CN109364872B - Preparation method of sulfur-based covering type alkaline ash adsorbent - Google Patents
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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
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- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/006—Radioactive compounds
Abstract
The invention discloses a preparation method of a sulfur-based covering type alkaline ash adsorbent, which comprises the following steps of (1) weighing fly ash, ground blast furnace slag, metakaolin and sodium hydroxide, mixing and stirring to obtain ash powder, dissolving the ash powder in water, and stirring to obtain ash slurry; (2) placing the ash slurry in an oven, drying, transferring to a muffle furnace, activating at a constant temperature, and cooling to room temperature to obtain alkaline ash; (3) weighing elemental sulfur and alkaline ash, mixing and grinding to obtain sulfur-doped alkaline ash; (4) and (3) placing the sulfur-doped alkaline ash in a vacuum tank, vacuumizing, sealing the vacuum tank, standing, placing in a muffle furnace, heating at 200-300 ℃ for 9-12 h, and cooling to room temperature to obtain the sulfur-based covering type alkaline ash adsorbent. The preparation method is simple, and the raw materials are cheap; the adsorbent can realize the high-efficiency removal of cesium ions in a water body containing various high-concentration competitive cations in coexistence; the adsorbent has strong stability and acid resistance.
Description
Technical Field
The invention relates to a preparation method of a radioactive cesium ion adsorbent in nuclear power generation, in particular to a preparation method of a sulfur-based covering type alkaline ash adsorbent.
Background
The operation of a nuclear power plant can generate a large amount of radioactive wastewater, the radioactive wastewater is taken as cesium ions which are one of radioactive elements, the cesium ions can be rapidly diffused and migrated in a water environment due to high solubility, and the cesium ions and various competitive ions (such as sodium, potassium, magnesium, aluminum, manganese and the like) can commonly coexist in a polluted water body, so that higher requirements are provided for the adsorption specificity and the adsorption capacity of an adsorption material for treating the cesium ions.
Inorganic ion exchange materials are widely used for adsorbing and capturing cesium ions due to good stability and corrosion resistance, but most of the ion exchange materials show low cesium ion exchange selectivity and are sensitive to other competitive ions existing in water. In order to improve the selective adsorption of cesium ions, other new adsorption materials such as titanosilicate, vanadosilicate, metal sulfide, metal hexacyanoferrate and the like have been developed, and particularly, crystalline titanosilicate has become a commercial ultrahigh-selectivity ion exchange material. However, although these new adsorbents are superior in performance, they are expensive and complicated in synthesis process compared to conventional adsorbents.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems, the invention aims to provide a preparation method for preparing a sulfur-based covering type alkaline ash adsorbent, the preparation method is simple, the cost of raw materials is low, and the prepared adsorbent has strong stability and high-efficiency and specific adsorption characteristics on cesium ions.
The technical scheme is as follows: in order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows: a preparation method of a sulfur-based covering type alkaline ash adsorbent comprises the following steps:
(1) preparing the ash slurry: respectively weighing fly ash, ground blast furnace slag, metakaolin and sodium hydroxide, mixing and stirring to obtain ash powder, dissolving the ash powder in water, and stirring to obtain ash slurry;
(2) preparing alkaline ash: placing the ash slurry in an oven to be dried to constant weight, then transferring to a muffle furnace for constant temperature activation, and cooling to room temperature to obtain alkaline ash;
(3) preparing sulfur-doped alkaline ash: respectively weighing elemental sulfur and alkaline ash, mixing and grinding to obtain sulfur-doped alkaline ash;
(4) preparing a sulfur-based covering type alkaline ash adsorbent: and (2) placing the sulfur-doped alkaline ash in a vacuum tank, vacuumizing, sealing the vacuum tank, standing, then placing the vacuum tank in a muffle furnace, heating for 9-12 hours at 200-300 ℃, completing high-temperature sublimation of elemental sulfur, and cooling to room temperature to obtain the sulfur-based coverage type alkaline ash adsorbent.
Preferably, in the step (1), the mass ratio of the fly ash to the ground blast furnace slag to the metakaolin is 8:1: 1-5: 2.5:2.5, and the mass ratio of the sodium hydroxide to the total mass of the fly ash to the ground blast furnace slag to the metakaolin is 1-2: 20; the solid-liquid ratio of the ash powder to water is 1g: 1-2.5 mL, and the mixing and stirring time of the ash powder and water is 0.5-2 h.
Preferably, the drying temperature of the drying oven in the step (2) is 100-150 ℃; the activation temperature in a muffle furnace is 250-350 ℃, and the activation time is 1-2 h.
Preferably, the mass ratio of the elemental sulfur to the alkaline ash in the step (3) is 1-2.5: 10, and the grinding time of the elemental sulfur and the alkaline ash in a grinding machine is 1-2 h.
Preferably, the vacuum degree in the step (4) is-0.04 to-0.08 MPa, and the standing time of the sealed vacuum tank is 5 to 10 min.
The working principle is as follows: based on the lewis acid-base (HSAB) theory, hard lewis acids have a high affinity with hard lewis bases, while soft lewis acids exhibit a high affinity with soft lewis bases. Hard lewis acids and bases specifically refer to acidic and basic substances with small atomic radii, high nuclear charges, and low polarizability, whereas soft lewis acids and bases have properties opposite to those of hard lewis acids and bases. In the waste stream, the cesium ions are soft lewis acids compared to other coexisting competing cations. Elemental sulfur, as a soft lewis base, selectively adsorbs cesium ions when treating contaminated waste streams containing multiple competing cations and cesium ions at the same time.
The fly ash has strong cation exchange capacity, and the microstructure of the fly ash comprises SiO4Tetrahedron and AlO6The two-dimensional layered structure composed of octahedrons also comprises a three-dimensional unit cell structure, a plurality of exchangeable cations exist between negative electricity unit layers of the structure, and cesium is adsorbed in an aqueous environment through a screening effect and an ion exchange path. Compared with fly ash, the blast furnace slag and metakaolin have different composition crystal structures and contain cations with different amounts and different valence states. The mixed ash is chosen as a substrate, which facilitates the complementation between materials in terms of structure and ionic content. Through the soaking of sodium hydroxide and the alkali activation in high temperature environment, the crystal structure fusion and geological polymerization among the fly ash, blast furnace slag and metakaolin are promoted to generate the excitation powderThe ion exchange activity of the coal ash, blast furnace slag and metakaolin, and the stability of the alkaline ash adsorbent. Meanwhile, under an acidic environment, the fly ash, the blast furnace slag and the metakaolin can absorb a large amount of H+This improves the acid resistance of the sulfur-coated basic ash adsorbent.
The sulfur-based covering type alkaline ash adsorbent realizes the high-efficiency removal of cesium ions in water through adsorption in multiple ways: the primary transfer of cesium ions from a water body to the surface of an adsorbent is realized through a Lewis acid-alkali reaction path and an electrostatic adsorption effect; further migration of cesium ions into the adsorbent structure is realized through ion exchange effect and molecular sieve effect; the solidification and stable sealing of cesium ions in the adsorbent are realized through hydration reaction and geological polymerization.
Has the advantages that: the preparation method of the adsorbent is simple, the related raw materials are cheap, and the preparation cost of the adsorbent is low; through elemental sulfur sublimation covering and alkali-activated ash, the specificity of an ion exchange material for cesium ion adsorption can be improved, the advantage of alkaline ash ion exchange is retained, the stability and the acid resistance of an adsorbent can be improved, and the cesium ions can be efficiently removed from a water body with pH of 3-12 and coexistence of various high-concentration competitive cations; the adsorbent has low chemical loss in the adsorption and recovery process.
Drawings
Fig. 1 is a flow chart of preparation of a sulfur-based covering type alkaline ash adsorbent and a process for removing cesium ions in a water body by using the sulfur-based covering type alkaline ash adsorbent.
Detailed Description
The invention is further described below with reference to the figures and examples.
Example 1
The mass ratio of the fly ash, the ground blast furnace slag and the metakaolin has the following influence on the removal rate of cesium ions in the water body:
as shown in fig. 1, the preparation process of the sulfur-based coating type alkaline ash adsorbent specifically comprises the following steps:
preparing the ash slurry: respectively weighing fly ash, ground blast furnace slag, metakaolin and sodium hydroxide, mixing and stirring to prepare ash powder. Wherein the mass ratio of the fly ash to the ground blast furnace slag to the metakaolin is 8:1:1, 7:1:2, 7:2:1, 7:1.5:1.5, 6:2:2 and 5:2.5:2.5 respectively, and the mass ratio of the sodium hydroxide to the total mass of the fly ash to the ground blast furnace slag to the metakaolin is 1: 20. Mixing the ash powder with distilled water at room temperature according to a solid-to-liquid ratio of 1g:1mL, and stirring for 0.5h to obtain ash slurry. Since the blast furnace slag has too large primary particles to affect its own reactivity, it is necessary to pulverize the blast furnace slag before use.
Preparing alkaline ash: and (3) placing the five ash slurry parts into a drying oven, drying at 100 ℃ to constant weight, transferring the dried ash into a muffle furnace, activating for 1h at the constant temperature of 250 ℃, and cooling to room temperature to obtain the alkaline ash.
Preparing sulfur-doped alkaline ash: weighing elemental sulfur powder and the alkaline ash respectively according to the mass ratio of 1:10, and placing the elemental sulfur powder and the alkaline ash into a grinding machine for grinding for 1h to obtain sulfur-doped alkaline ash.
Preparing a sulfur-based covering type alkaline ash adsorbent: and (2) placing the sulfur-doped alkaline ash in a glass vacuum tank, vacuumizing to the relative vacuum degree of-0.08 MPa, sealing the vacuum tank, standing for 5min, placing the vacuum tank in a muffle furnace, heating at 200 ℃ for 9h, sublimating elemental sulfur, and cooling to room temperature to obtain the sulfur-based covering type alkaline ash adsorbent.
Treating water containing cesium ions and various competitive cations: adding sulfur-based covering type alkaline ash adsorbent powder into the mixture according to the solid-to-liquid ratio of 1g to 1L, wherein the sulfur-based covering type alkaline ash adsorbent powder contains 5mg/L Cs+、100mg/L Na+、100mg/L K+、100mg/L Mg2+、100mg/L Ca2 +、100mg/L Al3+And stirring at 120rpm for 10min in a water body with pH of 3. Wherein, the pH value of the water body is titrated and adjusted by sulfuric acid and sodium hydroxide solution with the concentration of 0.5 moL/L. The concentration of cesium in the water body was determined according to the procedure specified in Standard underground Water quality inspection method for rubidium and cesium by flame emission Spectroscopy (DZ/T0064.36-93). The removal efficiency of the cesium ions in the water body is calculated according to the percentage ratio of the difference value of the concentration of the cesium ions in the water body before the experiment and the concentration of the cesium ions in the water body after the experiment to the concentration of the cesium ions in the liquid before the experiment, and the test resultsThe results are shown in Table 1.
TABLE 1 influence of mass ratio of fly ash, ground blast furnace slag and metakaolin on removal rate of cesium ions in water
As can be seen from the results in Table 1, the removal rate of cesium ions in the water body is greater than 97% after the sulfur-based covering type alkaline ash adsorbent powder is added into the water body. When the mass ratio of the fly ash to the ground blast furnace slag to the metakaolin is 7:1:2, the removal rate of cesium in the water body is the highest and is 99.4% (+ -0.3%). The sulfur-based covering type alkaline ash adsorbent has obvious specific adsorption on cesium ions, and high-concentration Na in water+、K+、Mg2+、Ca2+、Al3+Competitive ions had no significant effect on the cesium adsorption results.
Example 2
The influence of the mass ratio of the sodium hydroxide to the total mass of the fly ash, the ground blast furnace slag and the metakaolin on the removal rate of the cesium ions is as follows:
the preparation process is the same as that of example 1, and is different from that of example 1:
preparing the ash slurry: the mass ratio of the fly ash to the ground blast furnace slag to the metakaolin is 7:1:2, and the mass ratio of the sodium hydroxide to the fly ash to the ground blast furnace slag to the metakaolin is 1:20, 1.25:20, 1.5:20, 1.75:20 and 2: 20. The solid-liquid ratio of the ash powder to the distilled water is 1g:1.5mL, and the mixture is stirred for 1h to obtain ash slurry.
Preparing alkaline ash: and (3) drying the ash slurry in an oven at 125 ℃, activating for 1.5h in a muffle furnace at the constant temperature of 300 ℃, and cooling to room temperature to obtain alkaline ash.
Preparing sulfur-doped alkaline ash: the mass ratio of the elemental sulfur powder to the alkaline ash is 1.5:10, and the elemental sulfur powder and the alkaline ash are ground for 1.5h to obtain the sulfur-doped alkaline ash.
Preparing a sulfur-based covering type alkaline ash adsorbent: and (3) placing the sulfur-doped alkaline ash into a vacuum tank, vacuumizing to the relative vacuum degree of-0.06 MPa, sealing and standing for 7.5min, heating for 10h at 250 ℃ in a muffle furnace, and cooling to room temperature to obtain the sulfur-based covering type alkaline ash adsorbent.
Treating water containing cesium ions and various competitive cations: adding sulfur-based covering type alkaline ash adsorbent powder into the mixture according to the solid-to-liquid ratio of 1g to 1L, wherein the sulfur-based covering type alkaline ash adsorbent powder contains 10mg/L Cs+、100mg/L Na+、100mg/L K+、100mg/L Mg2+、100mg/L Ca2+、100mg/L Al3+And stirring at 120rpm for 10min in a water body with pH of 6. The concentration of cesium ions in the water was measured and the test results are shown in table 2.
TABLE 2 influence of the mass ratio of sodium hydroxide to the total mass of fly ash, ground blast furnace slag, metakaolin on the removal rate of cesium ions
As can be seen from the results in Table 2, the removal rate of cesium ions in the water body is greater than 96% after the sulfur-based covering type alkaline ash adsorbent powder is added into the water body. The removal rate of cesium ions in the water body increases with the increase of the mass ratio of the total mass of the sodium hydroxide to the total mass of the fly ash, the ground blast furnace slag and the metakaolin. When the mass ratio of the sodium hydroxide to the total mass of the fly ash, the ground blast furnace slag and the metakaolin is 1:10, the removal rate of cesium in the water body is the highest and is 99.6% (+ -0.3%). The sulfur-based covering type alkaline ash adsorbent has obvious specific adsorption on cesium ions, and high-concentration Na in water+、K+、Mg2+、Ca2+、Al3+Competitive ions had no significant effect on the cesium adsorption results.
Example 3
The mass ratio of elemental sulfur and alkaline ash to the cesium ion removal rate:
the preparation process is the same as that of example 1, and is different from that of example 1:
preparing the ash slurry: the mass ratio of the fly ash to the ground blast furnace slag to the metakaolin is 7:1:2, and the mass ratio of the sodium hydroxide to the total mass of the fly ash to the ground blast furnace slag to the metakaolin is 1: 10. And stirring the ash powder and distilled water at a solid-to-liquid ratio of 1g to 2mL for 1.5h to obtain ash slurry.
Preparing alkaline ash: and (3) drying the ash slurry in an oven at 150 ℃, activating for 2 hours in a muffle furnace at the constant temperature of 350 ℃, and cooling to room temperature to obtain alkaline ash.
Preparing sulfur-doped alkaline ash: the mass ratio of the elemental sulfur powder to the alkaline ash is 1:10, 1.5:10, 1.75:10, 2:10 and 2.5:10 respectively, and the elemental sulfur powder and the alkaline ash are ground for 2 hours to obtain the sulfur-doped alkaline ash.
Preparing a sulfur-based covering type alkaline ash adsorbent: and (3) placing the sulfur-doped alkaline ash into a vacuum tank, vacuumizing to the relative vacuum degree of-0.04 MPa, sealing and standing for 10min, heating for 11h at 300 ℃ in a muffle furnace, and cooling to room temperature to obtain the sulfur-based covering type alkaline ash adsorbent.
Treating water containing cesium ions and various competitive cations: adding sulfur-based covering type alkaline ash adsorbent powder into the mixture according to the solid-to-liquid ratio of 1g to 1L, wherein the sulfur-based covering type alkaline ash adsorbent powder contains 15mg/LCs+、100mg/LNa+、100mg/LK+、100mg/LMg2+、100mg/LCa2+、100mg/L Al3+And stirring at 120rpm for 10min in a water body with pH of 9. The concentration of cesium ions in the water was measured and the test results are shown in table 3.
TABLE 3 influence of mass ratio of elemental sulfur and basic ash on cesium ion removal rate
| Elemental sulfur: basic ash (mass ratio) | Removal rate of cesium ions | Percentage of error |
| 1:10 | 96.3％ | ±0.3％ |
| 1.5:10 | 98.3％ | ±0.3％ |
| 1.75:10 | 99.5％ | ±0.3％ |
| 2:10 | 99.1％ | ±0.2％ |
| 2.5:10 | 98.2％ | ±0.2％ |
As can be seen from the results in Table 3, the removal rate of cesium ions in the water body is greater than 96% after the sulfur-based covering type alkaline ash adsorbent powder is added into the water body. When the mass ratio of the elemental sulfur powder to the alkaline ash is 1.75:10, the removal rate of cesium in the water body is the highest and is 99.5% (+/-0.3%). The sulfur-based covering type alkaline ash adsorbent has obvious specific adsorption on cesium ions, and high-concentration Na in water+、K+、Mg2+、Ca2+、Al3+Competitive ions had no significant effect on the cesium adsorption results.
Example 4
Effect of competitive cation concentration on cesium ion removal rate:
the preparation process is the same as that of example 1, and is different from that of example 1:
preparing the ash slurry: the mass ratio of the fly ash to the ground blast furnace slag to the metakaolin is 7:1:2, and the mass ratio of the sodium hydroxide to the total mass of the fly ash to the ground blast furnace slag to the metakaolin is 1: 10. And stirring the ash powder and distilled water for 2 hours to obtain ash slurry, wherein the solid-to-liquid ratio of the ash powder to the distilled water is 1g:2.5 mL.
Preparing alkaline ash: and (3) drying the ash slurry in an oven at 150 ℃, activating for 2 hours in a muffle furnace at the constant temperature of 350 ℃, and cooling to room temperature to obtain alkaline ash.
Preparing sulfur-doped alkaline ash: and grinding the elemental sulfur powder and the alkaline ash for 2 hours to obtain the sulfur-doped alkaline ash, wherein the mass ratio of the elemental sulfur powder to the alkaline ash is 1.75: 10.
Preparing a sulfur-based covering type alkaline ash adsorbent: and (3) placing the sulfur-doped alkaline ash into a vacuum tank, vacuumizing to the relative vacuum degree of-0.04 MPa, sealing and standing for 10min, heating for 12h at 300 ℃ in a muffle furnace, and cooling to room temperature to obtain the sulfur-based covering type alkaline ash adsorbent.
Treating water containing cesium ions and various competitive cations: respectively adding sulfur-based covering type alkaline ash adsorbent powder into a mixture containing 20mg/L Cs according to the solid-to-liquid ratio of 1g to 1L+、100mg/L Na+、100mg/LK+、100mg/L Mg2+、100mg/L Ca2+、100mg/L Al3+；20mg/L Cs+、200mg/L Na+、200mg/L K+、200mg/L Mg2+、200mg/L Ca2+、200mg/L Al3+；20mg/L Cs+、300mg/L Na+、300mg/L K+、300mg/L Mg2+、300mg/L Ca2+、300mg/L Al3+Three groups of water bodies with different competitive cation concentrations and pH values of 12 are stirred for 10min at 120 rpm. The concentration of cesium ions in the water was measured and the test results are shown in table 4.
TABLE 4 Effect of competitive cation concentration on Cesium ion removal Rate
From the results in table 4, it can be seen that the removal rate of cesium ions in three water bodies is greater than 95% after the sulfur-based covering type alkaline ash adsorbent powder is added into the water body. The increase in the concentration of competing cations slightly reduces the rate of removal of cesium ions from the water body. When the water body contains 100mg/L of Na+、100mg/L K+、100mg/L Mg2+、100mg/L Ca2+、100mg/L Al3+At times, cesium removal was up to 98.6% (± 0.2%). The sulfur-based covering type alkaline ash adsorbent has obvious specific adsorption on cesium ions.
Claims (6)
1. The preparation method of the sulfur-based covering type alkaline ash adsorbent is characterized by comprising the following steps:
(1) preparing the ash slurry: respectively weighing fly ash, ground blast furnace slag, metakaolin and sodium hydroxide, mixing and stirring to obtain ash powder, dissolving the ash powder in water, and stirring to obtain ash slurry;
(2) preparing alkaline ash: placing the ash slurry in an oven to be dried to constant weight, then transferring to a muffle furnace for constant temperature activation, and cooling to room temperature to obtain alkaline ash;
(3) preparing sulfur-doped alkaline ash: respectively weighing elemental sulfur and alkaline ash, mixing and grinding to obtain sulfur-doped alkaline ash;
(4) preparing a sulfur-based covering type alkaline ash adsorbent: placing the sulfur-doped alkaline ash in a vacuum tank, vacuumizing, sealing the vacuum tank, standing, placing the vacuum tank in a muffle furnace, heating at 200-300 ℃ for 9-12 h, and cooling to room temperature to obtain a sulfur-based covering type alkaline ash adsorbent;
wherein the activation temperature in the step (2) is 250-350 ℃, and the activation time is 1-2 h; the mass ratio of the elemental sulfur to the alkaline ash in the step (3) is 1-2.5: 10.
2. The preparation method of the sulfur-based covering type basic ash adsorbent according to claim 1, wherein the mass ratio of the fly ash, the ground blast furnace slag and the metakaolin in the step (1) is 8:1:1 to 5:2.5:2.5, and the mass ratio of the sodium hydroxide to the total mass of the fly ash, the ground blast furnace slag and the metakaolin is 1 to 2: 20; the solid-liquid ratio of the ash powder to water is 1g: 1-2.5 mL.
3. The preparation method of the sulfur-based covering type basic ash adsorbent according to claim 1, wherein the mixing and stirring time of the ash powder and water in the step (1) is 0.5-2 h.
4. The method for preparing the sulfur-based coated basic ash adsorbent according to claim 1, wherein the drying temperature of the oven in the step (2) is 100-150 ℃.
5. The method for preparing the basic ash adsorbent according to claim 1, wherein the grinding time in the step (3) is 1-2 h.
6. The method for preparing the basic covering type ash adsorbent according to claim 1, wherein the vacuum degree in the step (4) is-0.04 to-0.08 MPa, and the standing time of the sealed vacuum tank is 5 to 10 min.
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| CN105621907A (en) * | 2016-01-18 | 2016-06-01 | 桂林电子科技大学 | Calcium-base geopolymer and preparation method thereof |
| CN107377010A (en) * | 2017-06-28 | 2017-11-24 | 安阳师范学院 | Novel microporous chalcogenide, its preparation method and application |
| CN107973559A (en) * | 2017-11-22 | 2018-05-01 | 广西大学 | The preparation method and applications of porous geological polymer microballoon |
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| JPS58210846A (en) * | 1982-06-02 | 1983-12-08 | Nippon Jiryoku Senko Kk | Method for producing moisture absorbent and adsorbent from slag or slag and coal ash, shale or calcium silicate |
| CN105621907A (en) * | 2016-01-18 | 2016-06-01 | 桂林电子科技大学 | Calcium-base geopolymer and preparation method thereof |
| CN107377010A (en) * | 2017-06-28 | 2017-11-24 | 安阳师范学院 | Novel microporous chalcogenide, its preparation method and application |
| CN107973559A (en) * | 2017-11-22 | 2018-05-01 | 广西大学 | The preparation method and applications of porous geological polymer microballoon |
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