CN110237806B - Cu-Attapulgite-NH2Preparation method of composite material and application of composite material in adsorption of iodine ions in radioactive water - Google Patents
Cu-Attapulgite-NH2Preparation method of composite material and application of composite material in adsorption of iodine ions in radioactive water Download PDFInfo
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- CN110237806B CN110237806B CN201910431875.XA CN201910431875A CN110237806B CN 110237806 B CN110237806 B CN 110237806B CN 201910431875 A CN201910431875 A CN 201910431875A CN 110237806 B CN110237806 B CN 110237806B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- 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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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention relates to the technical field of sewage purification treatment, and discloses Cu-attapulgite-NH for iodine ion adsorption2The preparation method of the composite material and the application of the composite material in absorbing iodide ions in radioactive water comprise the following steps: s1: dispersing acidified attapulgite clay in a copper nitrate solution, stirring and soaking for 24 hours at 40 ℃, centrifuging, washing with water, drying, dispersing in an organic solvent-water mixed solution, adding formic acid and ammonia water, and performing hydrothermal reaction to prepare a Cu-attapulgite material; s2: dispersing the Cu-attapulgite material into an aqueous solution, adding dioctadecyl dimethyl ammonium bromide, fully stirring, and carrying out hydrothermal reaction to prepare Cu-attapulgite-NH2A composite material. Compared with the prior art, the invention improves the adsorption capacity and selectivity of the existing copper-based adsorbent, and provides technical reference for removing radioactive iodine in wastewater.
Description
Technical Field
The invention relates to the technical field of sewage purification treatment, and particularly relates to Cu-attapulgite-NH2A preparation method of the composite material and application thereof in absorbing iodine ions in radioactive water.
Background
With the vigorous development of Chinese economy and the increasingly prominent environmental problems, the nuclear power industry becomes an important development strategy of China, and the total amount of nuclear power operation and building machines in China is expected to reach 88 GW in 2020. Effectively solving the problem of radiation pollution and having important significance on the safe use of nuclear energy. Radioactive iodine is commonly used as an indicator for monitoring breakage of nuclear fuel element cladding and as a signal nuclide for environmental monitoring after nuclear explosion, and is one of the inevitable products of nuclear fission. Therefore, the efficient removal of liquid-phase radioactive iodine is a key scientific problem to be solved for the safe utilization of nuclear power.
The technology such as chemical precipitation, porous material adsorption, ion exchange, membrane separation and the like can be used for removing the liquid-phase radioactive iodine. The metal materials used for chemical precipitation are expensive and easily cause secondary pollution of heavy metals. The selective adsorption efficiency of the porous material in a complex environment is difficult to guarantee. The ion exchange technology is also prone to secondary pollution due to the use of organic or inorganic solvents. Membrane separation techniques have good removal efficiency but are expensive to operate.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides Cu-attapulgite-NH2The preparation method of the composite material and the application of the composite material in adsorption of iodine ions in radioactive water physically adsorb liquid-phase radioactive pollutants by utilizing the charge characteristics of the surface of the composite material, and selectively adsorb the radioactive iodine by utilizing Cu, so that the iodine adsorption capacity and selectivity are improved compared with those of the traditional copper-based adsorbent, and a technical reference is provided for removal of the radioactive iodine in wastewater.
The technical scheme is as follows: the invention provides Cu-attapulgite-NH2The preparation method of the composite material comprises the following steps: s1: dispersing acidified attapulgite clay in a copper nitrate solution, stirring and soaking for 24 hours at 40 ℃, centrifuging, washing with water, drying, dispersing in an organic solvent-water mixed solution, adding formic acid and ammonia water, and performing hydrothermal reaction to prepare a Cu-attapulgite material; s2: dispersing the Cu-attapulgite material into an aqueous solution, adding dioctadecyl dimethyl ammonium bromide, fully stirring, and carrying out hydrothermal reaction to prepare Cu-attapulgite-NH2A composite material.
Preferably, in the S1, the mass ratio of the acidified attapulgite clay, the copper nitrate solution, the formic acid and the ammonia water is 1: 0.01-0.10: 0.05-3.0: 1.0 to 8.0.
Preferably, in the step S1, the temperature of the hydrothermal reaction is 150 ℃ and the reaction time is 2 h.
Preferably, in the S2, the mass ratio of the Cu-attapulgite material to the dioctadecyl dimethyl ammonium bromide is 1: 1 to 10.
Preferably, in the step S2, the temperature of the hydrothermal reaction is 120 ℃ and the reaction time is 2 h.
Preferably, in the S1, the preparation method of the acidified attapulgite clay is as follows:
preferably, the acidified attapulgite is prepared by dispersing attapulgite clay in deionized water, stirring, centrifuging to remove impurities, soaking in dilute hydrochloric acid, stirring and dispersing; and washing and freeze-drying for later use.
Preferably, in S1, the organic solvent-water mixed solution is an ethanol-water mixed solution with a mass fraction of 60%.
The invention also provides Cu-attapulgite-NH2The application of the composite material in absorbing iodine ions in radioactive water.
Preferably, the concentration of iodide ions in the radioactive water is 0.1 to 1.0 mM; the Cu-attapulgite-NH2The amount of the composite material put in the radioactive water is 0.5-2 g.L－1。
Preferably, the Cu-attapulgite-NH2The temperature of the composite material in the radioactive water body is 25-50 ℃, and the adsorption time is 0.5-24 h.
Has the advantages that: the method takes the attapulgite mineral with good stability, low price and large specific surface area as the matrix material, loads the copper nitrate in the attapulgite pore canals by an impregnation method, disperses the copper nitrate in the solution, and reduces and regulates the Cu-attapulgite composite material by formic acid and ammonia water by a hydrothermal synthesis method. Dispersing the composite material in a solution, adding dioctadecyl dimethyl ammonium bromide surfactant to regulate the surface charge of the attapulgite, and preparing the Cu-attapulgite through hydrothermal reactionAttapulgite-NH2A composite material.
The prepared Cu-attapulgite-NH2The composite material is used for adsorbing iodine ions in radioactive water, low-concentration iodine ions in solution are enriched by virtue of the positive charge characteristic of the surface of the attapulgite modified by amino (the attapulgite originally has negative charges, and the surface of the attapulgite is positively charged after the amino is modified, so that the adsorption of negative ions and iodine ions is facilitated), and then Cu in the composite material is reacted with a CuO compact layer on the surface to generate Cu2And reacting the O with iodide ions to generate cuprous iodide. In the adsorption process, due to the synergistic effect of physical adsorption and chemical adsorption, the Cu-attapulgite-NH2Compared with the traditional copper-based adsorbent, the composite material has higher adsorption capacity.
Compared with the prior art, its obvious advantage lies in: (1) the method adopts a simple hydrothermal synthesis method, has simple process, short synthesis time, cheap and easily obtained raw materials and no toxicity; (2) the synthesized Cu is positioned in the pore canal of the attapulgite, so that the falling of the Cu in the adsorption process is avoided; (3) the adsorbent has low price and is beneficial to practical application.
Drawings
FIG. 1 shows Cu-Attapulgite-NH prepared in embodiment 12SEM scanning electron microscope image of the composite material;
FIG. 2 shows Cu-Attapulgite-NH prepared in embodiment 12Composite adsorption performance curve diagram;
FIG. 3 shows Cu-Attapulgite-NH prepared in embodiment 12SEM scanning electron microscope image of the composite material;
FIG. 4 shows Cu-Attapulgite-NH prepared in embodiment 12Composite adsorption performance curve diagram;
FIG. 5 shows Cu-Attapulgite-NH prepared in embodiment 12SEM scanning electron microscope image of the composite material;
FIG. 6 shows Cu-Attapulgite-NH prepared in embodiment 12Graph of adsorption performance of the composite material.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
the present embodiment provides a Cu-attapulgite-NH2The preparation method of the composite material comprises the following steps:
preparing acidified attapulgite clay: dispersing attapulgite clay in deionized water, stirring, centrifuging to remove impurities, soaking in dilute hydrochloric acid, stirring, and dispersing to obtain acidified attapulgite; and washing and freeze-drying for later use.
Preparing a Cu-attapulgite material: dispersing 1 g of the purified acidified attapulgite material in 40 mL of 0.1M copper nitrate solution, stirring and soaking at 40 ℃ for 24h, centrifuging, washing with water for three times, and drying at 100 ℃. And transferring the mixture to a hydrothermal reaction kettle, dispersing the mixture in a 60% ethanol-water mixed solution, adding 2 mL of formic acid and 4 mL of ammonia water, and carrying out hydrothermal reaction at 150 ℃ for 2 h to prepare the Cu-attapulgite material.
Cu-Attapulgite-NH2Preparing a composite material: dispersing 1 g of the Cu-attapulgite material in 40 mL of aqueous solution, adding 4 g of dioctadecyl dimethyl ammonium bromide, fully stirring, transferring to a hydrothermal reaction kettle, and carrying out hydrothermal reaction at 120 ℃ for 2 h to obtain Cu-attapulgite-NH2A composite material.
Preparing the obtained Cu-attapulgite-NH2SEM of the composite material is shown in FIG. 1. Therefore, the prepared composite material can keep the original rod-shaped structure of the attapulgite.
Mixing 50 mg of the above prepared Cu-attapulgite-NH2And adding the composite material into 50 mL of a 1.0 mM radioactive iodide ion simulating solution, adsorbing for 30 min at normal temperature, filtering, and detecting the concentration of residual iodide ions in the solution.
As shown in the adsorption result of FIG. 2, Cu-attapulgite-NH2The composite material reaches adsorption balance within 10 h, the adsorption efficiency can reach 75%, and the adsorption capacity reaches 0.75 mmol/g.
Embodiment 2:
the present embodiment provides a Cu-attapulgite-NH2The preparation method of the composite material comprises the following steps:
preparing acidified attapulgite: is the same as embodiment 1, and will not be described herein.
Preparing a Cu-attapulgite material: dispersing 1 g of the purified acidified attapulgite material in 40 mL of 0.01M copper nitrate solution, stirring and soaking at 40 ℃ for 24h, centrifuging, washing with water for three times, and drying at 100 ℃. And transferring the mixture to a hydrothermal reaction kettle, dispersing the mixture in a 60% ethanol-water mixed solution, adding 0.05 mL of formic acid and 1 mL of ammonia water, and carrying out hydrothermal reaction at 150 ℃ for 2 h to prepare the Cu-attapulgite material.
Cu-Attapulgite-NH2Preparing a composite material: dispersing 1 g of the Cu-attapulgite material in 40 mL of aqueous solution, adding 2g of dioctadecyl dimethyl ammonium bromide, fully stirring, transferring to a hydrothermal reaction kettle, and carrying out hydrothermal reaction at 120 ℃ for 2 h to obtain Cu-attapulgite-NH2A composite material.
Preparing the obtained Cu-attapulgite-NH2SEM of the composite material is shown in FIG. 3. Therefore, the prepared composite material can keep the original rod-shaped structure of the attapulgite.
Mixing 50 mg of the above prepared Cu-attapulgite-NH2And adding the composite material into 20 mL of a 1.0 mM radioactive iodide ion simulating solution, adsorbing for 30 min at normal temperature, filtering, and detecting the concentration of residual iodide ions in the solution.
As shown in the adsorption result of FIG. 4, Cu-attapulgite-NH2The composite material reaches adsorption balance within 2 h, the adsorption efficiency can reach 60 percent, and the adsorption capacity reaches 0.24 mmol/g.
Embodiment 3:
the present embodiment provides a Cu-attapulgite-NH2The preparation method of the composite material comprises the following steps:
preparing acidified attapulgite: is the same as embodiment 1, and will not be described herein.
Preparing a Cu-attapulgite material: dispersing 1 g of the purified acidified attapulgite material in 40 mL of 0.12M copper nitrate solution, stirring and soaking at 40 ℃ for 24h, centrifuging, washing with water for three times, and drying at 100 ℃. And transferring the mixture to a hydrothermal reaction kettle, dispersing the mixture in a 60% ethanol-water mixed solution, adding 3 mL of formic acid and 6 mL of ammonia water, and carrying out hydrothermal reaction at 150 ℃ for 2 h to prepare the Cu-attapulgite material.
Cu-Attapulgite-NH2Preparing a composite material: dispersing 1 g of the Cu-attapulgite material in 40 mL of aqueous solution, adding 8 g of dioctadecyl dimethyl ammonium bromide, fully stirring, transferring to a hydrothermal reaction kettle, and carrying out hydrothermal reaction at 120 ℃ for 2 h to obtain Cu-attapulgite-NH2A composite material.
Preparing the obtained Cu-attapulgite-NH2SEM of the composite material is shown in FIG. 5. Therefore, the prepared composite material can keep the original rod-shaped structure of the attapulgite, but the agglomeration is serious.
Mixing 50 mg of the above prepared Cu-attapulgite-NH2And adding the composite material into 80 mL of a 1.0 mM radioactive iodide ion simulating solution, adsorbing for 30 min at normal temperature, filtering, and detecting the concentration of residual iodide ions in the solution.
As shown in the adsorption result of FIG. 6, Cu-attapulgite-NH2The composite material achieves adsorption balance within 12 h, the adsorption efficiency can reach 45%, and the adsorption capacity reaches 0.72 mmol/g.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. Cu-attapulgite-NH2The preparation method of the composite material is characterized by comprising the following steps:
s1: dispersing acidified attapulgite clay in a copper nitrate solution, stirring and soaking for 24 hours at 40 ℃, centrifuging, washing with water, drying, dispersing in an organic solvent-water mixed solution, adding formic acid and ammonia water, and performing hydrothermal reaction to prepare a Cu-attapulgite material;
s2: dispersing the Cu-attapulgite material in an aqueous solution, adding dioctadecyl dimethyl ammonium bromide, and fully stirringThen, the Cu-attapulgite-NH is prepared by hydrothermal reaction2A composite material.
2. The Cu-attapulgite-NH according to claim 12The preparation method of the composite material is characterized in that in the step S1, the mass ratio of the acidified attapulgite clay to the copper nitrate solution to the formic acid to the ammonia water is 1: 0.01-0.10: 0.05-3.0: 1.0 to 8.0.
3. The Cu-attapulgite-NH according to claim 12The preparation method of the composite material is characterized in that in the step S1, the temperature of the hydrothermal reaction is 150 ℃, and the reaction time is 2 h.
4. The Cu-attapulgite-NH according to claim 12The preparation method of the composite material is characterized in that in S2, the mass ratio of the Cu-attapulgite material to the dioctadecyl dimethyl ammonium bromide is 1: 1 to 10.
5. The Cu-attapulgite-NH according to claim 12The preparation method of the composite material is characterized in that in the step S2, the temperature of the hydrothermal reaction is 120 ℃, and the reaction time is 2 h.
6. The Cu-Attapulgite-NH according to any of claims 1 to 52The preparation method of the composite material is characterized in that in the step S1, the preparation method of the acidified attapulgite clay comprises the following steps:
dispersing attapulgite clay in deionized water, stirring, centrifuging to remove impurities, soaking in dilute hydrochloric acid, stirring, and dispersing to obtain the acidified attapulgite; and washing and freeze-drying for later use.
7. The Cu-Attapulgite-NH according to any of claims 1 to 52The preparation method of the composite material is characterized in that in the S1, the mixed solution of the organic solvent and the water is in mass fractionIs 60% ethanol-water mixed solution.
8. The Cu-attapulgite-NH of any one of claims 1 to 72The application of the composite material in absorbing iodine ions in radioactive water.
9. The Cu-attapulgite-NH of claim 82The application of the composite material in adsorption of iodine ions in radioactive water is characterized in that the concentration of the iodine ions in the radioactive water is 0.1-1.0 mM; the Cu-attapulgite-NH2The amount of the composite material put in the radioactive water is 0.5-2 g.L－1。
10. The Cu-attapulgite-NH of claim 82The application of the composite material in absorbing iodine ions in radioactive water is characterized in that the Cu-attapulgite-NH2The temperature of the composite material in the radioactive water body is 25-50 ℃, and the adsorption time is 0.5-24 h.
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| CN114259986B (en) * | 2021-12-28 | 2023-06-30 | 淮阴工学院 | Preparation method of magnetic activated carbon-red mud-attapulgite composite adsorbent |
| CN114345301B (en) * | 2022-01-19 | 2023-09-08 | 西南科技大学 | Preparation and application of Bi@ chrysotile aerogel for removing radioactive iodine gas and aerosol |
| CN117299068B (en) * | 2023-10-08 | 2024-04-30 | 保山学院 | Preparation method of copper-based carbon silicon material and application of copper-based carbon silicon material in adsorption of radioactive iodine |
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| CN102284274A (en) * | 2011-06-07 | 2011-12-21 | 天津大学 | Preparation method for modified montmorillonite adsorbent and application thereof to removing micro or trace iodine |
| CN104941584A (en) * | 2015-07-06 | 2015-09-30 | 河北工业大学 | SiO2/C composite material for adsorbing heavy metal ions in water body and application thereof |
| CN106824084A (en) * | 2017-03-15 | 2017-06-13 | 天津大学 | The preparation method of the carbon-supported catalyst of a kind of nano cuprous oxide/copper modification and except iodine application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102284274A (en) * | 2011-06-07 | 2011-12-21 | 天津大学 | Preparation method for modified montmorillonite adsorbent and application thereof to removing micro or trace iodine |
| CN104941584A (en) * | 2015-07-06 | 2015-09-30 | 河北工业大学 | SiO2/C composite material for adsorbing heavy metal ions in water body and application thereof |
| CN106824084A (en) * | 2017-03-15 | 2017-06-13 | 天津大学 | The preparation method of the carbon-supported catalyst of a kind of nano cuprous oxide/copper modification and except iodine application |
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Application publication date: 20190917 Assignee: Nanjing Anhuai Innovative Drug Research Institute Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2021980014408 Denomination of invention: Preparation method of Cu attapulgite NH2composite and its application in adsorption of iodine ions in radioactive water Granted publication date: 20210924 License type: Common License Record date: 20211213 |
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