CN106964311A - A kind of magnetic Nano Yi Meng clays for loading nano zero valence iron and preparation method thereof, application - Google Patents
A kind of magnetic Nano Yi Meng clays for loading nano zero valence iron and preparation method thereof, application Download PDFInfo
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- 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
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- 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
- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
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Abstract
The invention discloses a kind of preparation method for the magnetic Nano Yi Meng clays for loading nano zero valence iron, comprise the following steps：(1) deionized water is added in nanometer Yi Meng clays, stable suspension is made；(2) Iron(III) chloride hexahydrate is added in suspension, and adds absolute ethyl alcohol, precursor liquid is obtained after ultrasound and stirring；(3) sodium borohydride or solution of potassium borohydride are prepared, is added drop-wise to dropwise in precursor liquid in a nitrogen atmosphere；(4) obtained product is enriched with magnet, is washed out；(5) product is dried in vacuo, ground, obtain loading the magnetic Nano Yi Meng clay powders of nano zero valence iron.The magnetic Nano Yi Meng clays of the load nano zero valence iron prepared the invention also discloses the above method and its application.The magnetic Nano Yi Meng clays of load nano zero valence iron prepared by the present invention, with good reactivity, have significant treatment effect to chromyl waste water, and external magnetic field separation can be utilized after being disposed.
Description
Technical field
Prepared the present invention relates to nano material and application field, more particularly to a kind of magnetic Nano for loading nano zero valence iron
Yi Meng clays and preparation method thereof, application.
Background technology
With industrial expansion, the pollutant effluents discharge containing heavy metal is increasingly serious, and heavy metal ion difficulty is biodegradable,
Easily it is enriched with by biological chain, great threat is caused to human health.Clay mineral is more conventional environment self-repair material, tool
There are excellent ion exchange and absorption property.Meanwhile, clay mineral has fine particles, wide material sources, low cost and other advantages.
Clay mineral for absorbing heavy metal ions in water is difficult to be enriched with after processing waste water, therefore many researchers exist
Carried magnetic particle on clay, is prepared suitable for utilizing external magnetic field separation, the compound clay of enrichment, such as loading nanometer Fe3O4
Grain, nano zero-valence iron particle, nanometer Fe2O3Particle etc..Chinese patent CN105536752A disclose " a kind of magnetic montmorillonite answer
Close the preparation method of granule adsorbent ", granule adsorbent is prepared by montmorillonite screening modification, to the adsorption effect of cadmium up to 90%
More than.Chinese patent CN102063988A discloses " a kind of magnetic clay material and preparation method thereof ", is preparing inorganic-organic
It is former in surface of clay by the surface chemistry regulating and controlling effect and chemical reaction of surfactant on the basis of composite axis system
Position generation γ-Fe2O3Magnetic nanoparticle, the composite has good absorption and a catalytic performance, and realize absorption with it is outer
The coupling of field strength Magneto separate.
There is nano zero valence iron ferromagnetism also to have in-situ reducing repair ability, can apply to remove water in heavy metal from
Son and in water organic pollution carry out dechlorination, waste water process field have higher value.But nano zero-valence
Iron particle surface can be high, and itself has ferromagnetism, easily reunites.Nano zero valence iron in-situ reducing activity after reunion
Reduction, is unfavorable for it applied to wastewater treatment.Meanwhile, the aerial nano zero valence iron of exposure is easy to oxidation, or even spontaneous combustion.And
Nano zero valence iron dispersiveness can be not only improved using clay mineral load nano zero valence iron, its reunion is reduced, and can also be stablized
Nano zero valence iron, improves its oxidation resistance.Chinese patent CN 102344194X and CN102923835A disclose one kind respectively
Utilize the preparation method of montmorillonite-loaded nano zero valence iron.The composite magnetic clay mineral being made has clay and nano zero valence iron
Advantage, have good adsorption treatment ability.
The shortcoming of prior art is：Clay mineral for loading nano zero valence iron is generally the particle of micron grade, thick
Grain causes preparing Fe2+/Fe3+During saturation clay presoma, Fe2+/Fe3+The longer reaction time is needed to enter clay ore deposit
Between nitride layer, cause presoma preparation efficiency low；In addition, the magnetic mineral of the load nano zero valence iron prepared is smaller, it is unfavorable for
Magneto separate after adsorption treatment.
The content of the invention
In order to overcome the disadvantages mentioned above and deficiency of prior art, nano zero-valence is loaded it is an object of the invention to provide one kind
The magnetic Nano Yi Meng clays of iron, the magnetic coupling clay material with in-situ immobilization ability, adsorption treatment ability is strong, inhales simultaneously
It is attached be disposed after can rapidly be separated by externally-applied magnetic field.
Another object of the present invention is to the preparation side for the magnetic Nano Yi Meng clays for providing above-mentioned load nano zero valence iron
Method, substantially reduces presoma preparation time, improves preparation efficiency.
It is still another object of the present invention to provide the application of the magnetic Nano Yi Meng clays of above-mentioned load nano zero valence iron.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method for the magnetic Nano Yi Meng clays for loading nano zero valence iron, comprises the following steps：
(1) deionized water is added in nanometer Yi Meng clays, stable suspension is made；
(2) Iron(III) chloride hexahydrate solid is added in the suspension described in step (1), and the absolute ethyl alcohol added,
30~60min is stirred in ultrasound and obtains precursor liquid；
(3) compound concentration is 0.4~1.2mol/L sodium borohydride or solution of potassium borohydride, and step is then added drop-wise to dropwise
Suddenly in the precursor liquid that (2) are obtained, nitrogen is passed through during dropwise addition and is protected；Meanwhile, the rotating speed of regulation agitator for 400~
1000r/mim；After completion of dropping, the rotating speed of regulation agitator is 200~400r/mim, continues to react 30~60min；
(4) with the product that reaction is obtained in magnet enriching step (3), then washed respectively with deionized water and absolute ethyl alcohol
Product is multiple；
(5) product obtained in step (4) is dried in vacuo, product after mill-drying, obtains loading nano zero-valence
The magnetic Yi Meng clay powders of iron.
The preparation method of step (1) described suspension is：By solid content be 45~55wt.% nanometers of Yi Meng clays spend from
Sub- water is diluted to solid content for 1~10wt.%, then with vertical high shear dispersion machine 20~60min of high-speed stirred, forms stable
Suspension.
Iron(III) chloride hexahydrate concentration is 0.05~0.20mol/L, Iron(III) chloride hexahydrate and Yi Meng clays in step (2)
Mass ratio be 10:1~10, the volume ratio of deionized water and absolute ethyl alcohol is 1:1~4.
Ultrasonically treated in step (2) to stir simultaneously, ultrasonic power is 50~300W, the rotating speed of agitator for 400~
1000r/min, the time of ultrasonic agitation is 30~60min.
The mol ratio of sodium borohydride or solution of potassium borohydride and Iron(III) chloride hexahydrate is 1~9 in step (3):1, dropwise
When being added drop-wise to the precursor liquid that step (2) is obtained, rate of addition is 0.5~6mL/min.
Step (4) described magnet is Nd-Fe-B rare-earth permanent magnet magnet.
Step (5) vacuum drying, be specially：Drying temperature is 50~80 DEG C, and drying time is 6~12h.
The magnetic Nano Yi Meng clays of nano zero valence iron are loaded, the nano zero valence iron is in the form of scattered spherical particle
It is carried on nanometer Yi Meng clay lamellas.
The application of the magnetic Nano Yi Meng clays of described load nano zero valence iron, for remove the Cr VI in waste water from
Son.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) Yi Meng clays of the present invention, by layer silicate mineral by illite crystal layer and montmorillonite crystal layer along C
Axle is constituted perpendicular to (001) direction, with montmorillonite and illitic double properties.Yi Meng mineral grains are fine, with layer
Sheet-like morphology, favorable dispersibility, ultrasonic field auxiliary is lower to prepare Fe3+Saturation Yi Meng clays are only needed to 0.5~1 hour, with existing skill
Art is compared, and substantially reduces presoma preparation time, improves preparation efficiency.
(2) the magnetic Yi Meng clay intensity of magnetization of the load nano zero valence iron prepared using the method for the present invention is up to
37.71emu/g, meanwhile, the intensity of magnetization of absorption Cr (VI) composite magnetic clay afterwards is improved to 42.32emu/g.Adsorb Cr (VI)
Afterwards, composite magnetic clay can carry out Magneto separate by external magnetic field, reduce post processing cost.
Brief description of the drawings
Fig. 1 is the X-ray powder of the magnetic Yi Meng clays of the load nano zero valence iron prepared in embodiments of the invention 1
Last diffracting spectrum.
Fig. 2 is the scanning electricity of the magnetic Yi Meng clays of the load nano zero valence iron prepared in embodiments of the invention 1
Mirror figure.
Fig. 3 is absorption of the magnetic Yi Meng clays of load nano zero valence iron in embodiments of the invention 1 to Cr in water (VI)
Kinetic curve.
Fig. 4 is the magnetic of the magnetic Yi Meng clays of the front and rear load nano zero valence irons of absorption Cr (VI) of embodiments of the invention 1
Hysteresis line chart.
Fig. 5 is Fig. 4 partial enlarged drawing.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
Prepare the magnetic Nano Yi Meng clays of load nano zero valence iron：
(1) Yi Meng that the nanometer Yi Meng clays slurry preparation for being 50wt.% or so by solid content is 5wt.% into solid content
Clay slurry, then scattered 20 minutes in 1500r/min with vertical high shear dispersion machine, the nanometer Yi Meng for forming stable and uniform is sticked
Earth material is starched.
(2) 160mL absolute ethyl alcohols are added in 40mL 5wt.% Yi Meng clay slurries, 200mL mixed liquors are configured to.
Weigh Iron(III) chloride hexahydrate (FeCl3·6H2O) 4.84g, is then added in Yi Meng clay suspension liquid.Stirred under ultrasonic wave added
Mix 30min and obtain precursor liquid, ultrasonic power is 150W, and the rotating speed of agitator is 300r/min.Nitrogen is passed through during stirring
Protected.
(3) by 2.72g sodium borohydrides (NaBH4) be dissolved in 240mL deionized waters, reducing agent is made.
(4) sodium borohydride solution of step (3) preparation, drop rate is added dropwise in the precursor liquid obtained to step (2) dropwise
For 2mL/min.After completion of dropping, black product is obtained.Regulation stir speed (S.S.) is 200r/min, and 30 points are then persistently stirred again
Clock.Black product is separated from liquid phase with Nd-Fe-B rare-earth permanent magnet magnet, washs black respectively with deionized water and absolute ethyl alcohol
Color product 3 times.Obtained black product is dried in vacuo, dried solid is collected and is ground, obtains loading nanometer
The magnetic Nano Yi Meng clay powders of Zero-valent Iron.
The final product characteristic obtained with the method is as follows：
As shown in figure 1, nano zero valence iron is spherical in shape, a nanometer surface for Yi Meng clays can be dispersed in better, reunited
Significantly reduce.Meanwhile, nanometer Yi Meng clays are stripped into well dispersed lamellar two-dimension nano materials after grinding distribution.
Fig. 2 is the XRD diffraction patterns of the magnetic Yi Meng clays of the nano zero valence iron of the load prepared.44.7 ° are nano zero-valence
The characteristic diffraction peak of iron, the diffraction peaks broadening of nano zero valence iron is obvious, it was demonstrated that the crystallinity of nano zero valence iron is not high.
Cr VI (Cr in waste water is removed using the magnetic Yi Meng clays of load nano zero valence iron manufactured in the present embodiment
(VI)) test：
Leather tanning, is electroplated, and contains substantial amounts of Cr (VI) ion in the waste water of the industry discharge such as steel smelting.Cr (VI) is no
It can be degraded by human body, can accumulate and finally endanger the health of the mankind in the organ of human body.Cr (VI) has proven to a kind of
Carcinogen and there is cause gene mutation and teratogenesis risk.
Adsorption experiment step：
Cr (VI) aqueous solution for preparing of 100mL is added in three-necked flask, by the pH in Cr (VI) aqueous solution adjust to
2.3, add the magnetic Yi Meng clays of the load nano zero valence iron prepared in 100mg embodiments 1.In 30 DEG C of thermostat water bath
Reaction, the rotating speed of regulation agitator is 300r/min.Sampled in different time intervals, sample is separated using rare earth permanent-magnetic material
In magnetic clay.The content for determining Cr (VI) in supernatant is analyzed using ultraviolet-visible spectrophotometer.
As shown in figure 3, in the range of the pH of experiment, can be removed substantially in 60 minutes Cr (VI) whole in solution from
(after the magnetic Yi Meng adsorption treatments through overload nano zero valence iron, Cr (VI) ion concentration in solution is substantially reduced son, and low
In the detection limit of instrument.)
Fig. 4, Fig. 5 are the hysteresis curve of the magnetic Nano Yi Meng clays of load nano zero valence iron before and after absorption Cr (VI), can
There is ferromagnetism with the magnetic Nano Yi Meng clays for finding out load nano zero valence iron, and adsorb after Cr (VI), magnetic also slightly has
Enhancing.
Embodiment 2
Prepare the magnetic Nano Yi Meng clays of load nano zero valence iron：
(1) Yi Meng that the nanometer Yi Meng clays slurry preparation for being 45wt.% or so by solid content is 2wt.% into solid content
Clay slurry, then disperses 30min in 500r/min with vertical high shear dispersion machine, forms the nanometer Yi Meng clays of stable and uniform
Slurry.
(2) 100mL absolute ethyl alcohols are added in 100mL 2wt.% Yi Meng clay slurries, 200mL mixed liquors are configured to.
Weigh Iron(III) chloride hexahydrate (FeCl3·6H2O) 4.84g, is then added in Yi Meng clay suspension liquid.Stirred under ultrasonic wave added
Mix 30min and obtain precursor liquid, ultrasonic power is 100W, and the rotating speed of agitator is 500r/min.Nitrogen is passed through during stirring
Protected.
(3) by 2.72g sodium borohydrides (NaBH4) be dissolved in 120mL deionized waters, reducing agent is made.
(4) sodium borohydride solution of step (3) preparation, drop rate is added dropwise in the precursor liquid obtained to step (2) dropwise
For 2mL/min.After completion of dropping, black product is obtained.Regulation stir speed (S.S.) is 200r/min, and 30min is then persistently stirred again.
Black product is separated from liquid phase with Nd-Fe-B rare-earth permanent magnet magnet, black production is washed respectively with deionized water and absolute ethyl alcohol
Thing 3 times.Obtained black product is dried in vacuo, dried solid is collected and is ground, obtains loading nano zero-valence
The magnetic Nano Yi Meng clay powders of iron.
The magnetic Nano Yi Meng clay powder body examination test results and the class of embodiment 1 of load nano zero valence iron manufactured in the present embodiment
Seemingly, it will not be repeated here.
Embodiment 3
Prepare the magnetic Nano Yi Meng clays of load nano zero valence iron：
(1) Yi Meng that the nanometer Yi Meng clays slurry preparation for being 45wt.% or so by solid content is 10wt.% into solid content
Clay slurry, then disperses 60min with vertical high shear dispersion machine in 1000r/min, and the nanometer Yi Meng for forming stable and uniform is sticked
Earth material is starched.
(2) 160mL absolute ethyl alcohols are added in 40mL 10wt.% Yi Meng clay slurries, 200mL mixed liquors are configured to.
Weigh Iron(III) chloride hexahydrate (FeCl3·6H2O) 9.68g, is then added in Yi Meng clay suspension liquid.Stirred under ultrasonic wave added
Mix 60min and obtain precursor liquid, ultrasonic power is 250W, and the rotating speed of agitator is 500r/min.Nitrogen is passed through during stirring
Protected.
(3) by 6.72g sodium borohydrides (NaBH4) be dissolved in 240mL deionized waters, reducing agent is made.
(4) sodium borohydride solution of step (3) preparation, drop rate is added dropwise in the precursor liquid obtained to step (2) dropwise
For 4mL/min.After completion of dropping, black product is obtained.Regulation stir speed (S.S.) is 200r/min, and 60min is then persistently stirred again.
Black product is separated from liquid phase with Nd-Fe-B rare-earth permanent magnet magnet, black production is washed respectively with deionized water and absolute ethyl alcohol
Thing 3 times.Obtained black product is dried in vacuo, dried solid is collected and is ground, obtains loading nano zero-valence
The magnetic Nano Yi Meng clay powders of iron.
The magnetic Nano Yi Meng clay powder body examination test results and the class of embodiment 1 of load nano zero valence iron manufactured in the present embodiment
Seemingly, it will not be repeated here.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by the embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method for the magnetic Nano Yi Meng clays for loading nano zero valence iron, it is characterised in that comprise the following steps：
(1) deionized water is added in nanometer Yi Meng clays, stable suspension is made；
(2) Iron(III) chloride hexahydrate solid is added in the suspension described in step (1), and the absolute ethyl alcohol added, in ultrasound
30~60min of middle stirring obtains precursor liquid；
(3) compound concentration is 0.4~1.2mol/L sodium borohydride or solution of potassium borohydride, and step is then added drop-wise to dropwise
(2) in the precursor liquid obtained, during dropwise addition nitrogen is passed through to be protected；Meanwhile, the rotating speed of regulation agitator for 400~
1000r/mim；After completion of dropping, the rotating speed of regulation agitator is 200~400r/mim, continues to react 30~60min；
(4) with the product that reaction is obtained in magnet enriching step (3), then with deionized water and absolute ethyl alcohol difference washed product
Repeatedly；
(5) product obtained in step (4) is dried in vacuo, product after mill-drying, obtains loading nano zero valence iron
Magnetic Yi Meng clay powders.
2. the preparation method of the magnetic Nano Yi Meng clays of load nano zero valence iron according to claim 1, its feature exists
In the preparation method of step (1) described suspension is：It is 45~55wt.% nanometers of Yi Meng clay deionized waters by solid content
Solid content is diluted to for 1~10wt.%, then with vertical high shear dispersion machine 20~60min of high-speed stirred, stable hang is formed
Supernatant liquid.
3. the preparation method of the magnetic Nano Yi Meng clays of load nano zero valence iron according to claim 1, its feature exists
In Iron(III) chloride hexahydrate concentration is 0.05~0.20mol/L, the matter of Iron(III) chloride hexahydrate and Yi Meng clays in step (2)
Amount is than being 10:1~10, the volume ratio of deionized water and absolute ethyl alcohol is 1:1~4.
4. the preparation method of the magnetic Nano Yi Meng clays of load nano zero valence iron according to claim 1, its feature exists
In, ultrasonically treated in step (2) to stir simultaneously, ultrasonic power is 50~300W, and the rotating speed of agitator is 400~1000r/min,
The time of ultrasonic agitation is 30~60min.
5. the preparation method of the magnetic Nano Yi Meng clays of load nano zero valence iron according to claim 1, its feature exists
In the mol ratio of sodium borohydride or solution of potassium borohydride and Iron(III) chloride hexahydrate is 1~9 in step (3):1, it is added drop-wise to dropwise
During the precursor liquid that step (2) is obtained, rate of addition is 0.5~6mL/min.
6. the preparation method of the magnetic Nano Yi Meng clays of load nano zero valence iron according to claim 1, its feature exists
In step (4) described magnet is Nd-Fe-B rare-earth permanent magnet magnet.
7. the preparation method of the magnetic Nano Yi Meng clays of load nano zero valence iron according to claim 1, its feature exists
In step (5) vacuum drying is specially：Drying temperature is 50~80 DEG C, and drying time is 6~12h.
8. the preparation method of the magnetic Nano Yi Meng clays of any one of the claim 1~7 load nano zero valence iron is prepared into
The magnetic Nano Yi Meng clays of the load nano zero valence iron arrived, it is characterised in that the nano zero valence iron is with scattered spherical
The form of grain is carried on nanometer Yi Meng clay lamellas.
9. the application of the magnetic Nano Yi Meng clays of the load nano zero valence iron described in claim 8, it is characterised in that for taking off
Except the hexavalent chromium in waste water.
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| CN108033540A (en) * | 2017-11-06 | 2018-05-15 | 华南师范大学 | A kind of method that crystalline substance glue load nano zero-valence iron composite material removes heavy metal chromium |
| CN108160047A (en) * | 2018-01-02 | 2018-06-15 | 广东佳德环保科技有限公司 | A kind of coal-fired flue-gas goes the preparation method of the modified zeolite of the load nano zero valence iron of lead |
| WO2018166238A1 (en) * | 2017-03-16 | 2018-09-20 | 华南理工大学 | Zero-valent iron pillared montmorillonite repair material, and preparation method therefor and application thereof |
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| CN114367272A (en) * | 2021-12-09 | 2022-04-19 | 华东交通大学 | Preparation method of magnetic nano modified walnut shell adsorbent and application of magnetic nano modified walnut shell adsorbent in treatment of hexavalent chromium in soil |
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