CN108371938A - Mesoporous magnetic Nano iron oxide material, preparation method and applications - Google Patents
Mesoporous magnetic Nano iron oxide material, preparation method and applications Download PDFInfo
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- CN108371938A CN108371938A CN201810435583.9A CN201810435583A CN108371938A CN 108371938 A CN108371938 A CN 108371938A CN 201810435583 A CN201810435583 A CN 201810435583A CN 108371938 A CN108371938 A CN 108371938A
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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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- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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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
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
The invention discloses a kind of mesoporous magnetic Nano iron oxide material, preparation method and applications, by precipitating reagent and Fe2(SO4)3It is soluble in water, it is made into mixed solution, is sealed after stirring evenly and is placed in hydro-thermal in drying box, obtains nano-sized iron oxide presoma precipitation；Then presoma is precipitated at room temperature experience distillation water washing, ethyl alcohol washing, centrifugation successively, then is dried, roasts the obtained adsorbent.The present invention has many advantages, such as that simple for process, preparation condition is mild, raw material is cheap and easy to get.Obtained magnetic Nano iron oxide adsorbent has good adsorption capacity to Cr (VI).
Description
Technical field
The present invention relates to a kind of iron oxide material, preparation method and applications, more particularly to a kind of nano oxidized iron material
Material, preparation method and applications more particularly to a kind of iron oxide Cr (VI) being carried out pollution of chromium processing using absorption method are adsorbed
The preparation method and application of agent are applied to technical field of waste water processing.
Background technology
Heavy metal chromium pollution is mainly derived from the industrial wastewaters such as mining, plating, leather tanning and landfill leachate etc..Chromium exists
Valence state present in water environment is mainly Cr (III) and Cr (VI), and the toxicity of different chromium compounds is different, with the toxicity of Cr (VI)
Maximum, toxicity are 100 times of Cr (III), and the industrial wastewater containing Cr (VI) easily causes the heavy metal chromium of surface water and groundwater
Pollution, causes to seriously endanger to ecological environment.
The data of State Ministry of Environmental Protection shows, the whole nation grain of the underproduction ten thousand tons up to more than 1,000 due to heavy metal pollution every year,
And by nearly 20,000,000 hectares of the cultivated area of the heavy metal pollutions such as chromium, account for about the 1/5 of total cultivated area.Chromium can pass through digestion
The approach such as road, respiratory tract and skin invade human body, are mainly accumulated in liver kidney and incretory, cause slow poisoning, lead to office
Portion organ damage simultaneously further deteriorates, and has strong teratogenesis, carcinogenesis.In addition, ocean aquatile has stronger richness to chromium
Collection ability, chromium concn can make fish be poisoned when being 5mg/L, and when concentration reaches 20mg/L can make fish dead.In view of Cr (VI) dirts
The serious harm of dye, administers it and is just very necessary.
Traditional pollution of chromium treatment technology includes mainly chemical precipitation, reverse osmosis, ion exchange, activated carbon adsorption and coprecipitated
Form sediment etc., but the processing cost of these methods is generally higher, is especially showed when pollutant concentration is relatively low especially prominent.And biography
The wastewater treatment method of system is compared, and absorption method has many advantages, such as easy, easy to operate, high selectivity and versatile, especially
It is capable of the effluent containing heavy metal ions of effective purifying low-concentration.
Recently, patent CN101875003A discloses a kind of preparation method of the absorption resin with Cr ion cavities.It should
Chitosan, the polyethylene glycol polymeric monomer of methacrylic acid list sealing end, acrylic acid bi-end-blocking is added into ethanol water in method
Polyethylene glycol polymeric monomer, photoinitiator, acrylic or methacrylic acid and Cr (III) obtain solid production through ultraviolet light
Object, then it is 7 to adjust its pH through salt acid soak, ammonium hydroxide, drying obtains the absorption resin with Cr ion cavities.But this method is deposited
A large amount of organic solvent, raw material availability are low, process is relatively complicated, reaction condition is realized that difficulty etc. is serious and lacked adding
It falls into.
To sum up, exploitation preparation process is simple, mild condition, has the low of excellent absorption property to hypertoxic pollutant Cr (VI)
Cost adsorbents have important scientific meaning and good application prospect, become technical problem urgently to be resolved hurrily.
Invention content
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
Mesoporous magnetic Nano iron oxide material, preparation method and applications, preparation process is simple, and process conditions are mild, prepared Jie
Hole magnetic Nano iron oxide material has excellent absorption property to hypertoxic pollutant Cr (VI), and has certain magnetism, to reach
The purpose that heavy metal Cr (VI) and solution are completely separated by adsorbent, be one kind have prospect of the application and Low Cost Sorbents prepare and
Application process.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of preparation method of magnetic Nano iron oxide, includes the following steps：
A. prepared by nano-sized iron oxide presoma：
Precipitating reagent and inorganic molysite mixing is soluble in water, it is made into mixed solution, is carried out in drying box after stirring evenly
Hydro-thermal reaction obtains nano-sized iron oxide presoma precipitation；
B. mesoporous magnetic Nano Fe2O3It is prepared by powder：
Using washing of precipitate method, by the presoma prepared in the step a precipitation at room temperature by centrifuging,
Water washing, ethyl alcohol washing are distilled, processing then is dried to presoma, then presoma is subjected to roasting heat treatment, to
To mesoporous magnetic Nano Fe2O3Powder.
In above-mentioned nano-sized iron oxide forerunner production procedure, precipitating reagent used preferably uses CS (NH2)2、CO(NH2)2With
Any one in NaF or arbitrary several mixing material；Inorganic molysite used preferably uses ferric sulfate Fe2(SO4)3。
In above-mentioned nano-sized iron oxide forerunner production procedure, the method for preferably preparing mixed liquor is：Precipitation is weighed respectively
Agent and inorganic molysite dissolve in no less than 80ml water, magnetic agitation at least 30min, form mixed solution.
As currently preferred technical solution, in above-mentioned nano-sized iron oxide forerunner production procedure, by precipitating reagent with
The mixed aqueous solution of inorganic molysite is transferred in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, and reaction kettle is sealed and placed in dry
In dry case, hydro-thermal reaction at least 30h is carried out at not less than 200 DEG C, is then cooled to room temperature, filter out product precipitation, and carry out
It repeatedly cleans repeatedly, until the cleaning solution of product precipitation is in neutrality, then product precipitation is dried, obtains Fe2O3Forerunner
Object powder.
It, at room temperature, will in above-mentioned nano-sized iron oxide forerunner production procedure as currently preferred technical solution
The solution of product takes out from drying box, and the product that hydro-thermal reaction generation is filtered out with sand core funnel precipitates, and is washed with distilled water
The cleaning solution precipitated to product is in neutrality.
As currently preferred technical solution, in above-mentioned nano-sized iron oxide forerunner production procedure, washing will be passed through
Product afterwards is deposited under the constant temperature not less than 60 DEG C dry at least 5h, obtains Fe2O3Predecessor powder.
As currently preferred technical solution, in above-mentioned nano-sized iron oxide forerunner production procedure, in precipitating reagent and
When inorganic molysite is mixed, the mole that inorganic molysite is added is not less than a quarter of precipitating reagent mole.
As currently preferred technical solution, in above-mentioned mesoporous magnetic Nano Fe2O3In powder preparing processes, will before
Drive body carry out roasting heat treatment when, predecessor is placed in Muffle furnace, control heating rate be not less than 4 DEG C/min, not less than
At least 4h is roasted at 450 DEG C to get to mesoporous magnetic Nano Fe2O3Powder.
As currently preferred technical solution, in above-mentioned mesoporous magnetic Nano Fe2O3In powder preparing processes, precipitation is washed
It is experience distillation water washing, centrifugation successively to wash method, is washed twice altogether；Absolute ethyl alcohol washing is undergone again, is centrifuged, then
It washs secondary.
Mesoporous magnetic Nano Fe prepared by a kind of preparation method using magnetic Nano iron oxide of the present invention2O3Material, it is mesoporous
Magnetic Nano Fe2O3Material is in the sand-like pulverulence of dark brown.As currently preferred technical solution, mesoporous magnetic Nano
Fe2O3Contain Fe in material3O4, Fe3O4In mesoporous magnetic Nano Fe2O3Mass percentage content in material is not higher than
30wt.%, at room temperature, mesoporous magnetic Nano Fe2O3The specific saturation magnetization (Ms) of material is not less than 16.28emu/g, rectifys
Stupid power (Hc) is not less than 152.81Oe.Wherein Fe3O4In mesoporous magnetic Nano Fe2O3The activity in mesoporous can be increased in material
Site detaches regeneration convenient for initial adsorbent material to strengthen its adsorption capacity from water body, achievees the purpose that recycling, when
Fe3O4Component is more than upper limit group timesharing, and the anti-caking power of adsorbent is deteriorated, and be easy to cause collapsing for roasting process intermediary pore structure
It collapses or blocks.
Mesoporous magnetic Nano Fe prepared by a kind of preparation method using magnetic Nano iron oxide of the present invention2O3Material is answered
With by mesoporous magnetic Nano Fe2O3Material is as iron oxide Cr (VI) adsorbent, using absorption method, absorption heavy metal ion pollution
Hypertoxic pollutant Cr (VI) in water body；And adsorbent can be made heavy metal Cr (VI) and solution by controlling externally-applied magnetic field
It is detached, purified treatment is carried out to Cr pollutant effluents.
As currently preferred technical solution, by mesoporous magnetic Nano Fe2O3Material is adsorbed as iron oxide Cr (VI)
Agent handles Cr pollutant effluents, as magnetic Nano Fe using absorption method2O3After adsorbent reaches balance to the absorption of Cr (VI), use
Magnet rotor mechanical agitation Cr to be adsorbed (VI) solution, makes magnetic Nano Fe2O3Adsorbent is inhaled on magnet rotor, then will
Magnet rotor takes out from Cr to be adsorbed (VI) solution, to which heavy metal Cr (VI) is detached with the solution after adsorption treatment,
Purified treatment is carried out to Cr pollutant effluents.
As currently preferred technical solution, it is dirty that magnetic Nano iron oxide Cr (VI) adsorbent is applied to absorption severe toxicity
When contaminating object Cr (VI), the pH for adjusting Cr to be adsorbed (VI) solution is 2~3, is not higher than according to the maximal absorptive capacity of adsorbent
The standard of 20.2mg/g weighs the addition that magnetic Nano iron oxide Cr (VI) adsorbent is added to Cr to be adsorbed (VI) solution.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage：
1. the method for the present invention realizes the controllable preparation of magnetic Nano iron oxide adsorbent；
2. the method for the present invention desciccate at a lower temperature, not only reduces energy consumption, but be conducive to keep adsorbent it is stable,
Uniform pore structure；
3. magnetic Nano iron oxide adsorbent prepared by the method for the present invention has magnetic property, by magnetic Nano Fe2O3Adsorbent
It is placed in Cr to be adsorbed (VI) solution under magnet rotor mechanical agitation, can all be inhaled after very short 30s and be turned in magnetism
On son, achieve the purpose that make adsorbent be completely separated heavy metal Cr (VI) with solution by controlling external magnetic field；
4. the method for the present invention preparation process condition is simple and practicable, mild condition, raw material is cheap and easy to get, and prepared magnetism
Nano oxidized iron adsorbent there is good absorption property, the maximal absorptive capacity of adsorbent can reach 20.2mg/L, inhale Cr (VI)
Attached amount is larger, and the rate of adsorption is very fast.
Description of the drawings
Fig. 1 is the embodiment of the present invention one with CS (NH2)2The nanometer Fe prepared for precipitating reagent2O3To the absorption power of Cr (VI)
Learn curve.
Fig. 2 is the embodiment of the present invention two with CS (NH2)2The nanometer Fe prepared for precipitating reagent2O3To the adsorption isotherm of Cr (VI)
Line.
Fig. 3 is the embodiment of the present invention two with CS (NH2)2The nanometer Fe prepared for precipitating reagent2O3To the Langmuir of Cr (VI)
Isothermal adsorption line chart.
Specific implementation mode
Said program is described further below in conjunction with specific examples of the implementation, the preferred embodiment of the present invention is described in detail such as
Under：
Embodiment one
In the present embodiment, a kind of preparation method of magnetic Nano iron oxide, includes the following steps：
A. prepared by nano-sized iron oxide presoma：
Using CS (NH2)2As precipitating reagent, the CS (NH of 0.048mol are weighed2)2With the inorganic molysite Fe of 0.012mol2
(SO4)3It is dissolved in 80ml water, prepares the mixed aqueous solution of precipitating reagent and inorganic molysite, stirred 30min, be transferred to 100ml poly- four
In the stainless steel cauldron of vinyl fluoride substrate, and reaction kettle is sealed and placed in drying box, hydro-thermal reaction is carried out at 200 DEG C
30h, then cooled to room temperature, filters out product precipitation, and repeatedly clean repeatedly, each clear with distilled water and absolute ethyl alcohol
It washes down twice, until the cleaning solution of product precipitation is in neutrality, product is then deposited under 60 DEG C of constant temperature dry 5h, is obtained
Fe2O3Predecessor powder；
B. mesoporous magnetic Nano Fe2O3It is prepared by powder：
Using washing of precipitate method, by the presoma prepared in the step a precipitation, experience is distilled successively at room temperature
Water washing, centrifugation, wash twice altogether；Undergo again absolute ethyl alcohol washing, centrifuge, then wash it is secondary, then to forerunner
Processing is dried in body, then predecessor is placed in Muffle furnace, control heating rate be 4 DEG C/min, in the case where being warming up to 450 DEG C into
Row roasting 4h is to get to mesoporous magnetic Nano Fe2O3Powder.
By to mesoporous magnetic Nano Fe manufactured in the present embodiment2O3Powder is observed, mesoporous magnetic Nano Fe2O3Material
Material is in the sand-like pulverulence of dark brown.
To mesoporous magnetic Nano Fe manufactured in the present embodiment2O3Powder carries out constituent analysis, mesoporous magnetic Nano Fe2O3Material
Contain Fe in material3O4, Fe3O4In mesoporous magnetic Nano Fe2O3Mass percentage content in material is 30wt.%, at room temperature,
Mesoporous magnetic Nano Fe2O3The specific saturation magnetization (Ms) of material is 16.28emu/g, and coercivity (Hc) is 152.81Oe.
Prepare the K of a concentration of 20mg/L of 100ml2Cr2O7In solution to the beaker of 100ml, stirred in room temperature, moderate strength
Mix down the mesoporous magnetic Nano Fe manufactured in the present embodiment for rapidly joining 0.1g2O3Powder inhales magnetic Nano iron oxide Cr (VI)
Attached dose when being applied to absorption severe toxicity pollutant Cr (VI), adjusts the pH of Cr to be adsorbed (VI) solution as 2-3, takes at regular intervals
The suspension of 3ml or so, with the concentration of Cr (VI) in spectrophotometric analysis filtrate, measures 60min after filtering with microporous membrane
When balance, equilibrium adsorption capacity 18.96mg/g are basically reached to the absorption of Cr (VI), curve of adsorption kinetics is shown in Fig. 1.Fig. 1
For with CS (NH2)2The nanometer Fe prepared for precipitating reagent2O3To the curve of adsorption kinetics of Cr (VI), wherein C is in solution on the way
The residual concentration of Cr (VI), mg/L.At room temperature, Cr (VI) concentration is measured using diphenyl carbazide spectrophotometry, is adopted
Ultraviolet-uisible spectrophotometer is Japanese Shimadzu UVmini-1240 types.
Mesoporous magnetic Nano Fe manufactured in the present embodiment2O3Powder improves the texture property of mesoporous material, has aperture collection
In, the advantages that specific surface area is larger；And adsorbent surface will have certain magnetic property, can make suction by controlling external magnetic field
The attached dose of purpose for being completely separated heavy metal Cr (VI) and solution.The present embodiment desciccate at 60 DEG C, both reduces energy consumption,
Be conducive to keep adsorbent stabilization, uniform pore structure again.Magnetic Nano iron oxide adsorbent tool prepared by the present embodiment method
Be magnetic energy, by magnetic Nano Fe2O3Adsorbent is placed in Cr to be adsorbed (VI) solution under magnet rotor mechanical agitation,
All inhaled after the 30s of short period on magnet rotor, can reach by control external magnetic field make adsorbent by heavy metal
The purpose that Cr (VI) is completely separated with solution.The present embodiment preparation process condition is simple and practicable, mild condition, raw material are inexpensively easy
, and prepared magnetic Nano iron oxide adsorbent has good absorption property, the maximum adsorption of adsorbent to Cr (VI)
Amount is up to 20.2mg/L, and adsorbance is larger, the rate of adsorption is very fast.The present embodiment is by precipitating reagent and Fe2(SO4)3It is soluble in water, match
It is sealed at mixed solution, after stirring evenly and is placed in hydro-thermal in drying box, obtain nano-sized iron oxide presoma precipitation；Then forerunner
Body precipitates at room temperature experience distillation water washing, ethyl alcohol washing, centrifugation successively, then is dried, roasts the obtained suction
Attached dose.The present embodiment has many advantages, such as that simple for process, preparation condition is mild, raw material is cheap and easy to get.Obtained magnetism is received
Rice iron oxide adsorbent has good adsorption capacity to Cr (VI).The present embodiment is prepared for for adsorbing hypertoxic pollutant Cr
(VI) high magnetic nano-sized iron oxide Cr (VI) adsorbent has further opened up the technology that chemicals iron oxide is prepared and applied
Field.
Embodiment two
The present embodiment and embodiment one are essentially identical, are particular in that：
In the present embodiment, a kind of preparation method of magnetic Nano iron oxide, includes the following steps：
A. prepared by nano-sized iron oxide presoma：
Using CS (NH2)2As precipitating reagent, the CS (NH of 0.048mol are weighed2)2With the inorganic molysite Fe of 0.012mol2
(SO4)3It is dissolved in 80ml water, prepares the mixed aqueous solution of precipitating reagent and inorganic molysite, stirred 30min, be transferred to 100ml poly- four
In the stainless steel cauldron of vinyl fluoride substrate, and reaction kettle is sealed and placed in drying box, hydro-thermal reaction is carried out at 200 DEG C
30h, then cooled to room temperature, filters out product precipitation, and repeatedly clean repeatedly, each clear with distilled water and absolute ethyl alcohol
It washes down twice, until the cleaning solution of product precipitation is in neutrality, product is then deposited under 60 DEG C of constant temperature dry 5h, is obtained
Fe2O3Predecessor powder；
B. mesoporous magnetic Nano Fe2O3It is prepared by powder：
Using washing of precipitate method, by the presoma prepared in the step a precipitation, experience is distilled successively at room temperature
Water washing, centrifugation, wash twice altogether；Undergo again absolute ethyl alcohol washing, centrifuge, then wash it is secondary, then to forerunner
Processing is dried in body, then predecessor is placed in Muffle furnace, control heating rate be 4 DEG C/min, in the case where being warming up to 450 DEG C into
Row roasting 4h is to get to mesoporous magnetic Nano Fe2O3Powder.
The K of a concentration of 1mg/L, 5mg/L, 10mg/L, 25mg/L, 45mg/L, 100mg/L is respectively configured2Cr2O7Solution is each
In the beaker of 100ml to 100ml, constant room temperature, moderate strength stirring under simultaneously, rapidly join 0.1g the present embodiment prepare
Magnetic Nano Fe2O3Magnetic Nano iron oxide Cr (VI) adsorbent is applied to absorption severe toxicity pollutant Cr (VI) by powder sample
When, the pH for adjusting Cr to be adsorbed (VI) solution is 2-3, after certain time reaches adsorption equilibrium, appropriate amount of suspension is gone to be filtered through micropore
After membrane filtration, with the concentration of Cr (VI) in spectrophotometric analysis filtrate, magnetic Nano Fe is measured2O3The maximum adsorption of adsorbent
Amount is up to 20.2mg/g.
Its adsorption isothermal curve is shown in that Fig. 2, Langmuir absorption isotherms are shown in Fig. 3.Fig. 2 is with CS (NH2)2It is prepared for precipitating reagent
Nanometer Fe2O3To the adsorption isotherm of Cr (VI)；Fig. 3 is with CS (NH2)2The nanometer Fe prepared for precipitating reagent2O3To Cr's (VI)
Langmuir absorption isotherms.In figure 2 and figure 3, Ce is mass concentration when Cr (VI) is balanced, mg/L；Qe is Cr's (VI)
Equilibrium adsorption capacity, mg/g；Langmuir absorption isotherms are：At room temperature, Cr (VI) concentration is adopted
It is measured with diphenyl carbazide spectrophotometry, used ultraviolet-uisible spectrophotometer is Japanese Shimadzu UVmini-1240
Type.As shown in Figure 2, with CS (NH2)2The nanometer Fe prepared for precipitating reagent2O3Adsorbent, to the Cr (VI) of a concentration of 25mg/L
Solution shows maximum equilibrium adsorption capacity, value 20.2mg/g.From the figure 3, it may be seen that with CS (NH2)2It is received for prepared by precipitating reagent
Rice Fe2O3Langmuir models are met to the adsorption isotherm of Cr (VI), it was demonstrated that its absorption behavior mode is inhaled for monolayer chemistry
It is attached, and significant mesoporous characteristic is presented in adsorbent.
The present embodiment is by precipitating reagent and Fe2(SO4)3It is soluble in water, be made into mixed solution, after stirring evenly sealing be placed in it is dry
Hydro-thermal in dry case obtains nano-sized iron oxide presoma precipitation；Then the experience distillation washing successively at room temperature of presoma precipitation
It washs, ethyl alcohol washing, centrifuge, then be dried, roast the obtained adsorbent.The present embodiment have it is simple for process,
The advantages that preparation condition is mild, raw material is cheap and easy to get.Obtained magnetic Nano iron oxide adsorbent has Cr (VI) good
Adsorption capacity.
Embodiment three
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, mesoporous magnetic prepared by the preparation method of the magnetic Nano iron oxide prepared using above-described embodiment
Property nanometer Fe2O3Material, by mesoporous magnetic Nano Fe2O3Material is as iron oxide Cr (VI) adsorbent, using absorption method, absorption
Hypertoxic pollutant Cr (VI) in heavy metal ion polluted-water；And it can make adsorbent will a huge sum of money by controlling externally-applied magnetic field
Belong to Cr (VI) to be detached with solution, purified treatment is carried out to Cr pollutant effluents.
In the present embodiment, as magnetic Nano Fe2O3After adsorbent reaches balance to the absorption of Cr (VI), turned using magnetism
Sub- mechanical agitation Cr to be adsorbed (VI) solution, makes magnetic Nano Fe2O3Adsorbent is inhaled on magnet rotor, then turns magnetism
Son takes out from Cr to be adsorbed (VI) solution, to which heavy metal Cr (VI) is detached with the solution after adsorption treatment, to Cr dirts
It contaminates waste water and carries out purified treatment.
In the present embodiment, magnetic Nano iron oxide Cr (VI) adsorbent is applied to absorption severe toxicity pollutant Cr (VI)
When, the pH for adjusting Cr to be adsorbed (VI) solution is 2~3, and the standard of 20.2mg/g is not higher than according to the maximal absorptive capacity of adsorbent,
Weigh the addition that magnetic Nano iron oxide Cr (VI) adsorbent is added to Cr to be adsorbed (VI) solution.It can realize that mesoporous magnetism is received
Rice Fe2O3Powder accurately adds, and in the case where ensureing that Cr pollutant effluents carries out purified treatment, realizes accurate magnetic Nano oxygen
Change the control of iron Cr (VI) adsorbent amount.
Combination attached drawing of the embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can be with
The purpose of innovation and creation according to the present invention makes a variety of variations, under the Spirit Essence and principle of all technical solutions according to the present invention
Change, modification, replacement, combination or the simplification made, should be equivalent substitute mode, as long as meeting the goal of the invention of the present invention,
Without departing from the mesoporous magnetic Nano iron oxide material of the present invention, the technical principle of preparation method and applications and inventive concept,
Belong to protection scope of the present invention.
Claims (13)
1. a kind of preparation method of magnetic Nano iron oxide, which is characterized in that include the following steps：
A. prepared by nano-sized iron oxide presoma：
Precipitating reagent and inorganic molysite mixing is soluble in water, it is made into mixed solution, carries out hydro-thermal after stirring evenly in drying box
Reaction obtains nano-sized iron oxide presoma precipitation；
B. mesoporous magnetic Nano Fe2O3It is prepared by powder：
Using washing of precipitate method, by the presoma prepared in the step a precipitation at room temperature by centrifuging, distilling
Water washing, ethyl alcohol washing, are then dried processing, then presoma is carried out roasting heat treatment, to be situated between to presoma
Hole magnetic Nano Fe2O3Powder.
2. the preparation method of magnetic Nano iron oxide according to claim 1, it is characterised in that：It is used in the step a
Precipitating reagent uses CS (NH2)2、CO(NH2)2With any one or the arbitrary several mixing material in NaF；Inorganic molysite used
Using ferric sulfate Fe2(SO4)3。
3. the preparation method of magnetic Nano iron oxide according to claim 1, it is characterised in that：In the step a, it will sink
The mixed aqueous solution of shallow lake agent and inorganic molysite is transferred in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate, and simultaneously by reaction kettle sealing
It is placed in drying box, hydro-thermal reaction at least 30h is carried out at not less than 200 DEG C, is then cooled to room temperature, filter out product precipitation,
And repeatedly clean repeatedly, until the cleaning solution of product precipitation is in neutrality, then product precipitation is dried, obtains Fe2O3
Predecessor powder.
4. the preparation method of magnetic Nano iron oxide according to claim 1, it is characterised in that：In the step a, in room
Under temperature, the solution of product is taken out from drying box, the product that hydro-thermal reaction generation is filtered out with sand core funnel precipitates, with distillation
The cleaning solution that water washing is precipitated to product is in neutrality.
5. the preparation method of magnetic Nano iron oxide according to claim 1, it is characterised in that：It, will be through in the step a
The product crossed after washing is deposited under the constant temperature not less than 60 DEG C dry at least 5h, obtains Fe2O3Predecessor powder.
6. the preparation method of magnetic Nano iron oxide according to claim 1, it is characterised in that：In the step a, heavy
When shallow lake agent and inorganic molysite are mixed, the mole that inorganic molysite is added is not less than a quarter of precipitating reagent mole.
7. the preparation method of magnetic Nano iron oxide according to claim 1, it is characterised in that：In the step b, will before
Drive body carry out roasting heat treatment when, predecessor is placed in Muffle furnace, control heating rate be not less than 4 DEG C/min, not less than
At least 4h is roasted at 450 DEG C to get to mesoporous magnetic Nano Fe2O3Powder.
8. the preparation method of magnetic Nano iron oxide according to claim 1, it is characterised in that：In the step b, precipitation
Washing methods is experience distillation water washing, centrifugation successively, is washed twice altogether；Absolute ethyl alcohol washing is undergone again, is centrifuged,
It washs again secondary.
9. mesoporous magnetic Nano Fe prepared by a kind of preparation method using magnetic Nano iron oxide described in claim 12O3Material
Material, it is characterised in that：Mesoporous magnetic Nano Fe2O3Material is in the sand-like pulverulence of dark brown.
10. mesoporous magnetic Nano Fe according to claim 92O3Material, it is characterised in that：Mesoporous magnetic Nano Fe2O3Material
In contain Fe3O4, Fe3O4In mesoporous magnetic Nano Fe2O3Mass percentage content in material is not higher than 30wt.%, in room temperature
Under, mesoporous magnetic Nano Fe2O3The specific saturation magnetization (Ms) of material is not less than 16.28emu/g, and coercivity (Hc) is not less than
152.81Oe。
11. mesoporous magnetic Nano Fe prepared by a kind of preparation method using magnetic Nano iron oxide described in claim 12O3Material
The application of material, it is characterised in that：By mesoporous magnetic Nano Fe2O3Material is as iron oxide Cr (VI) adsorbent, using absorption method,
Adsorb the hypertoxic pollutant Cr (VI) in heavy metal ion polluted-water；And it can make adsorbent will by controlling externally-applied magnetic field
Heavy metal Cr (VI) is detached with solution, and purified treatment is carried out to Cr pollutant effluents.
12. according to mesoporous magnetic Nano Fe described in claim 112O3The application of material, it is characterised in that：As magnetic Nano Fe2O3
After adsorbent reaches balance to the absorption of Cr (VI), using magnet rotor mechanical agitation Cr to be adsorbed (VI) solution, magnetism is made to receive
Rice Fe2O3Adsorbent is inhaled on magnet rotor, then takes out magnet rotor from Cr to be adsorbed (VI) solution, to a huge sum of money
Belong to Cr (VI) to be detached with the solution after adsorption treatment, purified treatment is carried out to Cr pollutant effluents.
13. according to mesoporous magnetic Nano Fe described in claim 112O3The application of material, it is characterised in that：Magnetic Nano is aoxidized
When iron Cr (VI) adsorbent is applied to absorption severe toxicity pollutant Cr (VI), the pH for adjusting Cr to be adsorbed (VI) solution is 2~3, root
It is not higher than the standard of 20.2mg/g according to the maximal absorptive capacity of adsorbent, weighs to Cr to be adsorbed (VI) solution and magnetic Nano oxygen is added
Change the addition of iron Cr (VI) adsorbent.
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Application publication date: 20180807 |