CN110237806A - Cu- attapulgite-NH2The preparation method of composite material and its application in Adsorption of Radioactive water body in iodide ion - Google Patents
Cu- attapulgite-NH2The preparation method of composite material and its application in Adsorption of Radioactive water body in iodide ion Download PDFInfo
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- CN110237806A CN110237806A CN201910431875.XA CN201910431875A CN110237806A CN 110237806 A CN110237806 A CN 110237806A CN 201910431875 A CN201910431875 A CN 201910431875A CN 110237806 A CN110237806 A CN 110237806A
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- attapulgite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
Abstract
The present invention relates to dirty water decontamination handles technical fields, disclose a kind of Cu- attapulgite-NH for iodide ion absorption2The preparation method of composite material and its application in Adsorption of Radioactive water body in iodide ion, method includes the following steps: S1: dispersing Acid-treatment Palygorskite Clays in copper nitrate solution, after stirring impregnates for 24 hours at 40 DEG C, centrifugation, washing, drying, it is then dispersed in organic solvent-water mixed solution, it is subsequently added into formic acid and ammonium hydroxide, hydro-thermal reaction prepares Cu- attapulgite material；S2: dispersing the Cu- attapulgite material in aqueous solution, dioctadecyldimethylammonium bromide is added, after being sufficiently stirred, hydro-thermal reaction prepares Cu- attapulgite-NH2Composite material.Compared with prior art, the present invention improves the adsorption capacity and selectivity of existing copper-based adsorbent, and the removing for radioiodine in waste water provides Technical Reference.
Description
Technical field
The present invention relates to dirty water decontamination handles technical field, in particular to a kind of Cu- attapulgite-NH2Composite material
Preparation method and its application in Adsorption of Radioactive water body in iodide ion.
Background technique
With flourishing for China's economic and becoming increasingly conspicuous for environmental problem, Nuclear Power Industry has become the important hair of country
Exhibition strategy, it is contemplated that run to the year two thousand twenty China nuclear power and be up to 88 GW building installation total amount.Consequent is effectively solved to put
Pollution is penetrated to be of great significance to the safe handling of nuclear energy.The breakage monitoring that radioiodine is often used as Reactor fuel element cladding
The signal radionuclide of environmental monitoring after index and nuclear explosion, is one of inevitable outcome of nuclear fission.Thus, efficiently remove liquid phase radiation
Property iodine to be Nuclear Safety utilize institute's key scientific problems to be solved.
The technologies such as chemical precipitation, porous material absorption, ion exchange and UF membrane can be used for the removal of liquid phase radioiodine
It uses.The metal material that chemical precipitation uses is expensive and be easy to cause the secondary pollution of heavy metal.Porous material is in complexity
The selective absorption efficiency of environment is difficult to ensure.Due to the use of organic or inorganic solvent, so that ion exchange technique also easily produces
Raw secondary pollution.Though membrane separation technique possesses good removal efficiency, operating cost is costly.
Summary of the invention
Goal of the invention: aiming at the problems existing in the prior art, the present invention provides a kind of Cu- attapulgite-NH2Composite wood
The preparation method of material and its application in Adsorption of Radioactive water body in iodide ion utilize the charge characteristic object of composite material surface
Reason absorption liquid phase radioactive pollutant, using Cu selective absorption radioiodine, more traditional copper-based adsorbent improves iodine absorption
Capacity and selectivity, the removing for radioiodine in waste water provide Technical Reference.
Technical solution: the present invention provides a kind of Cu- attapulgite-NH2The preparation method of composite material, including following step
Rapid: S1: dispersing Acid-treatment Palygorskite Clays in copper nitrate solution, and at 40 DEG C after 24 h of stirring dipping, centrifugation, is dried at washing
It is dry, it is then dispersed in organic solvent-water mixed solution, is subsequently added into formic acid and ammonium hydroxide, hydro-thermal reaction prepares Cu- bumps
Stick stone material；S2: dispersing the Cu- attapulgite material in aqueous solution, and dioctadecyldimethylammonium bromide is added, fills
After dividing stirring, hydro-thermal reaction prepares Cu- attapulgite-NH2Composite material.
Preferably, in the S1, the Acid-treatment Palygorskite Clays, the copper nitrate solution, the formic acid and institute
The mass ratio for stating ammonium hydroxide is 1:0.01 ~ 0.10:0.05 ~ 3.0:1.0 ~ 8.0.
Preferably, in the S1, the temperature of the hydro-thermal reaction is 150 oC, and the reaction time is 2 h.
Preferably, in the S2, the matter of the Cu- attapulgite material and the dioctadecyldimethylammonium bromide
Amount is than being 1:1 ~ 10.
Preferably, in the S2, the temperature of the hydro-thermal reaction is 120 oC, and the reaction time is 2 h.
Preferably, in the S1, the Acid-treatment Palygorskite Clays the preparation method is as follows:
Preferably, in deionized water by attapulgite clay dispersion, stirring is placed in dilute hydrochloric acid and impregnates after being centrifuged decontamination,
Agitated and dispersion, is made the acidification attapulgite；It is lyophilized after washing spare.
Preferably, in the S1, the mixed solution of the organic solvent-water is that the alcohol-water that mass fraction is 60% is mixed
Close solution.
The present invention also provides a kind of Cu- attapulgite-NH2Composite material is in Adsorption of Radioactive water body in iodide ion
Using.
Preferably, the concentration of iodide ion is 0.1 ~ 1.0 mM in the radioactivity water body；Cu- attapulgite-the NH2It is multiple
Injected volume of the condensation material in the radioactivity water body is 0.5 ~ 2 gL- 1。
Preferably, the Cu- attapulgite-NH2Composite material in the radioactivity water body adsorb when temperature be
25 ~ 50 oC, adsorption time are 0.5 ~ 24 h.
The utility model has the advantages that the present invention Features of Attapulgite Minerals good, cheap and big specific surface using stability is as matrix material
Copper nitrate, is carried in attapulgite duct with infusion process, is redispersed in solution, using hydrothermal synthesis method, with formic acid by material
Cu- attapulgite composite material is restored and regulated and controled with ammonium hydroxide.It again disperses above-mentioned composite material in solution, is added double 18
Alkyl dimethyl bromination ammonium surfactant regulates and controls attapulgite surface charge, prepares Cu- attapulgite-through hydro-thermal reaction
NH2Composite material.
Cu- attapulgite-the NH that will be prepared2Composite material is for the iodide ion in Adsorption of Radioactive water body, by ammonia
(attapulgite original tape has negative electrical charge to the positive charge characteristic on attapulgite surface, after amido modified, makes its surface band after base modification
Positive charge is more advantageous to the absorption of anion-iodide ion), the low concentration iodide ion in enrichment solution recycles in composite material
Cu reacted with the CuO compacted zone on surface generate Cu2O is reacted with iodide ion generates cuprous iodide.In adsorption process, due to object
Reason absorption and chemisorption synergistic effect, so that Cu- attapulgite-NH2The more traditional copper-based adsorbent of composite material has higher
Adsorption capacity.
Compared with prior art, remarkable advantage is: (1) this method use simple hydrothermal synthesis method, simple process,
Generated time is short, and raw material are cheap and easy to get, nontoxic；(2) Cu synthesized is located in the duct of attapulgite, avoids in adsorption process
Cu's falls off；(3) adsorbent is cheap, is conducive to practical application.
Detailed description of the invention
Fig. 1 is the Cu- attapulgite-NH prepared in embodiment 12The SEM scanning electron microscope (SEM) photograph of composite material；
Fig. 2 is the Cu- attapulgite-NH prepared in embodiment 12Composite material absorption property curve graph；
Fig. 3 is the Cu- attapulgite-NH prepared in embodiment 12The SEM scanning electron microscope (SEM) photograph of composite material；
Fig. 4 is the Cu- attapulgite-NH prepared in embodiment 12Composite material absorption property curve graph；
Fig. 5 is the Cu- attapulgite-NH prepared in embodiment 12The SEM scanning electron microscope (SEM) photograph of composite material；
Fig. 6 is the Cu- attapulgite-NH prepared in embodiment 12Composite material absorption property curve graph.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
Embodiment 1:
Present embodiments provide for a kind of Cu- attapulgite-NH2The preparation method of composite material, comprising the following steps:
The preparation of Acid-treatment Palygorskite Clays: in deionized water by attapulgite clay dispersion, stirring, after being centrifuged decontamination,
It is placed in dilute hydrochloric acid and impregnates, acidification attapulgite is made in agitated and dispersion；It is lyophilized after washing spare.
The preparation of Cu- attapulgite material: 40 mL, 0.1 M is dispersed by the acidification attapulgite material after 1 g purification
In copper nitrate solution, after stirring impregnates for 24 hours at 40 DEG C, after centrifugation, washing three times, 100 oC drying.Transfer to hydro-thermal reaction
Kettle, using dispersing in 60% alcohol-water mixed solution, 2 mL formic acid, the 4 mL ammonium hydroxide of addition, after 150 oC hydro-thermal reaction, 2 h,
Prepare Cu- attapulgite material.
Cu- attapulgite-NH2The preparation of composite material: it is water-soluble that 40 mL are dispersed by the above-mentioned Cu- attapulgite material of 1 g
In liquid, 4 g dioctadecyldimethylammonium bromide are added, after being sufficiently stirred, are transferred in hydrothermal reaction kettle, 120 oC hydro-thermals are anti-
It answers after 2 h to get Cu- attapulgite-NH2Composite material.
Cu- attapulgite-the NH being prepared2The SEM Electronic Speculum of composite material is as shown in Figure 1.It can be seen that compound after preparation
Material is able to maintain the original club shaped structure of attapulgite.
By 50 mg Cu- attapulgite-NH obtained above2The simulated emission of composite material addition 50 mL, 1.0 mM
In the solution of iodide ion, at normal temperature, after adsorbing 30 min, filtering detects residual iodine ions concentration in solution.
As the absorption result of Fig. 2 shows Cu- attapulgite-NH2Composite material reaches adsorption equilibrium in 10 h, absorption
Efficiency can reach 75%, and adsorption capacity reaches 0.75 mmol/g.
Embodiment 2:
Present embodiments provide for a kind of Cu- attapulgite-NH2The preparation method of composite material, comprising the following steps:
It is acidified the preparation of attapulgite: it is identical with embodiment 1, it is not repeated herein.
The preparation of Cu- attapulgite material: 40 mL, 0.01 M is dispersed by the acidification attapulgite material after 1 g purification
In copper nitrate solution, after stirring impregnates for 24 hours at 40 DEG C, after centrifugation, washing three times, 100 oC drying.Transfer to hydro-thermal reaction
Kettle, using dispersing in 60% alcohol-water mixed solution, 0.05 mL formic acid, the 1 mL ammonium hydroxide of addition, 150 oC hydro-thermal reaction, 2 h
Afterwards, Cu- attapulgite material is prepared.
Cu- attapulgite-NH2The preparation of composite material: it is water-soluble that 40 mL are dispersed by the above-mentioned Cu- attapulgite material of 1 g
In liquid, 2 g dioctadecyldimethylammonium bromide are added, after being sufficiently stirred, are transferred in hydrothermal reaction kettle, 120 oC hydro-thermals are anti-
It answers after 2 h to get Cu- attapulgite-NH2Composite material.
Cu- attapulgite-the NH being prepared2The SEM Electronic Speculum of composite material is as shown in Figure 3.It can be seen that compound after preparation
Material is able to maintain the original club shaped structure of attapulgite.
By 50 mg Cu- attapulgite-NH obtained above2The simulated emission of composite material addition 20 mL, 1.0 mM
In the solution of iodide ion, at normal temperature, after adsorbing 30 min, filtering detects residual iodine ions concentration in solution.
As the absorption result of Fig. 4 shows Cu- attapulgite-NH2Composite material reaches adsorption equilibrium in 2 h, absorption
Efficiency can reach 60%, and adsorption capacity reaches 0.24 mmol/g.
Embodiment 3:
Present embodiments provide for a kind of Cu- attapulgite-NH2The preparation method of composite material, comprising the following steps:
It is acidified the preparation of attapulgite: it is identical with embodiment 1, it is not repeated herein.
The preparation of Cu- attapulgite material: 40 mL, 0.12 M is dispersed by the acidification attapulgite material after 1 g purification
In copper nitrate solution, after stirring impregnates for 24 hours at 40 DEG C, after centrifugation, washing three times, 100 oC drying.Transfer to hydro-thermal reaction
Kettle, using dispersing in 60% alcohol-water mixed solution, 3 mL formic acid, the 6 mL ammonium hydroxide of addition, after 150 oC hydro-thermal reaction, 2 h,
Prepare Cu- attapulgite material.
Cu- attapulgite-NH2The preparation of composite material: it is water-soluble that 40 mL are dispersed by the above-mentioned Cu- attapulgite material of 1 g
In liquid, 8 g dioctadecyldimethylammonium bromide are added, after being sufficiently stirred, are transferred in hydrothermal reaction kettle, 120 oC hydro-thermals are anti-
It answers after 2 h to get Cu- attapulgite-NH2Composite material.
Cu- attapulgite-the NH being prepared2The SEM Electronic Speculum of composite material is as shown in Figure 5.It can be seen that compound after preparation
Material is able to maintain the original club shaped structure of attapulgite, but it is more serious to reunite.
By 50 mg Cu- attapulgite-NH obtained above2The simulated emission of composite material addition 80 mL, 1.0 mM
In the solution of iodide ion, at normal temperature, after adsorbing 30 min, filtering detects residual iodine ions concentration in solution.
As the absorption result of Fig. 6 shows Cu- attapulgite-NH2Composite material reaches adsorption equilibrium in 12 h, absorption
Efficiency can reach 45%, and adsorption capacity reaches 0.72 mmol/g.
The technical concepts and features of above embodiment only to illustrate the invention, its object is to allow be familiar with technique
People cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent transformation or modification that Spirit Essence is done, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of Cu- attapulgite-NH2The preparation method of composite material, which comprises the following steps:
S1: dispersing Acid-treatment Palygorskite Clays in copper nitrate solution, and after stirring impregnates for 24 hours at 40 DEG C, centrifugation, is dried at washing
It is dry, it is then dispersed in organic solvent-water mixed solution, is subsequently added into formic acid and ammonium hydroxide, hydro-thermal reaction prepares Cu- bumps
Stick stone material；
S2: dispersing the Cu- attapulgite material in aqueous solution, and dioctadecyldimethylammonium bromide is added, sufficiently stirs
After mixing, hydro-thermal reaction prepares Cu- attapulgite-NH2Composite material.
2. Cu- attapulgite-NH according to claim 12The preparation method of composite material, which is characterized in that in the S1
In, the Acid-treatment Palygorskite Clays, the copper nitrate solution, the formic acid and the ammonium hydroxide mass ratio be 1:0.01 ~
0.10:0.05 ~ 3.0:1.0 ~ 8.0.
3. Cu- attapulgite-NH according to claim 12The preparation method of composite material, which is characterized in that described
In S1, the temperature of the hydro-thermal reaction is 150 oC, and the reaction time is 2 h.
4. Cu- attapulgite-NH according to claim 12The preparation method of composite material, which is characterized in that in the S2
In, the mass ratio of the Cu- attapulgite material and the dioctadecyldimethylammonium bromide is 1:1 ~ 10.
5. Cu- attapulgite-NH according to claim 12The preparation method of composite material, which is characterized in that in the S2
In, the temperature of the hydro-thermal reaction is 120 oC, and the reaction time is 2 h.
6. Cu- attapulgite-NH according to any one of claim 1 to 52The preparation method of composite material, feature exist
In, in the S1, the Acid-treatment Palygorskite Clays the preparation method is as follows:
In deionized water by attapulgite clay dispersion, stirring is placed in dilute hydrochloric acid and impregnates after being centrifuged decontamination, agitated
And dispersion, the acidification attapulgite is made；It is lyophilized after washing spare.
7. Cu- attapulgite-NH according to any one of claim 1 to 52The preparation method of composite material, feature exist
In in the S1, the mixed solution of the organic solvent-water is the alcohol-water mixed solution that mass fraction is 60%.
8. a kind of Cu- attapulgite-NH as described in any one of claims 1 to 72Composite material is in Adsorption of Radioactive water body
Application in middle iodide ion.
9. Cu- attapulgite-NH according to claim 82Composite material answering in iodide ion in Adsorption of Radioactive water body
With, which is characterized in that the concentration of iodide ion is 0.1 ~ 1.0 mM in the radioactivity water body；Cu- attapulgite-the NH2It is multiple
Injected volume of the condensation material in the radioactivity water body is 0.5 ~ 2gL- 1。
10. Cu- attapulgite-NH according to claim 82Composite material is in Adsorption of Radioactive water body in iodide ion
Using, which is characterized in that the Cu- attapulgite-NH2Composite material in the radioactivity water body adsorb when temperature be
25 ~ 50 oC, adsorption time are 0.5 ~ 24 h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114259986A (en) * | 2021-12-28 | 2022-04-01 | 淮阴工学院 | Preparation method of magnetic activated carbon-red mud-attapulgite composite adsorbent |
| CN114345301A (en) * | 2022-01-19 | 2022-04-15 | 西南科技大学 | Preparation and application of Bi @ chrysotile aerogel for removing radioactive iodine gas and aerosol |
| CN117299068A (en) * | 2023-10-08 | 2023-12-29 | 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 |
| 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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| 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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| 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114259986A (en) * | 2021-12-28 | 2022-04-01 | 淮阴工学院 | Preparation method of magnetic activated carbon-red mud-attapulgite composite adsorbent |
| CN114259986B (en) * | 2021-12-28 | 2023-06-30 | 淮阴工学院 | Preparation method of magnetic activated carbon-red mud-attapulgite composite adsorbent |
| CN114345301A (en) * | 2022-01-19 | 2022-04-15 | 西南科技大学 | Preparation and application of Bi @ chrysotile aerogel for removing radioactive iodine gas and aerosol |
| 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 |
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| 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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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 |