CN106824046B - A kind of copper cerium codope magnetic composite and its methods for making and using same - Google Patents
A kind of copper cerium codope magnetic composite and its methods for making and using same Download PDFInfo
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- CN106824046B CN106824046B CN201710126218.5A CN201710126218A CN106824046B CN 106824046 B CN106824046 B CN 106824046B CN 201710126218 A CN201710126218 A CN 201710126218A CN 106824046 B CN106824046 B CN 106824046B
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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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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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
- C02F2101/103—Arsenic compounds
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Abstract
The invention belongs to water-treatment technology fields, and in particular to a kind of copper cerium codope magnetic composite and its preparation and the application in removing arsenic in water.The present invention is raw material with molysite, mantoquita, cerium salt, and sodium acetate is alkali source, and ethylene glycol is solvent, passes through solvent structure copper cerium codope magnetic composite.The present invention obtains different sizes, the magnetic composite of the bimetal-doped of specific surface area by regulation copper doped, the molar ratio of ce metal salt.The preparation method has many advantages, such as that at low cost, simple process, arsenic absorption property are excellent and are easily achieved Magnetic Isolation, is of great significance for solving the arsenic pollution in water body.
Description
Technical field
The invention belongs to magnetic composite synthesis and water-treatment technology fields, and in particular to a kind of copper cerium codope is magnetic
Composite material and preparation method, and it is used for the application method of water body trivalent arsenic absorption.
Background technique
Arsenic in water body is mainly with the presence of the form of As (V) and As (III).Wherein, the toxicity of As (III) is significantly larger than As
(V), about 60 times, and As (III) is usually in molecular state, it is easier to it migrates, it is difficult to remove.And existing arsenic removal technology
It is most of that there is preferable removal effect to As (V), but to the very limited and poor of As (III).Therefore how effectively to control
Reason arsenic pollution, especially trivalent arsenic problem receive the highest attention of people.
In recent years, nano magnetic material is due to being effectively applied to arsenic-containing waste water with high surface energy, specific surface area
Adsorption treatment, and simple separation can be realized under the action of an external magnetic field, obtain extensive concern.Tang etc.
(J.Mater.Chem.A, 2013,1,830-836) adulterates Fe by the ratio of molysite and magnesium salts in regulation solution, synthesis Mg2O3
And further study absorption property (q to As (III)m=9.3mg/g)；T.M.Thi etc. (Appl.Surf.Sci., 2015,
340,166-172) have studied the Fe of Cu or Mn difference doping level synthesis3O4Influence to the absorption property of arsenic, compared to pure
Fe3O4(qm=30.3mg/g), magnetic material slightly promotes As (III) absorption property after doping and modification, respectively 32.7mg/g
And 36.4mg/g.However existing magnetic material does not all show ideal characterization of adsorption, general adsorption capacity to As in water body (III)
It is all smaller, it limits its application.And since existing magnetic material does not have catalytic activity, it is difficult to realize molecules in solution state As
(III) to the oxidation transformation of ionic state As (V), the adsorbing and removing of As (III) is seriously undermined.It develops novel with high catalytic activity
And the magnetic material of high arsenic adsorptivity is that research is crucial.
Based on this, the present invention proposes the method for copper cerium codope by copper, cerium with catalytic oxidation performance and synergistic effect
For ion doping in magnetic material, prepared magnetic composite not only collects high magnetic, catalysis oxidation and surface function abundant
The characteristics such as group show the performances such as excellent oxidation, absorption, separation in one.
Summary of the invention
The present invention provides a kind of copper cerium codope magnetic composite and its methods for making and using sames.Pass through party's legal system
Standby copper cerium codope magnetic composite has superior magnetic property, big specific surface area, surface functional group abundant, can
It realizes the oxidation transformation of molecules in solution state As (III) to ionic state As (V), there is high catalytic activity, therefore, have excellent
Arsenic adsorption effect, performance are stablized, and have great importance to industrial wastewater and Arsenic Contamination in Groundwater purification.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of preparation method of copper cerium codope magnetic composite, is made by the steps to obtain: first by molysite,
Mantoquita, cerium salt are added mixed dissolution in ethylene glycol solution, are uniformly mixing to obtain transparent yellow-green soln；Then anhydrous vinegar is added
Sour sodium obtains brown particles through solvent thermal reaction, and finally by brown material Magnetic Isolation, washing is dry to get copper cerium codope
Magnetic composite.
The preparation method of the copper cerium codope magnetic composite, the molysite, mantoquita, cerium salt are chlorate
Or nitrate.The molar concentration of molysite is 1-5mM, and molysite and mantoquita initial molar ratio are 10:1-2:1, mantoquita and cerium salt just
Beginning molar ratio is 10:1-1:2.
The preparation method of the copper cerium codope magnetic composite, the molysite, mantoquita, cerium salt total mole number
Molar ratio with anhydrous sodium acetate is 1:3.5-1:6.
The preparation method of the copper cerium codope magnetic composite, addition anhydrous sodium acetate, magnetic agitation 0.5-1h,
Rate is 500-1000rpm.
Mixed solution is gone to high pressure when solvent thermal reaction by the preparation method of the copper cerium codope magnetic composite
In reaction kettle, it is put into baking oven and is reacted at 200-220 DEG C；Reaction time is 6-12h.
Here temperature refers to reaction temperature set by baking oven.Reaction temperature is to influence material synthesized by the present invention
Key factor.When temperature is less than 200 DEG C, substance not can be carried out effective reaction and conversion in initial soln, influence substance
The substance of physicochemical properties, synthesis does not have magnetism, cannot effectively realize easy, quick separating.
The preparation method of the copper cerium codope magnetic composite obtains brown material after solvent thermal reaction is cooling,
Magnetic Isolation, water and ethyl alcohol respectively wash at least 3 times repeatedly, dry, obtain copper cerium codope magnetic composite.
A kind of copper cerium codope magnetic composite, is prepared by above-mentioned method.
The application method of the copper cerium codope magnetic composite, for removing trivalent arsenic in water body.
The copper cerium codope magnetic composite is specifically taken to be added in the aqueous solution containing sodium arsenite, dosage is
0.5g L-1；Arsenic solution initial concentration is 5-100mg g-1, initial pH value 5, after concussion reaction 12h, Magnetic Isolation, filtering.
Beneficial effects of the present invention:
(1) preparation method of copper cerium codope magnetic composite provided by the invention, it is simple process, easy to implement, and
Active component content is high, source is wide, price is low；
(2) copper cerium codope magnetic composite prepared by the present invention shows good oxidation, adsorbs, it can be achieved that As
(III) Efficient Conversion such as efficiently separates at the performances, and its physicochemical properties is stablized, and due to the interaction of cerium copper,
Resistance to deactivation is strong；
Resistance to deactivation can be investigated from the renewable ability of material.According to pertinent literature, single metal
The magnetic composite of doping is relatively poor to the renewable ability of heavy metal ion.As Tang et al. has probed into magnesium doping
Magnetic iron oxide is to the renewable ability of As (III), and after 5 circulation absorptions, the magnetic iron oxide of magnesium doping is to As
(III) adsorption capacity reports the Fe of Cu doping lower than initial 80%, Wang et al.3O4To the circular regeneration effect of As (III)
Fruit, after 6 circulation absorptions, the adsorption effect to As (III) is the 80% of initial capacity.And copper cerium prepared by the present invention is total
Doped magnetic composite material has preferable renewable ability to As (III), after 5 circulation absorptions, to As (III)
Adsorption capacity still can achieve initial 85%.It follows that copper cerium codope magnetic coupling material prepared by the present invention
Material has good resistance to deactivation.
(3) when the copper cerium codope magnetic composite of the method for the present invention preparation is used for the absorption of trivalent arsenic, have excellent
Arsenic absorption property and good chemical stability, resulting magnetic composite be easily recycled, reduce secondary pollution,
It has a good application prospect, is a kind of ideal arsenic-removing adsorption agent.
Detailed description of the invention
Fig. 1 is Copper-cladding Aluminum Bar magnetic composite and copper cerium codope magnetic composite a-f obtained in embodiment 1-6
SEM phenogram；
Fig. 2 is Copper-cladding Aluminum Bar magnetic composite and copper cerium codope magnetic composite a-f obtained in embodiment 1-6
TEM figure；
Fig. 3 is Copper-cladding Aluminum Bar magnetic composite and copper cerium codope magnetic composite obtained in embodiment 1-6 to As
(III) adsorption isotherm；
Fig. 4 is magnetic composite obtained in embodiment 1 and 4 to the adsorption efficiency and oxygenation efficiency of As (III)；
Fig. 5 adsorbs the As 3d XPS after As (III) for copper cerium codope magnetic composite d obtained in embodiment 4
Figure；
Fig. 6 is copper cerium codope magnetic composite d obtained in embodiment 4 to the circulation absorption capacity of As (III).
Specific embodiment
Below to the preparation method of copper cerium codope magnetic composite in the present invention and go water removal in trivalent arsenic application
It is more specifically described.
Embodiment 1: the preparation of Copper-cladding Aluminum Bar magnetic composite:
By 1.35g FeCl3·6H2O, with 0.427g CuCl2·2H236mL ethylene glycol solution is added in O, and ultrasound makes metal
Salt solid sufficiently dissolves, and is uniformly mixed, and 3.6g anhydrous sodium acetate is then added, after being vigorously stirred 30min, goes to autoclave
Interior 200 DEG C of reactions 6h；After being cooled to room temperature, Magnetic Isolation is washed, and 60 DEG C of dry 6h obtain Copper-cladding Aluminum Bar magnetic composite.It is right
Resulting product carries out SEM and TEM characterization, sees Fig. 1 (a) and Fig. 2 (a) respectively.
Embodiment 2
By 1.35g FeCl3·6H2O, 0.427g CuCl2·2H2O and 0.093g CeCl3·7H236mL second two is added in O
Alcoholic solution, ultrasound, dissolves metal salt solid sufficiently, is uniformly mixed (initial copper ion is 10:1 with cerium ion molar ratio), after
And 3.6g anhydrous sodium acetate is added, after being vigorously stirred 30min, go to 200 DEG C of reaction 6h in autoclave；It is cooled to room temperature
Afterwards, Magnetic Isolation, washing, 60 DEG C of dry 6h obtain copper cerium codope magnetic composite.To resulting product carry out SEM and
TEM characterization, is shown in Fig. 1 (b) and Fig. 2 (b) respectively.
Embodiment 3:
By 1.35g FeCl3·6H2O, 0.427g CuCl2·2H2O and 0.186g CeCl3·7H236mL second two is added in O
Alcoholic solution, ultrasound, dissolves metal salt solid sufficiently, is uniformly mixed (initial copper ion is 5:1 with cerium ion molar ratio), then
3.6g anhydrous sodium acetate is added, after being vigorously stirred 30min, goes to 200 DEG C of reaction 6h in autoclave；After being cooled to room temperature,
Magnetic Isolation, washing, 60 DEG C of dry 6h obtain copper cerium codope magnetic composite.And to resulting product carry out SEM and
TEM characterization, is shown in Fig. 1 (c) and Fig. 2 (c) respectively.
Embodiment 4:
By 1.35g FeCl3·6H2O, 0.427g CuCl2·2H2O and 0.372g CeCl3·7H236mL second two is added in O
Alcoholic solution, ultrasound, dissolves metal salt solid sufficiently, is uniformly mixed (initial copper ion is 2.5:1 with cerium ion molar ratio), after
And 3.6g anhydrous sodium acetate is added, after being vigorously stirred 30min, go to 200 DEG C of reaction 6h in autoclave；It is cooled to room temperature
Afterwards, Magnetic Isolation, washing, 60 DEG C of dry 6h obtain copper cerium codope magnetic composite, and carry out SEM to resulting product
And TEM characterization, Fig. 1 (d) and Fig. 2 (d) are seen respectively.
Embodiment 5:
By 1.35g FeCl3·6H2O, 0.427g CuCl2·2H2O and 0.931g CeCl3·7H236mL second two is added in O
Alcoholic solution, ultrasound, dissolves metal salt solid sufficiently, is uniformly mixed (initial copper ion is 1:1 with cerium ion molar ratio), then
3.6g anhydrous sodium acetate is added, after being vigorously stirred 30min, goes to 200 DEG C of reaction 6h in autoclave；After being cooled to room temperature,
Magnetic Isolation, washing, 60 DEG C of dry 6h obtain copper cerium codope magnetic composite, and to resulting product progress SEM and
TEM characterization, is shown in Fig. 1 (e) and Fig. 2 (e) respectively.
Embodiment 6:
By 1.35g FeCl3·6H2O, 0.427g CuCl2·2H2O and 1.862g CeCl3·7H236mL second two is added in O
Alcoholic solution, ultrasound, dissolves metal salt solid sufficiently, is uniformly mixed (initial copper ion is 1:2 with cerium ion molar ratio), then
3.6g anhydrous sodium acetate is added, after being vigorously stirred 30min, goes to 200 DEG C of reaction 6h in autoclave；After being cooled to room temperature,
Magnetic Isolation, washing, 60 DEG C of dry 6h obtain copper cerium codope magnetic composite, and to resulting product progress SEM and
TEM characterization, is shown in Fig. 1 (f) and Fig. 2 (f) respectively.
Embodiment 7:
Under room temperature, with the magnetic composite a-f prepared in 10mg embodiment 1-6 respectively to 20mL As (III) into
Row adsorption experiment.Initial arsenic solution concentration 5-100mg L-1, adjusting the initial pH of solution is 5, reaction time 12h, reaction temperature
It is 25 DEG C.By the mixed solution Magnetic Isolation after reaction, supernatant is taken to measure concentration using ICP-OES.Different proportion magnetism is multiple
Condensation material is shown in Fig. 3 to the adsorption isotherm of As (III).From the figure 3, it may be seen that the increase of the initial concentration with As (III) solution,
Adsorption capacity is continuously increased.In addition, copper cerium codope magnetic composite adsorbs As (III) with the increase of doping cerium amount
Performance presentation first increases the trend reduced afterwards.By Langmuir equation calculation, different proportion copper cerium codope magnetic composite
A, b, c, d, e, f are respectively 36.15mg g to the maximum adsorption capacity of As (III)-1,38.91mg g-1、40.64mg g-1、
93.93mg g-1、139.19mg g-1、71.59mg g-1.The above results show suitable copper, the doping of Ce elements can have
Effect ground improves material to the absorption property of pollutant, further proves copper cerium codope time property composite material prepared by the present invention
With excellent As (III) removal ability.
Embodiment 8
Under room temperature, with the magnetic composite a and d prepared in 10mg embodiment 1 and 4 respectively to 20mL As (III)
Carry out adsorption experiment.Initial arsenic solution concentration 40mg L-1, adjusting the initial pH of solution is 5, and reaction temperature is 25 DEG C.It takes respectively not
Magnetic Isolation is carried out with the mixed solution after the reaction time, takes supernatant using the dense of atomic fluorescence analysis instrument measurement As (III)
Degree.Different proportion magnetic composite is shown in Fig. 4 to the concentration for remaining As (III) in solution after the oxygenation efficiency and absorption of As (III).
As shown in Figure 4, with the extension of reaction time, the concentration of remaining As (III) gradually decreases in solution, and As in solution
(III) oxygenation efficiency constantly increases.Material a made from embodiment 1 is 21.1% to the oxygenation efficiency of As (III) as seen from the figure, real
Applying material d made from example 4 is 39.4%, about the 2 of material a times to the oxygenation efficiency of As (III).In addition, further anti-to adsorbing
Material after answering carries out XPS analysis, and arsenic element occurs in material surface, this shows that arsenic has been adsorbed on material by adsorption process
Surface, and As 3d spectrogram is fitted, there is As (III)-O and As (V)-O in 43.9eV and 45.1eV respectively.By upper
Result is stated it is found that magnetic composite made from copper, cerium codope not only has excellent absorption property to As (III) while can
To realize the efficient oxidation of As (III), the toxicity of arsenic in solution is effectively reduced, mitigates environmental pollution damage.
Embodiment 9
Under room temperature, circular regeneration absorption is carried out to As (III) using the magnetic composite d prepared in embodiment 4
Experiment.Initial arsenic solution concentration 100mg L-1, the concentration of adsorbent is 0.5g/L, and parsing agent uses NaOH solution, adjusts solution
Initial pH is 5, and reaction temperature is 25 DEG C, reaction time 12h.After absorption, using Magnetic Isolation, deionized water is then used
Three times by material washing, it is added to concussion parsing 12h in NaOH desorbed solution.Magnetic Isolation after parsing, washing are adsorbed again, such as
This circulation 5 times.The magnetic composite prepared in embodiment 4, which recycles 5 times, sees Fig. 6 to the adsorption effect of As (III).It can by Fig. 6
Know, with the increase of cycle-index, magnetic composite d declines the adsorption effect of As (III), this is mainly due to inhale
The arsenic being attached on magnetic composite d fails parsing completely in resolving, leads to the original active site obstruction of material, subtracts
Effective active site in few adsorption process.However, after 5 circular regenerations adsorb, the magnetic coupling material of the preparation of embodiment 4
Material d is still able to maintain initial 80% or more to the adsorption effect of As (III), and it is excellent that this illustrates that the material of this method preparation has
The ability of circular regeneration arsenic-adsorbing.
Claims (10)
1. a kind of preparation method of copper cerium codope magnetic composite, which is characterized in that be made by the steps to obtain: first
First by molysite, mixed dissolution in ethylene glycol solution is added in mantoquita, cerium salt, is uniformly mixing to obtain transparent yellow-green soln；Then
Anhydrous sodium acetate is added, obtains brown particles through solvent thermal reaction, finally by brown material Magnetic Isolation, washing, it is dry to get
Copper cerium codope magnetic composite.
2. the preparation method of copper cerium codope magnetic composite according to claim 1, which is characterized in that the iron
Salt, mantoquita, cerium salt are chlorate or nitrate.
3. the preparation method of copper cerium codope magnetic composite according to claim 1, which is characterized in that molysite rubs
Your concentration is 1-5mM, and molysite and mantoquita initial molar ratio are 10:1-2:1, and the initial molar ratio of mantoquita and cerium salt is 10:1-1:
2。
4. the preparation method of copper cerium codope magnetic composite according to claim 1, which is characterized in that the iron
Salt, mantoquita, the total mole number of cerium salt and the molar ratio of anhydrous sodium acetate are 1:3.5-1:6.
5. the preparation method of copper cerium codope magnetic composite according to claim 1, which is characterized in that be added anhydrous
Sodium acetate, magnetic agitation 0.5-1h, rate 500-1000rpm.
6. the preparation method of copper cerium codope magnetic composite according to claim 1, which is characterized in that solvent heat is anti-
At once mixed solution is gone in autoclave, is put into 200-220 DEG C of baking oven and reacts, reaction time 6-12h.
7. the preparation method of copper cerium codope magnetic composite according to claim 1, which is characterized in that solvent heat is anti-
Brown material, Magnetic Isolation are obtained after should cooling down, water and ethyl alcohol respectively wash at least 3 times repeatedly, and it is dry, obtain copper cerium codope magnetic
Property composite material.
8. a kind of copper cerium codope magnetic composite, which is characterized in that be by the described in any item method systems of claim 1-7
Made of standby.
9. the application method of copper cerium codope magnetic composite according to any one of claims 8, which is characterized in that for removing water body
Middle trivalent arsenic.
10. application method according to claim 9, which is characterized in that take the copper cerium codope magnetic composite
It is added in the aqueous solution containing sodium arsenite, dosage is 0.5g L-1；Arsenic solution initial concentration is 5-100mg g-1, initial pH value
It is 5, after concussion reaction 12h, Magnetic Isolation, filtering.
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| CN109759071A (en) * | 2018-12-15 | 2019-05-17 | 扬州海通电子科技有限公司 | A kind of preparation method of cerium dopping magnetic composite nano material |
| CN109569522B (en) * | 2018-12-20 | 2020-03-31 | 吴荣臻 | Iodine adsorption material and preparation method and application thereof |
| CN111085159B (en) * | 2020-01-19 | 2022-11-11 | 江苏中烟工业有限责任公司 | Magnetic nano adsorbent for removing arsenic and preparation method and application thereof |
| CN112717932A (en) * | 2020-12-31 | 2021-04-30 | 武汉理工大学 | Preparation method and application of copper-doped ferric oxide nano disc |
| CN114181068A (en) * | 2021-11-25 | 2022-03-15 | 江西省科学院能源研究所 | Cerium-doped copper oxalate nano material and preparation method thereof |
| CN114887608B (en) * | 2022-04-19 | 2023-11-10 | 北京化大天工科技发展有限公司 | Preparation method of cobalt-doped cerium oxide porous material and application of cobalt-doped cerium oxide porous material in arsenic pollution treatment |
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