2 is an XRD pattern of the material prepared in example 3 before and after adsorption of iodine.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Examples 1 to 3:
a preparation method of a bismuth-based silicon dioxide material comprises the following steps:
step one, dissolving bismuth nitrate into 100mL of nitric acid solution (1M) to obtain bismuth nitrate solution;
step two, adding nano SiO into bismuth nitrate solution2Stirring for 30min to obtain a solution I;
dissolving stannous chloride in a sodium hydroxide solution to obtain a solution II;
step four, mixing the solution I and the solution II, stirring for 5min, washing and filtering to obtain a solid;
step five, sintering the solid obtained in the step four for 6 hours at 400 ℃ in the argon-hydrogen reduction protective atmosphere to obtain the bismuth-based silicon dioxide material (Bi-SiO)2) (ii) a As shown in fig. 1, when the XRD patterns before and after doping with Bi are compared, the characteristic diffraction peak intensity of Bi increases as the Bi content increases. The result shows that the method successfully synthesizes the bismuth-based silicon dioxide (Bi-SiO)2) A material.
Example 4:
a preparation method of a bismuth-based silicon dioxide material comprises the following steps:
step one, dissolving bismuth nitrate into 100mL of nitric acid solution (1M) to obtain bismuth nitrate solution;
step two, adding nano SiO into bismuth nitrate solution2Stirring for 30min to obtain a solution I;
dissolving stannous chloride in a sodium hydroxide solution to obtain a solution II;
step four, mixing the solution I and the solution II, stirring for 5min, and carrying out intermittent irradiation, washing and filtering on the mixed reaction liquid of the solution I and the solution II by using an infrared lamp while stirring to obtain a solid; the power of the infrared lamp is 275W; the distance between the infrared lamp and the mixed reaction liquid is 5 cm; the intermittent irradiation is irradiation for 1min, and the irradiation is stopped for 30s, so as to circulate;
step five, sintering the solid obtained in the step four for 6 hours at 400 ℃ in the argon-hydrogen reduction protective atmosphere to obtain the bismuth-based silicon dioxide material (0.6 Bi-SiO)2-1)；
Example 5:
a preparation method of a bismuth-based silicon dioxide material comprises the following steps:
step one, dissolving bismuth nitrate into 100mL of nitric acid solution (1M) to obtain bismuth nitrate solution;
step two, adding nano SiO into bismuth nitrate solution2Stirring for 30min to obtain a solution I;
dissolving stannous chloride in a sodium hydroxide solution to obtain a solution II;
step four, mixing the solution I and the solution II, stirring for 5min, washing and filtering to obtain a solid;
fifthly, sintering the solid obtained in the fourth step for 6 hours at 400 ℃ in an argon-hydrogen reduction protective atmosphere to obtain a bismuth-based silicon dioxide material; the method comprises the following steps of (1) reprocessing the bismuth-based silicon dioxide material: placing bismuth-based silicon dioxide material in low temperature plasma treatment instrument, introducing gas into the low temperature plasma treatment instrument to form plasma, and treating the bismuth-based silicon dioxide material for 2min to obtain bismuth-based silicon dioxide material (0.6 Bi-SiO)2-2)；
The gas introduced into the low-temperature plasma treatment instrument is SF6And ethanol; the frequency of the low-temperature plasma processor is 15KHz, the power is 35W, and the processing temperature is 40 ℃; wherein ethanol is gasified and then mixed with SF6Mixing and introducing into a low-temperature plasma treatment instrument;
example 6:
a preparation method of a bismuth-based silicon dioxide material comprises the following steps:
step one, dissolving bismuth nitrate into 100mL of nitric acid solution (1M) to obtain bismuth nitrate solution;
step two, adding nano SiO into bismuth nitrate solution2Stirring for 30min to obtain a solution I;
dissolving stannous chloride in a sodium hydroxide solution to obtain a solution II;
step four, mixing the solution I and the solution II, stirring for 5min, and carrying out intermittent irradiation, washing and filtering on the mixed reaction liquid of the solution I and the solution II by using an infrared lamp while stirring to obtain a solid; the power of the infrared lamp is 275W; the distance between the infrared lamp and the mixed reaction liquid is 5 cm; the intermittent irradiation is irradiation for 1min, and the irradiation is stopped for 30s, so as to circulate;
fifthly, sintering the solid obtained in the fourth step for 6 hours at 400 ℃ in an argon-hydrogen reduction protective atmosphere to obtain a bismuth-based silicon dioxide material; the method comprises the following steps of (1) reprocessing the bismuth-based silicon dioxide material: placing bismuth-based silicon dioxide material in low temperature plasma treatment instrument, introducing gas into the low temperature plasma treatment instrument to form plasma, and treating the bismuth-based silicon dioxide material for 2min to obtain bismuth-based silicon dioxide material (0.6 Bi-SiO)2-3)；
The gas introduced into the low-temperature plasma treatment instrument is SF6And ethanol; the frequency of the low-temperature plasma processor is 15KHz, the power is 35W, and the processing temperature is 40 ℃; wherein ethanol is gasified and then mixed with SF6Mixing and introducing into a low-temperature plasma treatment instrument;
wherein, the dosage of each raw material in the examples 1-6 is shown in the table 1:
TABLE 1
Application of iodine adsorption:
A. weighing a certain amount of elemental iodine and placing the elemental iodine in a glass bottle;
B. a certain amount of the bismuth-based silica material m prepared in examples 1 to 60Wrapping with filter paperThe middle upper part of the glass bottle is used for sealing the bottle mouth;
C. placing the glass bottle in a 75 ℃ oven, and keeping the temperature for 24 hours;
D. the adsorption capacity is determined by a weighing method, and the weight m of the adsorbed bismuth-based silicon dioxide material is weighedtThe adsorption amount Q (mg/g) was calculated by the following formula:
Q(mg/g)＝(mt-m0)/m0×1000
table 2 shows bismuth-based silica materials (Bi-SiO) prepared in examples 1 to 62) Iodine adsorption performance of (1).
TABLE 2
From Table 2, it can be seen that pure nano SiO2The adsorption capacity of the material to iodine is only 92mg/g, the adsorption capacity of the material to iodine is greatly improved after Bi is loaded, the adsorption capacity is increased along with the increase of Bi content, and a sample is 0.6Bi-SiO2The iodine adsorption amount of the product is up to 894 mg/g; the iodine adsorption amount of the bismuth-based silicon dioxide material can be obviously improved by applying infrared radiation in the reaction process and treating the bismuth-based silicon dioxide material through low-temperature plasma; the results show that the bismuth-based silica material (Bi-SiO) of the present invention2) The iodine trapping performance of the material is far higher than that of other similar materials.
As shown in FIG. 2, 0.6Bi-SiO was compared2The XRD patterns before and after the adsorption of the iodine show that BiI appears in the XRD patterns after the adsorption of the iodine3And BiOI, indicating Bi-SiO2There is chemisorption of the material to the adsorption of iodine. The results show that the bismuth-based silica (Bi-SiO) of the present invention2) The material is a good iodine trapping material.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (7)
1. The preparation method of the bismuth-based silicon dioxide material is characterized by comprising the following steps:
dissolving bismuth nitrate in a nitric acid solution to obtain a bismuth nitrate solution;
step two, adding nano SiO into bismuth nitrate solution2Stirring for 30-45 min to obtain a solution I;
dissolving stannous chloride in a sodium hydroxide solution to obtain a solution II;
step four, mixing the solution I and the solution II, stirring for 5-10 min, washing, and filtering to obtain a solid;
fifthly, sintering the solid obtained in the fourth step for 5.5-6.5 hours at 350-450 ℃ in an argon-hydrogen reduction protective atmosphere to obtain a bismuth-based silicon dioxide material;
in the fourth step, while stirring, an infrared lamp is adopted to perform intermittent irradiation on the mixed reaction liquid of the solution I and the solution II; the power of the infrared lamp is 240-300W; the distance between the infrared lamp and the mixed reaction liquid is 5-10 cm; the intermittent irradiation is 1min, and the irradiation is stopped for 30s, so that the circulation is realized.
2. The preparation method of the bismuth-based silicon dioxide material as claimed in claim 1, wherein the mass volume ratio of the bismuth nitrate to the nitric acid solution is 2-8 g:100 mL; the concentration of the nitric acid solution is 0.5-1.5 mol/L.
3. The method for preparing a bismuth-based silica material according to claim 1, wherein the bismuth nitrate and the nano SiO2The mass ratio of (A) to (B) is 2-8: 1.5.
4. The preparation method of the bismuth-based silicon dioxide material as claimed in claim 1, wherein the mass volume ratio of the stannous chloride to the sodium hydroxide solution is 1.5-5.5 g: 70-120 mL; the concentration of the sodium hydroxide solution is 1.5-2.5 mol/L.
5. The method for preparing the bismuth-based silica material according to claim 1, wherein in the fifth step, the bismuth-based silica material is reprocessed by the process of: and (3) placing the bismuth-based silicon dioxide material in a low-temperature plasma treatment instrument, and introducing gas into the low-temperature plasma treatment instrument to form plasma to treat the bismuth-based silicon dioxide material for 1-3 min.
6. The method for preparing the bismuth-based silica material according to claim 5, wherein the gas introduced into the low-temperature plasma treatment apparatus is SF6And ethanol; the frequency of the low-temperature plasma treatment instrument is 10-30 KHz, the power is 30-60W, and the treatment temperature is 30-45 ℃; wherein ethanol is gasified and then mixed with SF6Mixing and introducing into a low-temperature plasma processor.
7. Use of a bismuth-based silica material according to any one of claims 1 to 6 for the capture of radioiodine.
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