CN113578266B - Preparation and application of nano magnesium silicate biochar - Google Patents
Preparation and application of nano magnesium silicate biochar Download PDFInfo
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- CN113578266B CN113578266B CN202110897138.6A CN202110897138A CN113578266B CN 113578266 B CN113578266 B CN 113578266B CN 202110897138 A CN202110897138 A CN 202110897138A CN 113578266 B CN113578266 B CN 113578266B
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Abstract
The invention discloses a preparation and application of nano magnesium silicate biochar, which is prepared by washing, drying, crushing, sieving and drying collected forestry and agricultural residues to prepare biomass particles, soaking the biomass particles in a sodium metasilicate solution for a certain time to prepare silicon-carrying biomass particles, carbonizing the silicon-carrying biomass particles, sequentially adding absolute ethyl alcohol, deionized water, sodium acetate and magnesium chloride, and carrying out solvothermal reaction. The method utilizes agricultural and forestry wastes as raw materials to prepare the biochar, the raw materials are rich, the preparation is simple, the obtained nano magnesium silicate biochar has an obvious adsorption effect on the radioactive element uranium, and the nano magnesium silicate biochar can be used as an adsorbent for adsorption separation of the radioactive element uranium in spent fuel aqueous solution.
Description
Technical Field
The invention belongs to the field of carbon materials, and particularly relates to preparation and application of a nano magnesium silicate biochar adsorbent.
Background
Uranium (U) is an actinide belonging to the periodic table of elements, having an atomic number of 92, and is a natural radionuclide widely distributed in the earth's crust. The uranium is mainly composed of 238 U、 235 U、 234 U is composed of three isotopes, wherein 238 The abundance of U is maximum, it decays by releasing alpha rays, and the half-life is as long as 4.468X 10 9 And (5) year. Uranium is also the only naturally fissionable nuclide and is often used as fuel in nuclear power plants to produce nuclear energy. Nowadays, with the aggravation of energy crisis, the nuclear power industry is gradually favored by various countries, and the development of nuclear power becomes one of energy development strategies in China. With the development of nuclear power, how to develop and utilize uranium resources hasThe significance is important.
Nuclear power plant reactors produce spent fuel containing large amounts of incompletely reacted U and U fission products (e.g., tc). At present, the international method for treating the spent fuel mainly comprises direct treatment and post-treatment. The direct disposal means that the spent fuel is stored in special equipment after being cooled. The direct disposal method can not recycle a large amount of uranium in the spent fuel, wastes valuable uranium resources and increases the disposal volume of the nuclear waste. The post-treatment method is a treatment mode favored by the state nowadays, and the post-treatment method not only can recover precious resources in the nuclear waste, but also reduces the radiation of the nuclear waste. The radioactive property of the spent fuel without any treatment from the light water reactor can be reduced to the level of natural uranium ore after 13 ten thousand years, but if the actinides in the spent fuel can be removed, the standing time is reduced to 270 years, and the pressure and the hazard of the final disposal of nuclear waste are greatly reduced.
The PUREX post-treatment process is a common process for separating uranium from spent fuel at present, and the PUREX post-treatment process uses an organic solvent to contact with a spent nuclear fuel water solution, so that uranium or other ions are transferred to an organic phase, and the organic solvent is subjected to back extraction by using an acid solution to recover uranium and other resources. However, the spent fuel usually contains technetium with strong radioactivity, which causes the degradation of part of the organic extraction solvent, and the oxidation of the technetium causes the increase of the amount of the reducing agent used subsequently, so that the operation cost of the PUREX post-treatment process is increased.
The adsorption method is simple, convenient and quick, is suitable for recycling uranium from low-concentration uranium-containing wastewater, and is widely applied to nuclear wastewater treatment. Biochar has been widely studied as a material with a developed pore structure, a large specific surface area, abundant surface functional groups and low price. However, the original state biochar has the defects of small adsorption amount and poor selectivity. Therefore, the development of a novel biochar which is low in cost, efficient and feasible has great significance for selective adsorption separation of low-concentration U (VI) in radioactive wastewater.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a simple, feasible and low-cost preparation method of nano magnesium silicate biochar, agricultural and forestry waste is used as a raw material, the effect of treating waste by waste is achieved, and the prepared nano magnesium silicate biochar can be used as an adsorbent for selective adsorption separation of low-concentration U (VI) in radioactive wastewater.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of nano magnesium silicate biochar comprises the following steps:
1) And (3) granulating: washing, drying, crushing, screening and drying the collected agricultural and forestry waste to prepare biomass particles;
2) Carrying out silicon loading: dipping the biomass particles prepared in the step 1) in a sodium metasilicate solution for a certain time, and drying to prepare silicon-loaded biomass particles;
3) Carbonizing: carbonizing the silicon-carrying biomass particles prepared in the step 2) for a certain time, and cooling to room temperature to prepare silicon-carrying biochar particles;
4) Preparing nano magnesium silicate biochar: placing the silicon-loaded biochar particles prepared in the step 3) into an inner container of a hydrothermal kettle, sequentially adding absolute ethyl alcohol, deionized water, sodium acetate and magnesium chloride, and carrying out solvothermal reaction to obtain the nano magnesium silicate biochar.
The agricultural and forestry waste in the step 1) is one or more of rice hulls, sawdust, bamboo shoot shells, water hyacinth, corncobs and coconut shells.
The sieving in the step 1) is to sieve the mixture by a sieve with 20 to 100 meshes; the drying temperature is 60-110 ℃.
The concentration of the sodium metasilicate solution in the step 2) is 0.1-5 mol/L; the dipping temperature is 20-120 ℃, and the time is 1-24 h.
The carbonization temperature in the step 3) is 100-1000 ℃, and the carbonization time is 0.5-10 h.
In the step 4), 1-20 mL of absolute ethyl alcohol, 1-30 mL of deionized water, 0.1-1.0 g of sodium acetate and 0.1-3.0 g of magnesium chloride are added to every 1g of silicon-loaded biochar particles.
The temperature of the solvothermal reaction in the step 4) is 120-180 ℃, and the time is 4-8 h.
The nanometer magnesium silicate charcoal prepared by the methodThe specific surface area is 20-1000 m 2 The average pore diameter is 0.1-10 nm, wherein the particle diameter of the magnesium silicate nano-particles is 0.1-100 nm.
The obtained nano magnesium silicate biochar can be used as an adsorbent for adsorption separation of radioactive element uranium in spent fuel aqueous solution.
The invention has the beneficial effects and outstanding advantages that:
1. the raw material used by the invention is agricultural and forestry waste, the source is wide, the cost is low, and the U (VI) in the nano magnesium silicate biochar adsorption separation solution prepared by using the raw material can achieve the purpose of treating wastes with processes of wastes against one another.
2. The nano magnesium silicate charcoal prepared by the invention has the loaded nano magnesium silicate particles with shapes of linear or flower and the particle size of 0.1 to 100 nm.
3. The nano magnesium silicate biochar prepared by the invention has good separation and adsorption performance on U (VI) in wastewater, the removal rate is up to more than 90%, the maximum adsorption quantity can be 476 mg uranium per gram of adsorbent, and the effective separation of U (VI) in the solution can be realized.
4. The nano magnesium silicate charcoal prepared by the invention has good stability, and the removal rate can still be kept above 95% after multiple adsorption-desorption cycles.
Drawings
FIG. 1 shows the uranium removal rate of the nano magnesium silicate biochar after 6 times of adsorption-desorption cycles.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
A preparation method of nano magnesium silicate biochar comprises the following steps:
(1) Granulating: cleaning the collected sawdust, drying, crushing, sieving with a 60-mesh sieve, and drying at 70 ℃ to obtain sawdust particles;
(2) Carrying out silicon loading: taking a proper amount of sieved sawdust particles, and placing the sawdust particles in 50 mL of 1 mol/L Na 2 SiO 3 Solutions ofSoaking at 55 ℃ for 10 h, then filtering and separating, washing to be neutral, and drying to obtain silicon-carrying wood dust particles;
(3) Carbonizing: 1g of silicon-carrying wood dust particles are carbonized for 2 hours at 500 ℃ to prepare silicon-carrying biochar particles;
(4) Preparing nano magnesium silicate biochar: 1g of silicon-loaded biochar particles are taken and added with 1g of MgCl 2 3 mL of absolute ethyl alcohol, 20 mL of deionized water and 1g of sodium acetate are mixed, then transferred to a liner of a hydrothermal kettle, put into an oven for processing at 120 ℃ for 8 h, cooled to room temperature, and dried at 60 ℃ for 1 h to obtain the nano magnesium silicate biochar material with the surface area of 757 m 2 In terms of/g, the mean pore diameter is 2.1 nm.
Example 2
A preparation method of nano magnesium silicate biochar comprises the following steps:
(1) And (3) granulating: cleaning the collected sawdust, drying, crushing, sieving with a 50-mesh sieve, and drying at 80 ℃ to obtain sawdust particles;
(2) Carrying out silicon loading: taking a proper amount of sieved sawdust particles, and placing the sawdust particles in 100 mL of 5 mol/L Na 2 SiO 3 Soaking the silicon-carrying wood chips in the solution at 100 ℃ for 5 hours, filtering, separating, washing to be neutral, and drying to obtain silicon-carrying wood chip particles;
(3) Carbonizing: 2 g of silicon-carrying wood dust particles are carbonized for 1 hour at the temperature of 600 ℃ to prepare silicon-carrying biochar particles;
(4) Preparing nano magnesium silicate biochar: 1g of silicon-loaded biochar particles are taken, and 2 g of MgCl is added 2 5 mL of absolute ethyl alcohol, 20 mL of deionized water and 1g of sodium acetate are mixed, then the mixture is transferred to a hydrothermal kettle liner, the mixture is put into an oven for processing for 8 hours at 140 ℃, the mixture is cooled to room temperature and dried for 1 hour at 60 ℃, and the nano magnesium silicate biochar material with the surface area of 453 m is obtained 2 In terms of/g, the mean pore diameter is 15.3 nm.
Example 3
A preparation method of nano magnesium silicate biochar comprises the following steps:
(1) Granulating: cleaning the collected sawdust, drying, crushing, sieving with a 80-mesh sieve, and drying at 100 ℃ to obtain sawdust particles;
(2) Carrying out silicon loading:taking a proper amount of sieved sawdust particles, and placing the sawdust particles in 100 mL of 2 mol/L Na 2 SiO 3 Soaking in the solution at 80 ℃ for 4 h, filtering, separating, washing to neutrality, and drying to obtain silicon-carrying wood dust particles;
(3) Carbonizing: 2 g of silicon-carrying wood dust particles are carbonized for 1 hour at 800 ℃ to prepare silicon-carrying biochar particles;
(4) Preparing nano magnesium silicate biochar: 1g of silicon-loaded biochar particles are taken and added with 1g of MgCl 2 10 mL of absolute ethyl alcohol, 10 mL of deionized water and 0.2 g of sodium acetate are mixed, transferred to a liner of a hydrothermal kettle, put into an oven for processing for 8 h at 140 ℃, cooled to room temperature, dried for 1 h at 60 ℃ to obtain the nano magnesium silicate biochar material with the surface area of 867 m 2 In terms of/g, the mean pore diameter is 5.7 nm.
Example 4
A preparation method of nano magnesium silicate biochar comprises the following steps:
(1) And (3) granulating: cleaning the collected sawdust, drying, crushing, sieving with a 100-mesh sieve, and drying at 100 ℃ to obtain sawdust particles;
(2) Carrying out silicon loading: taking a proper amount of sieved sawdust particles, and placing the sawdust particles in 80 mL of 3 mol/L Na 2 SiO 3 Soaking the silicon-carrying wood chips in the solution at 120 ℃ for 1 h, then filtering and separating, washing to be neutral, and drying to obtain silicon-carrying wood chips;
(3) Carbonizing: 2 g of silicon-carrying wood dust particles are carbonized for 4 hours at 400 ℃ to prepare silicon-carrying biochar particles;
(4) Preparing nano magnesium silicate biochar: 1g of silicon-loaded biochar particles are taken, and 2 g of MgCl is added 2 Mixing 15 mL of absolute ethyl alcohol, 5 mL of deionized water and 1g of sodium acetate, transferring the mixture into a liner of a hydrothermal kettle, putting the mixture into an oven for processing for 8 h at 140 ℃, cooling to room temperature, and drying for 1 h at 60 ℃ to obtain the nano magnesium silicate biochar material with the surface area of 341 m 2 In terms of/g, the mean pore diameter is 8.6 nm.
Example 5
A preparation method of nano magnesium silicate biochar comprises the following steps:
(1) And (3) granulating: cleaning the collected sawdust, drying, crushing, sieving with a 80-mesh sieve, and drying at 80 ℃ to obtain sawdust particles;
(2) Carrying out silicon loading: taking a proper amount of the sieved sawdust particles, and placing the sawdust particles in 80 mL of 2 mol/L Na 2 SiO 3 Soaking in the solution at 60 ℃ for 10 h, then filtering and separating, washing to be neutral, and drying to obtain silicon-carrying wood dust particles;
(3) Carbonizing: 2 g of silicon-carrying wood dust particles are carbonized for 1 h at 900 ℃ to prepare silicon-carrying biochar particles;
(4) Preparing nano magnesium silicate biochar: 1g of silicon-loaded biochar particles are taken and added with 1g of MgCl 2 Mixing 8 mL of absolute ethyl alcohol, 22 mL of deionized water and 0.5 g of sodium acetate, transferring the mixture into a liner of a hydrothermal kettle, putting the mixture into an oven for processing for 4 h at 180 ℃, cooling to room temperature, and drying for 1 h at 60 ℃ to obtain the nano magnesium silicate biochar material. Surface area of 578 m 2 In terms of a/g, the mean pore diameter is 2.41 nm.
Comparative example
A preparation method of silicon-loaded biochar particles comprises the following steps:
(1) Granulating: cleaning the collected sawdust, drying, crushing, sieving with a 80-mesh sieve, and drying at 80 ℃ to obtain sawdust particles;
(2) Carrying out silicon loading: taking a proper amount of the sieved sawdust particles, and placing the sawdust particles in 80 mL of 2 mol/L Na 2 SiO 3 Soaking in the solution at 60 ℃ for 10 h, then filtering and separating, washing to be neutral, and drying to obtain silicon-carrying wood dust particles;
(3) Carbonizing: and (3) carbonizing 2 g of silicon-carrying wood dust particles at 900 ℃ for 1 h to obtain the silicon-carrying biochar particles.
1. The adsorbents prepared in examples 1 to 5 and comparative example were used for adsorption experiments of uranium-containing wastewater, respectively, the solid-to-liquid ratio of the adsorbent to the uranium-containing wastewater (50 mg/L) was 0.1 g/L, the pH of the solution was 5, and the adsorption experiments were performed at 25 ℃.
TABLE 1
Experimental results show that the nano magnesium silicate charcoal adsorbent prepared in example 2 has the best adsorption capacity for uranium, and the adsorption amount of the adsorbent reaches 476 mg/L. In addition, the adsorption capacity of the nano magnesium silicate biochar to uranium is far greater than that of silicon-loaded biochar particles under the same conditions.
2. The adsorption-desorption cycle experiment of the nano magnesium silicate biochar prepared in the example 2 is carried out, and the specific experimental method is as follows:
adsorption experiment: the solid-liquid ratio of the adsorbent to the uranium-containing wastewater (20 mg/L) is 0.1 g/L, the pH of the solution is 5, and an adsorption experiment is carried out at 25 ℃; and (3) placing the uranium-adsorbed nano magnesium silicate charcoal in an oven at 80 ℃ for 24 hours, and then using the charcoal for desorption experiments.
Desorption experiment: taking 0.5 mol/L sodium carbonate solution as a desorbent according to the mass-volume ratio of the desorbent to the uranium-adsorbed nano magnesium silicate biochar being 2 g/L, and carrying out a desorption experiment at 25 ℃; and washing the desorbed nano magnesium silicate biochar with deionized water to be neutral, putting the nano magnesium silicate biochar in an oven at 80 ℃ for 24 hours, and using the nano magnesium silicate biochar for a subsequent adsorption-desorption cycle experiment.
The above adsorption-desorption cycle experiment was repeated 6 times, and the results are shown in fig. 1.
As can be seen from FIG. 1, the nano magnesium silicate biochar prepared by the invention has good stability, and the removal rate can still be kept above 95% after multiple adsorption-desorption cycles.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A preparation method of nano magnesium silicate biochar for absorbing and separating radioactive element uranium in spent fuel aqueous solution is characterized by comprising the following steps: the method comprises the following steps:
1) Granulating: washing, drying, crushing, screening and drying the collected agricultural and forestry waste to prepare biomass particles;
2) Carrying out silicon loading: soaking the biomass particles prepared in the step 1) in a sodium metasilicate solution for a certain time, and drying to prepare silicon-loaded biomass particles;
3) Carbonizing: carbonizing the silicon-carrying biomass particles prepared in the step 2) for a certain time, and cooling to room temperature to prepare silicon-carrying biochar particles;
4) Preparing nano magnesium silicate biochar: placing the silicon-loaded biochar particles prepared in the step 3) into a hydrothermal kettle inner container, sequentially adding absolute ethyl alcohol, deionized water, sodium acetate and magnesium chloride, and performing solvothermal reaction to obtain nano magnesium silicate biochar;
in the step 4), 1-20 mL of absolute ethyl alcohol, 1-30 mL of deionized water, 0.1-1.0 g of sodium acetate and 0.1-3.0 g of magnesium chloride are added into every 1g of silicon-carrying biochar particles.
2. The method for preparing nano magnesium silicate biochar according to claim 1, characterized in that: the agricultural and forestry waste in the step 1) is one or more of rice hulls, sawdust, bamboo shoot shells, water hyacinth, corncobs and coconut shells.
3. The method for preparing nano magnesium silicate biochar according to claim 1, which is characterized in that: the sieving in the step 1) is to sieve the mixture by a sieve of 20 to 100 meshes; the drying temperature is 60-110 ℃.
4. The method for preparing nano magnesium silicate biochar according to claim 1, which is characterized in that: the concentration of the sodium metasilicate solution in the step 2) is 0.1-5 mol/L; the dipping temperature is 20-120 ℃, and the time is 1-24 h.
5. The method for preparing nano magnesium silicate biochar according to claim 1, which is characterized in that: the carbonization temperature in the step 3) is 100-1000 ℃, and the carbonization time is 0.5-10 h.
6. The method for preparing nano magnesium silicate biochar according to claim 1, which is characterized in that: the temperature of the solvothermal reaction in the step 4) is 120-180 ℃, and the time is 4-12h.
7. A nano magnesium silicate biochar prepared by the method of any one of claims 1 to 6, wherein: the specific surface area is 20-1000 m 2 The average pore diameter is 0.1-10 nm, wherein the particle diameter of the magnesium silicate nano-particles is 0.1-100 nm.
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