CN104353412A - Iron hydroxide/sepiolite compound arsenic adsorbing agent as well as preparation method and application thereof - Google Patents
Iron hydroxide/sepiolite compound arsenic adsorbing agent as well as preparation method and application thereof Download PDFInfo
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- CN104353412A CN104353412A CN201410679476.2A CN201410679476A CN104353412A CN 104353412 A CN104353412 A CN 104353412A CN 201410679476 A CN201410679476 A CN 201410679476A CN 104353412 A CN104353412 A CN 104353412A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
-
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention provides an iron hydroxide/sepiolite compound arsenic adsorbing agent. The iron hydroxide/sepiolite compound arsenic adsorbing agent is powdery, and is prepared by adopting the following steps: preparing a soluble ferric salt and a ferrous salt which are used as raw materials into a solution and then adding in sepiolite powder and fully mixing; then dropwise mixing with an alkaline solution and stirring, collecting a generated precipitate, washing with water and drying to obtain the iron hydroxide/sepiolite compound arsenic adsorbing agent. The iron hydroxide/sepiolite compound arsenic adsorbing agent provided by the invention can be used for removing inorganic trivalent arsenic in underground water or drinking water, and excellent arsenic removal performance. Meanwhile, the invention further provides a preparation method of the iron hydroxide/sepiolite compound arsenic adsorbing agent. The preparation method is simple and is mild in conditions, and safe and stable in performance.
Description
Technical field
The invention provides preparation method and the application thereof of the nano combined arsenic adsorbent of a kind of iron hydroxide/sepiolite, belong to technical field of water purification.
Background technology
In the last few years, the arsenic pollution in underground water was a global threat, had become the major issue that millions of people all over the world pay close attention to, due to high toxicity and the carcinogenicity of arsenic.The water that Long Term Contact arsenic pollutes can cause very large negative effect to human health, also can cause the generation of a lot of serious disease, as cutaneum carcinoma, lung cancer and carcinoma of urinary bladder etc.Arsenic Contamination in Groundwater causes the large-scale arsenic poisoning in Asia and the U.S. widely, particularly in some countries of India, Bangladesh, Vietnam, Thailand, Chile and periphery.Usually there are two kinds of main states of oxidation in inorganic arsenic, i.e. arsenite (NaAsO
2) and arsenate (Na
2hAsO
4), but As (III) is larger than the toxicity of As (V), mainly because As (III) has stronger toxicity and mobility.Method for the treatment of arsenic polluted water has a lot, wherein absorption method is considered to most effective method, therefore simple, efficient, the green economy of development and Design material for water treatment and meet the national drinking water standard that reaches 10 μ g/L simultaneously and there is the common objective that high adsorption capacity becomes whole world researchers.
Summary of the invention
The invention provides the nano combined arsenic adsorbent of a kind of iron hydroxide/sepiolite, this adsorbent has excellent arsenic removal performance, simultaneously simple, the mild condition of its preparation method, and performance safety is stablized.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
The nano combined arsenic adsorbent of a kind of iron hydroxide/sepiolite, described adsorbent is powdered, obtain in the following ways: with soluble ferric iron salt and ferrous salt for raw material, add sepiolite powder after being configured to solution and fully stir, and then it is dropwise mixed with alkaline solution and stirs, generated sediment is collected and washes, after drying, the nano combined arsenic adsorbent of iron hydroxide/sepiolite can be obtained.
The present invention additionally provides the preparation method of the nano combined arsenic adsorbent of above-mentioned iron hydroxide/sepiolite simultaneously, comprises the following steps: (1), by soluble ferrite and soluble ferric iron salt according to Fe
2+: Fe
3+the mol ratio of=1:2 is incorporated in anaerobic water, until dissolve completely after fully stirring, obtains filemot solution;
(2), by sepiolite be added in above-mentioned filemot solution, after ultrasonic disperse also fully stirs, then add disodium phosphate soln, stir, namely obtained containing iron ion/sepiolite solution;
(3), by sodium carbonate mix with sodium hydroxide solution, configuration alkaline carbon acid group solution;
(4), under room temperature and churned mechanically condition, mix what prepared containing iron ion/sepiolite solution and alkaline carbon acid group dropwise and continue to stir, produce cyan precipitation, pH value is constant is in the process 10 ~ 11;
(5), collecting precipitation, under centrifugal condition, adopt absolute ethyl alcohol and distilled water washing, removing supernatant;
(6), finally by the product drying after washing, dried solid abrasive is powdered, i.e. the obtained nano combined arsenic adsorbent of iron hydroxide/sepiolite.
Described soluble ferrite and soluble ferric iron salt are ferrous sulfate and ferric sulfate.
Described sepiolite is the fibrous clay minerals of diameter 30nm.
In step (5), wash under the centrifuge condition of 10000rpm rotating speed.
In step (6), described drying steps is 60
at temperature, vacuum drying 4 ~ 10h.
Iron hydroxide/sepiolite provided by the present invention nano combined arsenic adsorbent can be used in removing the inorganic trivalent arsenic in underground water or drinking water.
Layered double hydroxide (LDHs) because it is abundant cheap, be easy to synthesis and possess excellent adsorption capacity, be the emphasis studied of researchers and focus in arsenic polluted water process material.Because the charged difference of interlayer makes it with structure positive charge, and it also has larger specific area, at present, reports all to some extent in the pollutant such as anion, organic dyestuff, heavy metal ion of layered double hydroxide in process waste water.
Fe (II, III) hydroxide is commonly called as patina (Green Rust, GRs), belong to layered double hydroxide (LDH) family, its crystal structure be by positively charged shepardite structural laminate plate and anion, water molecule layer is stacking forms, aobvious electroneutral, its la m is respectively divalence and trivalent metal cation, the ion of interlayer is anion, and their structure and composition depend on the anion of combination.GRs is divided into two classes according to X-ray diffraction by the people such as Bernal at first: a class is the GR1 with plane anion, has GR1 (Cl
-), GR1 (CO
3 2-), GR1 (SO
3 2-), their crystal structure is considered to be similar to pyroaurite Mg
iI 6fe
iII 2(OH)
16cO
34H
2o; Another kind of is the GR2 with three-dimensional anion, up to the present, only has two kinds of GR2 (SO
4 2-) and GR2 (SeO
4 2-) be found, its crystal structure is not yet determined.The existence of ferrous ion in GR structure, makes GR have special character, can show extremely strong adsorption capacity and redox ability, and its special structure, composition and adjustable sex change simultaneously makes it be widely used in the field such as catalysis and absorption.
In the present invention, sepiolite is as a kind of fibrous natural nano-mineral material of excellent performance, and (external surface area is 500m to have very large specific area
2/ g, inner ratio surface area is 400m
2/ g), and outer surface contains a large amount of silicone hydroxyl groups, shows very strong surface-active and absorption property.Nanoscale Iron hydroxide is combined with sepiolite, while the chemisorbed utilizing it modified, the powerful physisorption of sepiolite itself can be played again, make its better processing effect in purification of water quality.
Accompanying drawing explanation
The XRD figure of the nano combined arsenic adsorbent of the iron hydroxide/sepiolite of Fig. 1 prepared by the present invention;
Fig. 2 is the TEM figure of the nano combined arsenic adsorbent of iron hydroxide/sepiolite prepared by the present invention;
Fig. 3 is that the nano combined arsenic adsorbent of iron hydroxide/sepiolite prepared by the present invention is to the adsorpting rate curve figure of arsenic;
Fig. 4 is that the nano combined arsenic adsorbent of iron hydroxide/sepiolite prepared by the present invention is to the adsorption isotherm line chart of arsenic.
Detailed description of the invention
Below in conjunction with drawings and the specific embodiments, detailed specific description is done to the present invention, but protection scope of the present invention is not limited to following examples.
Embodiment 1
The preparation method of iron hydroxide/sepiolite nano combined arsenic adsorbent prepared in the present embodiment is as follows: 100mL high purity water is passed into nitrogen 30min to remove the oxygen in water, under room temperature and mechanical agitation state, to adding the sulphate of iron of 0.133mol/L and the ferrous sulfate of 0.267mol/L except in the water of deoxidation, both mol ratios are Fe
2+: Fe
3+=1:2, continues to stir until dissolve, obtains brown solution; Be dispersed in iron-containing liquor by 1g sepiolite again, sealing allows it keep the environment of anaerobic, first ultrasonic disperse 30min, then after stirring 60h, adds the disodium phosphate soln of 0.02mol/L, stir in solution, namely obtains containing iron ion/sepiolite solution.
Prepare certain density carbonate solution again: take a certain amount of natrium carbonicum calcinatum, be added in the sodium hydroxide solution of 100mL 0.8mol/L, make the ultimate density of carbonate solution be 0.466mol/L.
Under room temperature and churned mechanically condition, mix what prepared containing iron ion/sepiolite solution and carbonate dropwise and continue to stir, produce cyan precipitation immediately, in the process, pH value is constant is about 10.5, collecting precipitation.
By collect in upper step be deposited in the centrifuge condition of 10000rpm rotating speed under, with absolute ethyl alcohol, distilled water centrifuge washing repeatedly, abandoning supernatant, by solids 80
at temperature, vacuum drying 7h, more dried solids is ground into powder, namely obtain the nano combined arsenic adsorbent of iron hydroxide/sepiolite.
The nano combined arsenic adsorbent of iron hydroxide/sepiolite obtained in the present embodiment adopts XRD characterization method to carry out material phase analysis, as shown in Figure 1, result shows that the nano combined arsenic adsorbent of Fe (II, III)-LDH/SEP is that 7.288 ° of (110) crystal face characteristic diffraction peaks located still exist at 2 θ angles, sepiolite before the reaction its thing phase constituent rear does not change, and still keeps original structure.Be simultaneously that new diffraction maximum has appearred in 11.74 °, 23.65 °, 33.56 ° places at 2 θ angles, it meets rhombohedron Fe
6(OH)
12(CO
3) standard card (JCPDS Card No.46-0098,
), the crystal face of its correspondence is respectively (003), (006), (012).Adopt the microstructure of transmission electron microscope to nano combined arsenic adsorbent to observe, as shown in Figure 2, Fe (II, III)-LDH in hexahedral shape, size is more homogeneous equably load is surperficial at sepiolite.
Iron hydroxide/sepiolite nano combined arsenic adsorbent prepared in the present embodiment can be used in removing the inorganic trivalent arsenic in underground water or drinking water, and concrete application is as follows:
1, a certain amount of As is got
2o
3be dissolved in the NaOH solution of 1mol/L, subacidity is neutralized to the HCl solution of 2mol/L, be mixed with high purity water constant volume the trivalent arsenic solution that initial concentration is 5mg/L, allocating its pH value by the HCl of 1mol/L and NaOH solution is 6.5, and simulation is containing inorganic arsenious water.Get 50mL above-mentioned containing in inorganic trivalent arsenic solution loading 250mL tool plug conical flask, add the nano combined arsenic adsorbent of iron hydroxide/sepiolite prepared in 50mg the present embodiment and ultrasonic disperse 30min, then be placed on 25
jolting on bath constant temperature oscillator, in sampling and measuring water, arsenic concentration is with the change in reaction time, with the membrane filtration of 0.45 μm, As (III) concentration remaining in filtrate is measured again with Atomic fluorophotometry, result shows that the rate of adsorption of this nano combined arsenic adsorbent is very fast, as shown in Figure 3, in 3 hours, adsorption capacity can reach 24.56mg/g.Simulate with pseudo-second order kinetic, the coefficient R that matching obtains
2value is 0.9985.As can be seen here, Fe (II, III)-LDH/SEP adsorbs As (III) and meets pseudo-second order kinetic model, and adsorption process is mainly rate determining step with chemisorbed.
2, a certain amount of As is got
2o
3be dissolved in the NaOH solution of 1mol/L, be neutralized to subacidity with the HCl solution of 2mol/L, be mixed with initial concentration with high purity water constant volume and be respectively 0.2,0.7,2,7,8,16,17,20,30, the trivalent arsenic solution of 36mg/L, allocating its pH value by the HCl of 1mol/L and NaOH solution is 6.5, and simulation is containing inorganic arsenious water.Get 50mL respectively above-mentioned containing inorganic trivalent arsenic solution loading 250mL tool plug conical flask, add the nano combined arsenic adsorbent of iron hydroxide/sepiolite prepared in 50mg the present embodiment and ultrasonic disperse 30min, be placed on jolting 24h on 25 DEG C of water-bath constant temperature oscillators again, after making it adsorb to reach balance, with the membrane filtration of 0.45 μm, As (III) concentration remaining in filtrate when measuring different initial concentration adsorption equilibrium with Atomic fluorophotometry.As shown in Figure 4, Fe (II, III)-LDH/SEP nano combined arsenic adsorbent has good adsorption capacity to As (III) to result, and can reach adsorption equilibrium within a short period of time, and accessible maximum adsorption capacity is 109.42mg/g.Carry out matching with Langmuir Adsorption thermodynamics isotherm model, matching show that the adsorption capacity of this adsorbent is 135.50mg/g, the matching coefficient of determination (R of model
2) be 0.9891, illustrate that the nano combined arsenic adsorbent that the present invention obtains has larger adsorption capacity to trivalent arsenic, in the saturated condition the arsenic of the adsorbable at most nearly 135.50mg of every 1g adsorbent.
Embodiment 2
The preparation method of iron hydroxide/sepiolite nano combined arsenic adsorbent prepared in the present embodiment is as follows: 100mL high purity water is passed into nitrogen 30min to remove the oxygen in water, under room temperature and mechanical agitation state, to adding the sulphate of iron of 0.133mol/L and the ferrous sulfate of 0.267mol/L except in the water of deoxidation, both mol ratios are Fe
2+: Fe
3+=1:2, continues to stir until dissolve, obtains brown solution; Be dispersed in iron-containing liquor by 1g sepiolite again, sealing allows it keep the environment of anaerobic, first ultrasonic disperse 30min, then after stirring 60h, adds the disodium phosphate soln of 0.02mol/L, stir in solution, namely obtains containing iron ion/sepiolite solution.
Prepare certain density carbonate solution again: take a certain amount of natrium carbonicum calcinatum, be added in the sodium hydroxide solution of 100mL 0.8mol/L, make the ultimate density of carbonate solution be 0.466mol/L.
Under room temperature and churned mechanically condition, mix what prepared containing iron ion/sepiolite solution and carbonate dropwise and continue to stir, produce cyan precipitation immediately, in the process, pH value is constant is about 10, collecting precipitation.
By collect in upper step be deposited in the centrifuge condition of 10000rpm rotating speed under, with absolute ethyl alcohol, distilled water centrifuge washing repeatedly, abandoning supernatant, by solids 80
at temperature, vacuum drying 5h, more dried solids is ground into powder, namely obtain the nano combined arsenic adsorbent of iron hydroxide/sepiolite.
Embodiment 3
The preparation method of iron hydroxide/sepiolite nano combined arsenic adsorbent prepared in the present embodiment is as follows: 100mL high purity water is passed into nitrogen 30min to remove the oxygen in water, under room temperature and mechanical agitation state, to adding the sulphate of iron of 0.133mol/L and the ferrous sulfate of 0.267mol/L except in the water of deoxidation, both mol ratios are Fe
2+: Fe
3+=1:2, continues to stir until dissolve, obtains brown solution; Be dispersed in iron-containing liquor by 1g sepiolite again, sealing allows it keep the environment of anaerobic, first ultrasonic disperse 30min, then after stirring 60h, adds the disodium phosphate soln of 0.02mol/L, stir in solution, namely obtains containing iron ion/sepiolite solution.
Prepare certain density carbonate solution again: take a certain amount of natrium carbonicum calcinatum, be added in the sodium hydroxide solution of 100mL 0.8mol/L, make the ultimate density of carbonate solution be 0.466mol/L.
Under room temperature and churned mechanically condition, mix what prepared containing iron ion/sepiolite solution and carbonate dropwise and continue to stir, produce cyan precipitation immediately, in the process, pH value is constant is about 11, collecting precipitation.
By collect in upper step be deposited in the centrifuge condition of 8000rpm rotating speed under, with absolute ethyl alcohol, distilled water centrifuge washing repeatedly, abandoning supernatant, by solids 80
at temperature, vacuum drying 9h, more dried solids is ground into powder, namely obtain the nano combined arsenic adsorbent of iron hydroxide/sepiolite.
Claims (7)
1. the nano combined arsenic adsorbent of iron hydroxide/sepiolite, it is characterized in that: described adsorbent is powdered, obtain in the following ways: with soluble ferric iron salt and ferrous salt for raw material, add sepiolite powder after being configured to solution and fully stir, and then it is dropwise mixed with alkaline solution and stirs, generated sediment is collected and washes, after drying, the nano combined arsenic adsorbent of iron hydroxide/sepiolite can be obtained.
2. the preparation method of the nano combined arsenic adsorbent of iron hydroxide/sepiolite according to claim 1, is characterized in that comprising the following steps: (1), by soluble ferrite and soluble ferric iron salt according to Fe
2+: Fe
3+the mol ratio of=1:2 is incorporated in anaerobic water, until dissolve completely after fully stirring, obtains filemot solution;
(2), by sepiolite be added in above-mentioned filemot solution, after ultrasonic disperse also fully stirs, then add disodium phosphate soln, stir, namely obtained containing iron ion/sepiolite solution;
(3), by sodium carbonate mix with sodium hydroxide solution, configuration alkaline carbon acid group solution;
(4), under room temperature and churned mechanically condition, mix what prepared containing iron ion/sepiolite solution and alkaline carbon acid group dropwise and continue to stir, produce cyan precipitation, pH value is constant is in the process 10 ~ 11;
(5), collecting precipitation, under centrifugal condition, adopt absolute ethyl alcohol and distilled water washing, removing supernatant;
(6), finally by the product drying after washing, dried solid abrasive is powdered, i.e. the obtained nano combined arsenic adsorbent of iron hydroxide/sepiolite.
3. preparation method according to claim 2, is characterized in that: described soluble ferrite and soluble ferric iron salt are ferrous sulfate and ferric sulfate.
4. preparation method according to claim 2, is characterized in that: described sepiolite is the fibrous clay minerals of diameter 30nm.
5. preparation method according to claim 2, is characterized in that: in step (5), washs under the centrifuge condition of 10000rpm rotating speed.
6. preparation method according to claim 2, is characterized in that: in step (6), described drying steps be
at temperature, vacuum drying 4 ~ 10h.
7. the purposes of the nano combined arsenic adsorbent of iron hydroxide/sepiolite according to claim 1, is characterized in that: for removing the inorganic trivalent arsenic in underground water or drinking water.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105771894A (en) * | 2016-04-15 | 2016-07-20 | 上海大学 | Phosphorus removal adsorbing agent for expanded graphite loaded composite metal and preparation method thereof |
| CN107335408A (en) * | 2017-07-31 | 2017-11-10 | 河海大学 | A kind of preparation method and application for the cyclodextrin for coating iron aluminium hydroxide |
| CN113118202A (en) * | 2021-04-13 | 2021-07-16 | 武汉理工大学 | Curing agent for efficiently repairing arsenic-polluted soil and application thereof |
| CN114377659A (en) * | 2021-12-13 | 2022-04-22 | 湖南德创永禾环保科技有限公司 | Preparation method of nano composite thallium removal agent |
| CN114774130A (en) * | 2022-04-15 | 2022-07-22 | 哈尔滨工业大学 | Modified clay mineral for repairing arsenic-lead-antimony composite contaminated soil and preparation method and application thereof |
| CN114849641A (en) * | 2022-04-18 | 2022-08-05 | 河南大学 | Petal-shaped nano iron hydroxide and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105771894A (en) * | 2016-04-15 | 2016-07-20 | 上海大学 | Phosphorus removal adsorbing agent for expanded graphite loaded composite metal and preparation method thereof |
| CN107335408A (en) * | 2017-07-31 | 2017-11-10 | 河海大学 | A kind of preparation method and application for the cyclodextrin for coating iron aluminium hydroxide |
| CN113118202A (en) * | 2021-04-13 | 2021-07-16 | 武汉理工大学 | Curing agent for efficiently repairing arsenic-polluted soil and application thereof |
| CN113118202B (en) * | 2021-04-13 | 2022-06-03 | 武汉理工大学 | Curing agent for efficiently repairing arsenic-polluted soil and application thereof |
| CN114377659A (en) * | 2021-12-13 | 2022-04-22 | 湖南德创永禾环保科技有限公司 | Preparation method of nano composite thallium removal agent |
| CN114774130A (en) * | 2022-04-15 | 2022-07-22 | 哈尔滨工业大学 | Modified clay mineral for repairing arsenic-lead-antimony composite contaminated soil and preparation method and application thereof |
| CN114849641A (en) * | 2022-04-18 | 2022-08-05 | 河南大学 | Petal-shaped nano iron hydroxide and preparation method and application thereof |
| CN114849641B (en) * | 2022-04-18 | 2023-03-10 | 河南大学 | Petal-shaped nano iron hydroxide and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN104353412B (en) | 2016-08-24 |
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