CN110813212A - Method for inhibiting nano-silver generation - Google Patents
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- CN110813212A CN110813212A CN201911029251.1A CN201911029251A CN110813212A CN 110813212 A CN110813212 A CN 110813212A CN 201911029251 A CN201911029251 A CN 201911029251A CN 110813212 A CN110813212 A CN 110813212A
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Abstract
The invention discloses a method for inhibiting nano-silver generation, which comprises the following steps: irradiating by adopting a gamma ray irradiation source under the condition that an Ag + solution and a reducing agent coexist; the molar ratio of Ag + to the reducing agent in the solution is 1: 5-6.5. According to the method for inhibiting the production of the nano silver, the strong reducing agent is added into the Ag + solution, and the gamma ray irradiation source is adopted for irradiation, so that the production of the nano silver in the process water environment of the production and operation of the nuclear power station can be effectively inhibited.
Description
Technical Field
The invention particularly relates to a method for inhibiting nano-silver generation in a nuclear power plant operating water environment.
Background
It is well known that silver ions will rapidly reduce to metallic silver in the presence of strong reducing agents, in the form of silver mirrors deposited or attached to the surface of the ware. Whereas nano-silver is a particle below 100nm in size, often stably present in suspension in solution, the size of which is much smaller than the silver particles present in the former silver precipitate or silver mirror. In order to prepare such small-sized, suspension-stable nanosilver, extensive studies have shown that, in addition to the two requirements of silver ions and reducing agent, there is generally a prerequisite, namely a stabilizer, which acts to slowly reduce the silver ions to silver atoms, ensuring that the silver atoms slowly accumulate again as small-sized nanosilver suspended in solution, rather than rapidly accumulating as large-sized silver precipitates. Stabilizers generally include class 2. The first kind, silver ion stabilizer, usually a weak complexing agent for silver ions, which allows silver ions to be slowly released and reduced to silver atoms by a strong reducing agent, thereby ensuring that silver atoms are slowly accumulated to nano silver; the second type, nano-silver stabilizers, often serve both to stabilize and to limit the growth of the nano-silver. Citric acid is the most classical and widely adopted stabilizer for silver ions, and the high-efficiency preparation of nano silver is realized by utilizing the weak complexation of its polycarboxyl, wherein the adopted reducing agent is usually hydrazine hydrate with strong reducibility. However, the research on nano silver stabilizers is more and more, the nano silver stabilizers can better control the particle size uniformity of nanoparticles, meanwhile, in order to ensure the slow reduction of silver ions, weak reducing agents are often adopted, but the requirement of rapid preparation is difficult to realize due to weak reducing capability. In order to solve the contradiction, certain auxiliary factors are often used for activation under the condition that a stabilizing agent and a weak reducing agent coexist. For example, the gelatin is used as a stabilizer and a weak reducing agent, and is assisted by gamma rays, laser and ultraviolet light, so that the nano silver can be efficiently prepared. For another example, under the assistance of gamma-rays, the carboxymethyl cellulose hydrogel and the graphene are used as a stabilizer and a very weak reducing agent, and the nano silver can be effectively prepared in situ. The aqueous solution can be ionized and excited under the high-energy irradiation of gamma rays, so that reducing free radicals and oxidizing free radicals are generated. When a scavenging agent similar to isopropanol which is an oxidizing free radical exists in the system, silver ions in the system can be reduced by existing reducing free radicals, and at the moment, if a nano-silver stabilizing agent exists in the system, silver nanoparticles are easy to generate. The nano silver can be effectively prepared by gamma-ray irradiation with a surfactant as a stabilizer and isopropanol as an oxidative free radical scavenger. In conclusion, the nano silver can be effectively generated only by the presence of the stabilizer and the reducing agent in the preparation system, wherein the reducing agent comprises a strong reducing agent, a weak reducing agent under the assistance of rays and a strong reducing free radical.
In the process environment of nuclear power plant production operation, radioactive waste liquid contains nano silver, which can be enriched in marine organisms through food chain, therefore, a technical method for inhibiting production and eliminating is needed. For the inhibition of the generation of nano silver, based on the analysis of the technical scheme of nano silver preparation, the first method is that a reducing agent or a strong reducing agent cannot exist in the process water of power station production operation, however, for the normal operation of production, hydrazine hydrate which is a strong reducing agent is necessary, so that the first condition is provided for the effective generation of nano silver, and silver ions are necessarily reduced regardless of the existence of a scavenging agent of oxidative free radicals. However, whether in the form of nanosilver or not, analysis can be performed from the process water environment of the power plant production operation. In fact, in the process water, no stabilizer, including silver ion stabilizer and nano silver stabilizer, is added, and the two factors of slowly reducing silver ions and slowly accumulating to form nano silver or stably accumulating reduced silver atoms do not exist. Of course, no high concentration of silver ions is added into the process water, and the source of the silver ions depends on the silver ions slowly released from the pipeline material, which just plays the role of the silver ion stabilizer (such as citric acid) and indirectly provides the condition of the stabilizer for the generation of nano silver. Therefore, it is inevitable that nano silver is generated, and how to suppress the generation of nano silver becomes an important problem. Based on the analysis, the invention provides a method for inhibiting the production of nano silver in the process water environment of the production and operation of the nuclear power station.
Disclosure of Invention
In view of the above, the present invention provides a method for inhibiting the production of nano silver, which can effectively inhibit the production of nano silver in a process water environment of a nuclear power plant production operation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for inhibiting the production of nano-silver, comprising the steps of: irradiating by adopting a gamma ray irradiation source under the condition that an Ag + solution and a reducing agent coexist; the molar ratio of Ag + to the reducing agent in the solution is 1: 5-6.5.
According to some preferred embodiment modes of the present invention, the gamma ray irradiation source is60And the irradiation intensity of the Co irradiation source is less than or equal to 30Gy/min, and the irradiation time is 5-7 h.
According to some preferred embodiment modes of the invention, the reducing agent is hydrazine hydrate.
According to some preferred embodiment modes of the present invention, the concentration of Ag + in the Ag + solution is 0.03 to 0.05 g/L.
According to some preferred embodiment modes of the present invention, the Ag + solution is a silver nitrate solution.
According to some preferred embodiment modes of the present invention, the Ag + solution further includes an acidic substance.
According to some preferred embodiment modes of the invention, the acidic substance is boric acid.
According to some preferred embodiment modes of the present invention, the concentration of boric acid in the Ag + solution is 2 to 3 g/L.
Preferably, the method specifically comprises the following steps: mixing boric acid solution, silver nitrate solution and hydrazine hydrate, vibrating uniformly in dark place, and adopting60And irradiating by using a Co irradiation source.
Compared with the prior art, the invention has the advantages that: according to the method for inhibiting the production of the nano silver, the strong reducing agent is added into the Ag + solution, and the gamma ray irradiation source is adopted for irradiation, so that the production of the nano silver in the process water environment of the production and operation of the nuclear power station can be effectively inhibited.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a graph comparing the relative amounts of nanosilver produced in preferred example 1 of the present invention and comparative examples 1-3;
FIG. 2 is a UV spectrum of a sample of preferred example 1 of the present invention and comparative examples 1 to 3;
FIG. 3 is a UV spectrum of a sample of preferred example 1 and comparative examples 4-5 of the present invention and a blank control;
FIG. 4 is an enlarged view of a portion of FIG. 3;
FIG. 5 is a UV spectrum of a sample of preferred example 1 and comparative examples 4-5 of the present invention and a blank control;
FIG. 6 shows the particle size distribution of irradiated samples of preferred embodiment 1 of the present invention measured by dynamic light scattering;
FIG. 7 TEM photograph of an irradiated sample of the preferred embodiment 1 of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not a whole embodiment. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents used in the following examples are as follows: AgNO3(AR, 99.8%), hydrazine hydrate (AR, NH)2-NH2H2O, 80%), boric acid (AR, H)3BO399%), high purity nitrogen (Shanghai Wu Steel gas), and experimental water was triple distilled water.
The test instrument was as follows: ultraviolet visible light absorberSpectrometer (PE Lambda 365, PE Corp., USA), laser particle sizer (Zetasizer Nano ZS, Malvern, UK), transmission electron microscope (HT7700, Hitachi, Japan),60co irradiation source (nuclear power research institute, China), constant temperature shaking table (Julabo SW23, Youlebo, Germany).
Example 1
Sample configuration: adding 12.5mL (H) of prepared boric acid solution into a 50mL round-bottom centrifuge tube with scales3BO3Concentration of 4.8g/L), 6.5mL of triple distilled water, 1.0mL of AgNO3Solution (concentration 0.777g/L) and 5.0mL hydrazine hydrate solution (N)2H4·H2O, the concentration is 0.2g/L), namely the total 25mL of the reaction system is covered and shaken evenly in a dark place.
Irradiation test: after the sample is prepared, the sample is placed in a lightproof paper sample box, and the sample box is immediately placed in60And (3) a Co irradiation source is used for carrying out irradiation, the intensity is less than or equal to 30Gy/min, the time is 6h, and the total dose is less than or equal to 10.8 kGy. And after the irradiation is finished, immediately detecting the sample.
Example 2
Sample configuration: 10.0mL (H) of the prepared boric acid solution is added into a 50mL round-bottom centrifuge tube with scales respectively3BO3Concentration of 4.8g/L), 12mL of triple distilled water, 1.5mL of AgNO3Solution (concentration 0.777g/L) and 11.0mL hydrazine hydrate solution (N)2H4·H2O, concentration is 0.2g/L), namely the total volume of the reaction system is 34.5mL, and the reaction system is covered and shaken evenly in dark.
Irradiation test: after the sample is prepared, the sample is placed in a lightproof paper sample box, and the sample box is immediately placed in60And (3) a Co irradiation source is used for carrying out irradiation, the intensity is less than or equal to 30Gy/min, the time is 7h, and the total dose is less than or equal to 12.6 kGy. And after the irradiation is finished, immediately detecting the sample.
Comparative example 1 oxygen removal for 40min
Sample configuration: adding 12.5mL (H) of prepared boric acid solution into a 50mL round-bottom centrifuge tube with scales3BO3Concentration of 4.8g/L) and 6.5mL of triple distilled water, and slowly introducing high-purity nitrogen into the solution by using a nitrogen purging instrument to remove dissolved oxygen, wherein the oxygen removal time is 4And 0 min. Adding deoxygenated triple distilled water, adding the volume of the solution to 19.0mL, and adding 1.0mL of LAgNO3Solution (concentration of 0.777g/L) and 5.0m L hydrazine hydrate solution (N)2H4·H2O, the concentration is 0.2g/L), namely the total 25mL of the reaction system is covered and shaken evenly in a dark place.
Irradiation test: after the sample is prepared, the sample is placed in a lightproof paper sample box, and the sample box is immediately placed in60And (3) a Co irradiation source is used for carrying out irradiation, the intensity is less than or equal to 30Gy/min, the time is 6h, and the total dose is less than or equal to 10.8 kGy. And after the irradiation is finished, immediately detecting the sample.
Comparative example 2 oxygen removal for 60min
Comparative example 2 is substantially the same as the procedure of comparative example 1 except that the oxygen removal time in this comparative example is 60 min.
Comparative example 3 No irradiation
Sample configuration: adding 12.5mL (H) of prepared boric acid solution into a 50mL round-bottom centrifuge tube with scales3BO3Concentration of 4.8g/L), 6.5mL of triple distilled water, 1.0mL of AgNO3Solution (concentration 0.777g/L) and 5.0mL hydrazine hydrate solution (N)2H4·H2O, the concentration is 0.2g/L), namely the total 25mL of the reaction system is covered and shaken evenly in a dark place. And then, carrying out sample detection after keeping the sample in dark, sealing and storing at room temperature for 6h without irradiation.
Comparative examples 4 and 5 triple distilled water instead of hydrazine hydrate
Comparative example 4 is essentially the same procedure as in example 1 except that triple distilled water was used instead of hydrazine hydrate in this comparative example.
The Ag + content of the sample in comparative example 5 was twice the Ag + content of the sample in comparative example 4.
EXAMPLES results and discussion
The samples of example 1 and comparative examples 1 to 3 were tested, and the results are shown in FIGS. 1 and 2.
As can be seen from the UV spectrum in fig. 2, compared with the non-irradiated sample in comparative example 3, the samples irradiated to produce nano-silver, including the non-oxygen-removed sample in example 1 and the oxygen-removed samples in comparative examples 1 and 2, have significantly reduced absorption between 500 and 700nm, while the absorption around 410nm is increased, indicating that the irradiation causes less nano-silver with large particle size and more nano-silver with small particle size to be produced during the nano-silver production process. For this reason, it is likely that the high energy provided by irradiation causes structural damage to the large particle size nanoparticles produced.
To illustrate the total amount of nanoparticles in the sample solution, we expressed the relative amount of nanosilver in the solution as the vector mode of the spectrum (i.e., the square root of the sum of the squares of all absorbances) in the range of 350-700nm, see FIG. 1. Due to the possibility of generating H during irradiation by dissolved oxygen2O2And H is2O2And also oxidatively digesting nano silver, and thus, a control test was conducted on the influence of dissolved oxygen in irradiation, i.e., comparative examples 1 and 2. As can be seen from fig. 1, the sample with 60min oxygen produced slightly less nano-silver than the sample with 40min oxygen, however, this difference compared to the standard deviation of the parallel samples, there was no significant difference, indicating that 40min had completely removed the dissolved oxygen in the system. Compared with the samples without oxygen removal (40min and 60min), the nano silver of the samples irradiated without oxygen removal is not obviously reduced, thereby showing that under the reducing water environment in which hydrazine hydrate exists, the dissolved oxygen is little or even almost no. This is related to the addition of hydrazine hydrate, a reducing agent, to the system, indicating that hydrazine hydrate is effective in eliminating dissolved oxygen. Compared with the unirradiated control sample, the only difference between the sample and the above sample is 'irradiation and non-irradiation', because the sample and the above sample are operated in parallel, and the irradiation generation H is also excluded2O2But also the possibility of digesting the nano silver. This indicates that irradiation causes a reduction in the amount of nanosilver produced, indicating that irradiation can suppress the production of nanosilver in this environment. Irradiation inhibited nanosilver production by 26.6% on the average of the oxygen-depleted 40min and 60min samples.
Effect of hydrazine (di) hydrate on producing nano silver by irradiation
The comparison of results between the blank control (boric acid solution), example 1 and comparative examples 4 and 5 can further illustrate that irradiation can suppress the production of nano-silver, whereas irradiation itself cannot cause the silver source to produce nano-silver, which is not a factor in producing nano-silver. In comparative example 4 and comparative example 5, triple distilled water was used instead of hydrazine hydrate, i.e. the silver source was present in the system but the reducing agent was not present. After irradiation, the UV spectra of comparative example 4 and comparative example 5 have no effective absorption in the characteristic absorption interval (350-700nm) of the nano-silver, and completely coincide with the baseline spectrum of the blank control group, both are baseline noise, which indicates that the silver source cannot generate nano-silver under the irradiation condition without hydrazine hydrate, and the irradiation cannot enable the silver source to generate nano-silver regardless of the amount of the silver source. Therefore, the source of nano silver generation in the process water environment is that hydrazine hydrate reduces silver ions, but not irradiation. In contrast, irradiation can suppress the production of nano silver.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (9)
1. A method for inhibiting the production of nano-silver, comprising: the method comprises the following steps: irradiating by adopting a gamma ray irradiation source under the condition that an Ag + solution and a reducing agent coexist; the molar ratio of Ag + to the reducing agent in the solution is 1: 5-6.5.
2. The method for inhibiting the production of nano-silver according to claim 1, wherein: the gamma ray irradiation source is60And the irradiation intensity of the Co irradiation source is less than or equal to 30Gy/min, and the irradiation time is 5-7 h.
3. The method for inhibiting the production of nano-silver according to claim 2, wherein: the reducing agent is hydrazine hydrate.
4. The method for inhibiting the production of nano-silver according to claim 3, wherein: the concentration of Ag + in the Ag + solution is 0.03-0.05 g/L.
5. The method for inhibiting the production of nano-silver according to claim 3, wherein: the Ag + solution is silver nitrate solution.
6. The method for inhibiting the production of nano-silver according to claim 3, wherein: the Ag + solution also comprises an acidic substance.
7. The method for inhibiting the production of nano-silver according to claim 6, wherein: the acidic substance is boric acid.
8. The method for inhibiting the production of nano-silver according to claim 7, wherein: the concentration of boric acid in the Ag + solution is 2-3 g/L.
9. The method for inhibiting the production of nano-silver according to claim 6, wherein: the method specifically comprises the following steps: mixing boric acid solution, silver nitrate solution and hydrazine hydrate, vibrating uniformly in dark place, and adopting60And irradiating by using a Co irradiation source.
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