CN111939770B - Bismuth-based functional material for adsorbing gaseous iodine and preparation method and application thereof - Google Patents
Bismuth-based functional material for adsorbing gaseous iodine and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of nuclear fuel post-treatment, and discloses a bismuth-based functional material for adsorbing gaseous iodine and a preparation method and application thereof, wherein bismuth salt and polyacrylonitrile are dissolved in a solvent and mixed to form a precursor solution; carrying out electrostatic spinning to obtain a fiber membrane; and pre-oxidizing in an air atmosphere and carbonizing in an inert gas atmosphere to obtain the bismuth-based functional material. The material takes the carbon nanofiber membrane as a carrier, and the metal bismuth nanoparticles are uniformly attached to the fibers, so that abundant active sites are provided for chemical adsorption of iodine, the adsorption capacity of the material can reach 560mg/g, and the material can effectively adsorb and separate gaseous iodine. Meanwhile, the material is simple in preparation method and low in raw material cost, and more importantly, compared with most of powdery adsorbents, the material has a macro membrane morphological structure with good flexibility and high thermal stability, is expected to be applied to large-scale industrialization in the spent fuel post-treatment process, and has a wide prospect.
Description
Technical Field
The invention relates to the technical field of nuclear fuel post-treatment, in particular to a bismuth-based functional material for adsorbing gaseous iodine and a preparation method and application thereof.
Background
The nuclear power is an ideal green energy source and has the advantages of safety, cleanness, economy, high efficiency and the like. In the development of nuclear power, China always adheres to the policy of closed cycle of nuclear fuel, and inevitably carries out post-treatment on the spent fuel, so that a large amount of radioactive waste gas is inevitably generated in the treatment process of the spent fuel. Radioactive gaseous iodine (I)129、I131) One of them is that, because of its extremely high volatility and radioactive toxicity, exposure to radioactive iodine can cause metabolic disorders, mental retardation, and increased risk of thyroid cancer.
At present, radioactive gaseous iodine is mainly separated by a solid adsorption method in the industry, and the adsorption materials researched more are active carbon, zeolite, macroporous resin, metal organic framework compound (MOF) and the like. Among them, silver-containing zeolite is the most commonly used iodine-adsorbing material and is also a target bar with iodine-adsorbing property. CN109569535A discloses an adsorption material for enriching radioactive iodine in seawater and a preparation method thereof, the adsorption material is CuFC/AgFC, the loading body is a polypropylene fiber filter element, the adsorption material is simple and convenient to manufacture, the cost is low, the radioactive iodine in seawater can be quickly enriched in a short time, the efficiency of a single-pass method and the efficiency of an eight-cycle adsorption method are respectively 55% and 100%, and the adsorption material can be respectively applied to seawater samples of a large-volume surface layer and a small-volume middle layer (bottom layer).
However, a large part of iodine adsorbed by the silver-containing zeolite exists in the form of iodine molecules, so that the iodine is easy to desorb and migrate; meanwhile, the silver is expensive and has the defects of toxicity, low utilization rate, easy aging and the like, so that the industrial application of the silver-containing zeolite is limited to a certain extent. Therefore, the search for a novel efficient iodine adsorbent has very important practical significance.
The bismuth-based porous material is an emerging iodine adsorbent in recent years, can quickly capture iodine simple substances, and has the advantages of low cost, easy material synthesis, low toxicity, high adsorption capacity and the like compared with other functional materials (silver-based zeolite, MOF and the like). While the adsorbent captures iodine and is finally converted into BiI3And Bi5O7I has a very good thermodynamic stability so that the captured iodine is not easily desorbed. Therefore, we believe that bismuth-based porous materials are expected to replace silver-based materials commonly used in the current spent fuel reprocessing processes.
Jae Hwan Yang et al reported a method for removing the metal in the nuclear materials journal129I bismuth-based adsorbent Synthesis method (Jae Hwan Yang, et al, "Novel Synthesis of bismuth-based adsorbents for the removal of129In off-gas, "Journal of Nuclear Materials 457(2015):1-8.), which is prepared by mixing polyvinyl alcohol (PVA) as a template with a precursor solution of bismuth nitrate pentahydrate, and calcining in air to remove PVA and synthesize a porous block material. The iodine capture capacity of the synthesized sample can reach 1.9 times of that of commercial silver exchanged zeolite (AgX), and the thermodynamic stability of the reaction product explains the high iodine removal efficiency.
A bismuth-based composite material prepared by a sol-gel method (Facheng Yi, Mianxin Song, et al. "Novel synthesis of Bi-Bi) was reported in journal of hazardous hazards2O3–TiO2-C composition for capturing iodine-129in off-gas, "Journal of Hazardous materials.365(2019):81-87 ], and an orthogonal test shows that the iodine capturing capacity of the optimal composite material at 200 ℃ is about 504.0 + -19.5 mg/g.
Recently, Fateme Rezaei et al reported in the Journal of Chemical Engineering a bismuth-loaded mordenite adsorbent prepared by wet impregnation (Fateme Rezaei, et al, "Development of bismuth-molybdenum adsorbents for iodine capture from off-gas streams." Chemical Engineering Journal (2020):123583.), and leaching experiments were performed to test the stability of the adsorbent in aqueous solution after iodine capture.
However, in the above-reported bismuth-based adsorbents, oxides of bismuth are contained, and it is known from their article that since gibbs free energy of reaction becomes larger than zero, it does not have a trapping effect on iodine as a simple substance, which results in insufficient adsorption performance for iodine and is difficult to further improve. In addition, their thermodynamic stability is not very good, and significant decomposition occurs when the temperature reaches 300 ℃.
Based on the above, the bismuth-based porous material for adsorbing iodine needs to be further researched, and the adsorption capacity, adsorption efficiency, adsorption stability and the like of the material to iodine are improved.
Disclosure of Invention
The invention aims to provide a bismuth-based adsorption material which has abundant active sites and high adsorption capacity to gaseous iodine, has stable performance, and can solve the problems of low adsorption capacity, high cost, difficult recovery and the like of the existing silver-based adsorbent.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method of the bismuth-based functional material for adsorbing gaseous iodine is characterized by comprising the following steps of:
(1) dissolving bismuth salt and polyacrylonitrile in a solvent, and mixing to form a precursor solution;
(2) carrying out electrostatic spinning on the precursor solution under high pressure to obtain a fiber membrane;
(3) pre-oxidizing the fiber membrane in an air atmosphere;
(4) carbonizing the pre-oxidized fiber film in an inert gas atmosphere to obtain the bismuth-based functional material.
The electrostatic spinning is a special fiber manufacturing process, can effectively manufacture fiber filaments with nanometer-level diameters, and has the advantages of simple equipment, low spinning cost and controllable process. According to the invention, bismuth salt and polyacrylonitrile are mixed to form a precursor solution, a fiber structure is obtained after electrostatic spinning, and then the bismuth-based composite material which takes carbon nano-fiber as a carrier and metal bismuth particles are uniformly distributed in the surface and inner pore channels of the carbon fiber is formed through the subsequent pre-oxidation and carbonization processes.
The preoxidation is a bridge after the precursor (precursor) is started (carbon fiber), the fibers are crosslinked to form a trapezoidal polymer, the fibers are ensured to have good shapes in the subsequent high-temperature carbonization process, the phenomena of fusion, doubling and the like are avoided, and the prepared carbon fiber has excellent mechanical properties. In the high-temperature carbonization process, the carbon fibers are heated and decomposed, a large number of pore channel structures are left in the fibers, meanwhile, bismuth nitrate is decomposed into bismuth oxide firstly along with the rise of temperature, and then the bismuth oxide is reduced into simple substance bismuth through reaction with the carbon fibers, a large number of gases generated in the process can drive bismuth particles to migrate to the pore channel structures on the outer surface and the inner portion of the fibers, so that the agglomeration of the simple substance bismuth can be effectively avoided, and abundant active sites are provided for capturing iodine gas. The bismuth-based material is used as the iodine adsorbent, so that the iodine simple substance can be rapidly captured, and the nano-grade fiber filament obtained by polyacrylonitrile electrostatic spinning is combined, so that the active sites of the material are increased, and the adsorption capacity of the material to iodine is improved.
In the step (1), the mass ratio of the bismuth salt to the polyacrylonitrile to the solvent is (0.06-0.10): (0.08-0.14): 1. within the proportion range, the bismuth salt can be completely dissolved in the solvent, and the viscosity of the solution is not too high, so that smooth spinning can be realized; polyacrylonitrile is good in spinnability, and continuous and uniform filaments cannot be spun when the concentration is too high or too low. The contents of polyacrylonitrile and bismuth salt are very important, and the content of the bismuth salt is increased as much as possible under the condition that spinning can be carried out, so that more active sites are provided, and the spinnability of the polyacrylonitrile is considered.
In the step (2), the electrostatic spinning voltage is 10-26 KV, and the spinning speed is 0.03-0.15 mL/min. The spinning voltage is relatively related to the spinning speed, and when the voltage is adjusted to be larger, the corresponding spinning speed is also increased. The spinning speed is too high or the voltage is not proper, so that the needle head is blocked or the positive pole and the negative pole of the voltage are broken down, and danger is caused or the spinning effect is poor.
Preferably, the electrostatic spinning voltage is 18-26 KV, and the spinning speed is 0.05-0.15 mL/min. The filaments obtained within this range are uniform and can provide uniform attachment points for the bismuth salt.
In the step (3), the pre-oxidation parameters are as follows: the heating rate is 2-5 ℃/min, the pre-oxidation temperature is 220-300 ℃, and the heat preservation time is 0.5-3 h. Within the temperature rise rate and temperature range, residual solvent in the precursor can be effectively removed, and the fibers are mutually crosslinked to form a trapezoidal polymer, so that the fibers are ensured to have good shapes in the high-temperature carbonization process, the phenomena of melting, doubling and the like are avoided, and the prepared carbon fibers have excellent mechanical properties.
In the step (4), the carbonization parameters are as follows: the heating rate is 5-20 ℃/min, the carbonization temperature is 700-900 ℃, and the heat preservation time is 1-3 h. When the temperature rise rate is too slow, carbonization time is too long, and when the temperature rise rate is too fast, mechanical properties of the carbon fibers are reduced. The carbonization temperature is controlled to be 700-900 ℃, carbon fibers with stable performance can be well prepared, and meanwhile bismuth oxide can be completely reduced to simple substance bismuth in the temperature range.
The bismuth salt includes bismuth nitrate, bismuth acetate, bismuth nitrate or bismuth oxalate and hydrate thereof. Preferred are hydrates of bismuth nitrate, such as bismuth nitrate pentahydrate.
The solvent comprises dimethylformamide, dimethylacetamide and dimethyl sulfoxide, so that the bismuth salt and polyacrylonitrile can be dissolved, and dimethylformamide is preferred.
The invention also provides the bismuth-based functional material prepared by the preparation method.
The invention also provides the application of the bismuth-based functional material in adsorbing gaseous iodine. The material has very high adsorption capacity and high adsorption rate to gaseous iodine, can reach more than 90% of saturated adsorption capacity only in half an hour, has good thermal stability, can not be oxidized at 300 ℃ in the air, and can be stabilized to more than 800 ℃ even under inert atmosphere.
Compared with the prior art, the invention has the following beneficial effects:
(1) the bismuth-based functional material provided by the invention takes the carbon nanofiber membrane as a carrier, and the metal bismuth nanoparticles are uniformly attached to the fiber, so that abundant active sites are provided for iodine adsorption, gaseous iodine can be effectively adsorbed and separated, and meanwhile, the bismuth-based functional material is good in thermal stability and cannot be oxidized at high temperature.
(2) Compared with a silver-based adsorbent, the bismuth-based functional material provided by the invention has the advantages of low raw material price and simple preparation method.
(3) Compared with most of powdery adsorbents, the bismuth-based functional material provided by the invention has a macroscopic film form and a network structure formed by fiber connection under a microscopic view, and is more convenient for large-scale industrial application in the spent fuel post-treatment process.
Drawings
FIG. 1 is a schematic diagram of the preparation process and application of the bismuth-based functional material of the present invention.
FIG. 2 is an SEM image of the functional materials of comparative examples 1(a, b), examples 1(c, d) and application examples 1(e, f).
Figure 3 XRD patterns of the functional materials of comparative example 1, example 1 and application example 1.
Fig. 4 is a graph showing the kinetics of iodine adsorption for the functional materials of example 1 and comparative example 1.
Fig. 5 is a TGA plot of the functional material of example 1 and application example 1.
FIG. 6 is an XRD pattern of the bismuth-based functional material of example 2.
Fig. 7 is an isothermal adsorption curve of the functional material of example 1 in application example 2 at different concentrations of iodine gas.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Those skilled in the art should understand that they can make modifications and equivalents without departing from the spirit and scope of the present invention, and all such modifications and equivalents are intended to be included within the scope of the present invention.
The raw materials bismuth nitrate pentahydrate, polyacrylonitrile and dimethylformamide used in the following examples were all purchased from alatin chemical co.
Example 1
The preparation process of the bismuth-based functional material is schematically shown in figure 1:
(1) preparing a precursor solution: according to the mass ratio of 0.08: 0.10: 1, weighing bismuth nitrate pentahydrate, polyacrylonitrile and dimethylformamide, and stirring to uniformly mix the bismuth nitrate pentahydrate, the polyacrylonitrile and the dimethylformamide to obtain spinning precursor solution;
(2) electrostatic spinning: spinning the precursor solution prepared in the step (1) in an electrostatic spinning machine at the voltage of 24KV and the spinning speed of 0.010mL/min to obtain a fiber membrane;
(3) pre-oxidation: and (3) heating the fiber membrane prepared in the step (2) to 260 ℃ at the speed of 2 ℃/min in the air atmosphere, and keeping the temperature for 2 h.
(4) Carbonizing: and (4) heating the pre-oxidized fiber film prepared in the step (3) to 800 ℃ at the speed of 5 ℃/min in the atmosphere of inert gas, and keeping the temperature for 2 hours to obtain the bismuth-based functional material for adsorbing gaseous iodine.
Comparative example 1
The preparation process according to the examples is distinguished in that in step (1) only 0.10: 1, preparing a mixed solution of polyacrylonitrile and dimethylformamide, not adding bismuth nitrate pentahydrate, and obtaining the bismuth-free functional material by the same other steps.
Application example 1
Respectively selecting 0.1g of the bismuth-based functional material prepared in the example 1 and the bismuth-free functional material prepared in the comparative example 1; the above selected materials were respectively put into an iodine adsorption apparatus as shown in fig. 1, the concentration of iodine gas in the apparatus was maintained at 1g/L, the reaction temperature was 200 ℃, and then their iodine adsorption capacities were calculated by weighing the mass change of the adsorbents after different reaction times. Calculated according to the formula:
iodine adsorption capacity ═ (mass after reaction-mass before reaction)/mass before reaction;
in order to ensure that the increase in mass was due to the reaction of iodine instead of air to form an oxide, 0.1g of the bismuth-based functional material prepared in example 1 was weighed, placed in an air atmosphere, kept at a temperature of 200 ℃ as a blank, and then weighed for a mass change.
Characterization analysis was performed on the iodine adsorbing material prepared in example 1, the bismuth-free material in comparative example 1, and the adsorbed material in experimental example 1, and they obtained SEM graph shown in fig. 2, XRD graph shown in fig. 3, electrosorption kinetics graph shown in fig. 4, and TGA thermogravimetric graph shown in fig. 5, respectively.
Wherein, as shown in FIG. 2, in which (a) and (b) are the fibers obtained in comparative example 1, it can be seen that the surface thereof is smooth without any adhesion; (c) and (d) the surface morphology of the bismuth-based functional material prepared in example 1 shows that in a network structure formed by carbon nanofibers with diameters of 200-500 nm, bismuth nanoparticles are relatively uniformly attached to the fibers, so that abundant active sites are provided for iodine adsorption, and the improvement of the adsorption amount of iodine is facilitated. Wherein (e) and (f) are the surface morphology of the fiber after adsorption of iodine in application example 1, it is understood that the particles on the fiber changed from spherical to flaky after adsorption. The bismuth attached to the fiber is called as an effective iodine adsorption active site, so that the iodine can be effectively adsorbed, and the adsorption mechanism of the material is obtained, wherein a new stable phase bismuth iodide and a small part of physical adsorption are generated mainly through the reaction of chemical adsorption elemental bismuth and iodine gas. Because each filament is distributed with bismuth nano-particles, the iodine adsorption quantity of the material is greatly improved.
As shown in FIG. 3, it can be seen from the XRD curves of the functional materials of comparative example 1, example 1 and application example 1 that the diffraction peak on the curve after adsorption was changed from Bi (ICDD PDF No.85-1330) to BiI3(ICDD PDF No.48-1795)。
As shown in fig. 4, it can be seen that the bismuth-based functional material prepared in example 1 has very good thermal stability in air atmosphere, and is not oxidized by air even at a high temperature of 200 ℃; meanwhile, the bismuth-based functional material can be observed to have a very high rate of adsorbing gaseous iodine, and can reach more than 90% of the saturated adsorption capacity in half an hour; when the reaction time reached 2h, the adsorption of gaseous iodine reached saturation at 560 mg/g.
The maximum adsorption capacity of the bismuth-free material prepared in the comparative example 1 is less than 200mg/g, which is greatly different from the adsorption capacity of the bismuth-based functional material of the example 1 to iodine.
Thermogravimetric analysis was performed on the functional material after capturing iodine gas in example 1 and application example 1 under the protection of nitrogen gas by using a thermogravimetric analyzer, as shown in fig. 5. It is clear that the mass of the material of example 1 does not change substantially by only 8.12% mass reduction when the temperature is raised to 800 c, whereas the mass of the adsorbed material decreases by 62.45%. Through comparative analysis, the mass change can be attributed to the following three parts: 8.12% in example 1 is due to adsorption of moisture in the air or to a small amount of decomposition of the adsorbent itself; whereas 16.88% in application example 1 was physical adsorption of iodine gas; the rest 37.45 percent is generated into BiI by chemical adsorption3Decomposition of (3). Therefore, the bismuth-based functional material obtained in the example 1 has excellent thermal stability, can not be decomposed up to 800 ℃, and can be decomposed at 400 ℃ higher than that of the material in the prior art, and the bismuth-based functional material obtained in the example has excellent stability.
Application example 2
In order to explore the iodine gas trapping performance of the bismuth-based functional material at low concentration, a series of isothermal adsorption experiments are also carried out. 0.1g of the bismuth-based functional material prepared in example 1 was taken, and iodine contents of different concentrations were simulated by adding iodine simple substances of different masses, so as to explore the functional material at different concentrations. Similarly, the reaction temperature is controlled to be 200 ℃, the iodine capture performance of the bismuth-based functional material is calculated by weighing the mass change of the bismuth-based functional material after 4 hours, and the result is shown in figure 6.
Example 2
The preparation process schematic diagram of the bismuth-based functional material is also shown in figure 1:
(1) preparing a precursor solution: according to the mass ratio of 0.08: 0.10: 1, weighing bismuth nitrate pentahydrate, polyacrylonitrile and dimethylformamide, and stirring to uniformly mix the bismuth nitrate pentahydrate, the polyacrylonitrile and the dimethylformamide to obtain spinning precursor solution;
(2) electrostatic spinning: spinning the precursor solution prepared in the step (1) in an electrostatic spinning machine at the voltage of 24KV and the spinning speed of 0.010mL/min to obtain a fiber membrane;
(3) pre-oxidation: and (3) heating the fiber membrane prepared in the step (2) to 260 ℃ at the speed of 2 ℃/min in the air atmosphere, and keeping the temperature for 2 h.
(4) Carbonizing: and (4) heating the pre-oxidized fiber film prepared in the step (3) to 650 ℃ at the speed of 5 ℃/min in the atmosphere of inert gas, and keeping the temperature for 2 hours to obtain the bismuth-based functional material for adsorbing gaseous iodine.
The XRD curve of this material is shown in fig. 7, and the adsorption performance of the material to iodine was determined according to application example 1, and the maximum adsorption capacity of the material was 396 ± 23mg/g, which resulted in a decrease in the amount of iodine adsorbed due to the fact that the bismuth oxide decomposed from bismuth nitrate could not be completely reduced to elemental bismuth due to the decrease in temperature during carbonization.
Example 3
The preparation process schematic diagram of the bismuth-based functional material is also shown in figure 1:
(1) preparing a precursor solution: according to the mass ratio of 0.06: 0.12: 1, weighing bismuth nitrate pentahydrate, polyacrylonitrile and dimethylformamide, and stirring to uniformly mix the bismuth nitrate pentahydrate, the polyacrylonitrile and the dimethylformamide to obtain spinning precursor solution;
(2) electrostatic spinning: spinning the precursor solution prepared in the step (1) in an electrostatic spinning machine, wherein the voltage is 20KV, and the spinning speed is 0.010mL/min, so as to obtain a fiber membrane;
(3) pre-oxidation: and (3) heating the fiber membrane prepared in the step (2) to 280 ℃ at the speed of 2 ℃/min in the air atmosphere, and keeping the temperature for 1 h.
(4) Carbonizing: and (4) heating the pre-oxidized fiber film prepared in the step (3) to 8000 ℃ at the speed of 5 ℃/min in the atmosphere of inert gas, and keeping the temperature for 2 hours to obtain the bismuth-based functional material for adsorbing gaseous iodine. After reacting for 4h at 200 ℃, the adsorption performance of the material to iodine is measured according to application example 1, and the maximum adsorption capacity is 440 +/-18 mg/g.
In conclusion, the adsorption capacity of the silver adsorbent reported in the prior art to iodine is mostly within 150-300 mg/g, and the bismuth-based functional material disclosed by the invention realizes great improvement of the adsorption capacity to iodine, has excellent thermal stability and low cost, and is expected to be used for replacing the existing silver-based adsorption material.
Claims (7)
1. The preparation method of the bismuth-based functional material for adsorbing gaseous iodine is characterized by comprising the following steps of:
(1) dissolving bismuth salt and polyacrylonitrile in a solvent, and mixing to form a precursor solution; the mass ratio of the bismuth salt to the polyacrylonitrile to the solvent is (0.06-0.10): (0.08-0.14): 1;
(2) carrying out electrostatic spinning on the precursor solution under high pressure to obtain a fiber membrane;
(3) pre-oxidizing the fiber membrane in an air atmosphere;
(4) carbonizing the pre-oxidized fiber film in an inert gas atmosphere to obtain the bismuth-based functional material; the carbonization parameters are as follows: the heating rate is 5-20 ℃/min, the carbonization temperature is 700-900 ℃, and the heat preservation time is 1-3 h.
2. The method for preparing the bismuth-based functional material for adsorbing gaseous iodine according to claim 1, wherein in the step (2), the electrostatic spinning voltage is 10-26 KV, and the spinning speed is 0.03-0.15 mL/min.
3. The method for preparing bismuth-based functional material for adsorbing gaseous iodine according to claim 1, wherein in the step (3), the pre-oxidation parameters are as follows: the heating rate is 2-5 ℃/min, the pre-oxidation temperature is 220-300 ℃, and the heat preservation time is 0.5-3 h.
4. The method for preparing a bismuth-based functional material for adsorbing gaseous iodine according to claim 1, wherein the bismuth salt comprises bismuth nitrate, bismuth acetate, bismuth nitrate or bismuth oxalate and hydrates thereof.
5. The method for preparing a bismuth-based functional material for adsorbing gaseous iodine according to claim 1, wherein the solvent comprises dimethylformamide, dimethylacetamide, and dimethylsulfoxide.
6. A bismuth-based functional material prepared according to the preparation method of any one of claims 1 to 5.
7. The use of the bismuth-based functional material of claim 6 for adsorbing gaseous iodine.
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