CN110142035A - A kind of preparation method and application of the magnetic nanoparticle of poly-dopamine modification - Google Patents
A kind of preparation method and application of the magnetic nanoparticle of poly-dopamine modification Download PDFInfo
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- CN110142035A CN110142035A CN201910437453.3A CN201910437453A CN110142035A CN 110142035 A CN110142035 A CN 110142035A CN 201910437453 A CN201910437453 A CN 201910437453A CN 110142035 A CN110142035 A CN 110142035A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a kind of preparation method and applications of the magnetic nanoparticle of poly-dopamine modification, belong to magnetic nanoparticle technical field of modification.The present invention uses FeCl3·6H2O、Na3C6H5O7·2H2O and CH3COONa prepares nanometer Fe3O4Particle；The pH value for using dilute hydrochloric acid to adjust Tris solution obtains Tris-HCl buffer for 8.0~8.5；By nanometer Fe3O4Particle is added to 5~10min of ultrasonic disperse processing in Tris-HCl buffer and obtains solution A；Dopamine hydrochloride is added to 1~2min of ultrasonic disperse processing in Tris-HCl buffer and obtains solution B；Solution B is added in solution A and under agitation reaction 10~obtain Fe for 24 hours3O4@PDA particle, collects nanometer Fe by external magnetic field3O4@PDA particle is dried in vacuo the magnetic nanoparticle up to poly-dopamine modification respectively with deionized water and ethanol washing 2 times or more.The magnetic nanoparticle that poly-dopamine is modified in the present invention has good biocompatibility, high stability, high-adsorption-capacity and superparamagnetism as heavy metal absorbent.
Description
Technical field
The present invention relates to a kind of preparation method and applications of the magnetic nanoparticle of poly-dopamine modification, belong to magnetic Nano
Granule modified technical field.
Background technique
With industrialized rapid development, the problem of various water pollutions, emerges one after another, heavy metal ion due to its toxicity and
Bio-refractory becomes the key points and difficulties of water harnessing.If heavy metal pollution cannot be handled in time and effectively, meeting
The health of harm ecology and the mankind.Therefore, the heavy metal ion in removal water body, which is that scientific researchers are too impatient to wait, to solve
The problem of.Currently, the administering method of heavy metal has chemical precipitation method, redox in the related water pollution that domestic and foreign scholars propose
Method, ion-exchange, electrolysis method, bioanalysis etc., but there is at high cost, complicated for operation or need specified conditions for these methods
The disadvantages of.
Summary of the invention
It is not easily recycled based on conventional adsorbent and poor biocompatibility, the present invention provides a kind of magnetism of poly-dopamine modification
The magnetic nanoparticle of the preparation method and application of nano particle, poly-dopamine modification of the present invention passes through as heavy metal absorbent
The efficient capture to heavy metal ion is realized using the high poly-dopamine of functional group densities, and is realized by magnetic separation technique
The separation and recovery of adsorbent has good biocompatibility, high stability and high-adsorption-capacity；Poly-dopamine modification of the present invention
Magnetic nanoparticle preparation process it is simple, reaction condition is mild and stability is high, has in field for the treatment of of water pollution wide
Application prospect.
A kind of preparation method of the magnetic nanoparticle of poly-dopamine modification, the specific steps are as follows:
(1) by FeCl3·6H2O、Na3C6H5O7·2H2O and CH3COONa is added in ethylene glycol solution and in ultrasound condition
Lower dissolution, then 30~45min of reaction obtains precursor solution under agitation；
(2) step (1) precursor solution is placed in 8~10h of reaction under the conditions of temperature is 180~200 DEG C and obtains nanometer
Fe3O4Particle is cooled to room temperature, and collects nanometer Fe by external magnetic field3O4Particle is washed 2 times with ethyl alcohol and deionized water respectively
More than；
(3) concentrated hydrochloric acid is add to deionized water and is configured to dilute hydrochloric acid solution, trishydroxymethylaminomethane is dissolved in
Tris solution is obtained in deionized water, the pH value for using dilute hydrochloric acid solution to adjust Tris solution obtains Tris-HCl for 8.0~8.5
Buffer；
(4) nanometer Fe for washing step (2)3O4Particle is added to ultrasonic disperse in the Tris-HCl buffer of step (3)
5~10min of processing obtains solution A；Dopamine hydrochloride is added in the Tris-HCl buffer of step (3) at ultrasonic disperse
1~2min of reason obtains solution B；Solution B is added in solution A and under agitation reaction 10~obtain Fe for 24 hours3O4@PDA
Particle collects nanometer Fe by external magnetic field3O4@PDA particle, uses deionized water and ethanol washing 2 times or more respectively, and vacuum is dry
The dry magnetic nanoparticle up to poly-dopamine modification.
Preferably, FeCl in the step (1)3·6H2O、Na3C6H5O7·2H2O and CH3The mass ratio of COONa is 1.35:
1.00:3.60。
Further, step (1) stirring rate is 750~800rpm.
The concentration of step (3) dilute hydrochloric acid solution is 0.1~0.2mol/L, the concentration of Tris solution is 0.01~
0.015mol/L。
Nanometer Fe in step (4) solution A3O4The concentration of particle is 0.006~0.0135g/mL, dopamine in solution B
The concentration of hydrochloride is 0.003~0.005g/mL.
Step (4) nanometer Fe3O4The mass ratio of particle and dopamine hydrochloride is (1.2~2.7): (1.2~2.0).
The magnetic nanoparticle of the poly-dopamine modification is applied in heavy metal cadmium ion in processing sewage.
The magnetic nanoparticle of poly-dopamine modification application method in heavy metal cadmium ion in processing sewage:
The pH value for adjusting sewage is 5~7, is then added in sewage at the magnetic nanoparticle stirring of poly-dopamine modification
Manage 2~2.5h；The magnetic nanoparticle of poly-dopamine modification and the solid-to-liquid ratio (S:L) of sewage are 2:5.
The magnetic nanoparticle of poly-dopamine modification of the present invention is using magnetic ferroferric oxide nanometer particle as kernel, with poly-
Dopamine is shell, and due to amino and phenolic hydroxyl group rich in poly-dopamine layer, poly-dopamine had both been used as four oxidations
The protection shell of three-iron is also used as modifying agent to be functionalized ferroso-ferric oxide.
Beneficial effects of the present invention:
(1) magnetic nanoparticle of poly-dopamine modification of the present invention is as heavy metal absorbent by using functional group densities
High poly-dopamine realizes that the separation of adsorbent is returned by magnetic separation technique to realize the efficient capture to heavy metal ion
It receives；
(2) magnetic nanoparticle of poly-dopamine modification of the present invention has superparamagnetism, Yi Ci as heavy metal absorbent
The advantages of separation；
(3) magnetic nanoparticle of poly-dopamine modification of the present invention has good bio-compatible as heavy metal absorbent
Property, high stability and high-adsorption-capacity；Cadmium ion in energy efficient capture sewage, stability is high, reusable；
(4) preparation process of the magnetic nanoparticle of poly-dopamine modification of the present invention is simple, and reaction condition is mild and stablizes
Property it is high, have broad application prospects in field for the treatment of of water pollution.
Detailed description of the invention
Fig. 1 is magnetic Fe3O4And Fe3O4The TEM of@PDA nanoparticle schemes: (a) being magnetic Fe3O4Nanoparticle；(b),(c)
It (d) is respectively cladding PDA with a thickness of 10~14nm (embodiment 1), 16~25nm (embodiment 2) and 40~50nm (embodiment
3) magnetic Fe3O4@PDA nanoparticle.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
A kind of embodiment 1: preparation method of the magnetic nanoparticle of poly-dopamine modification, the specific steps are as follows:
(1) by FeCl3·6H2O、Na3C6H5O7·2H2O and CH3COONa is added in ethylene glycol solution and in ultrasound condition
Lower dissolution, then reaction 30min obtains precursor solution under the conditions of stirring rate is 750rpm；Wherein FeCl3·6H2O、
Na3C6H5O7·2H2O and CH3The mass ratio of COONa is 1.35:1.00:3.60；
(2) step (1) precursor solution is placed in reaction 10h under the conditions of temperature is 180 DEG C and obtains nanometer Fe3O4Particle, it is cold
But to room temperature, nanometer Fe is collected by external magnetic field3O4Ethyl alcohol and deionized water washing 2 times or more are respectively adopted in particle；
(3) concentrated hydrochloric acid is add to deionized water and is configured to dilute hydrochloric acid solution, trishydroxymethylaminomethane is dissolved in
Tris solution is obtained in deionized water, is used dilute hydrochloric acid solution to adjust the pH value of Tris solution and is obtained Tris-HCl buffering for 8.0
Liquid；Wherein the concentration of dilute hydrochloric acid solution is 0.1mol/L, and the concentration of Tris solution is 0.01mol/L；
(4) nanometer Fe for washing step (2)3O4Particle is added to ultrasonic disperse in the Tris-HCl buffer of step (3)
Processing 5min obtains solution A；Dopamine hydrochloride is added to ultrasonic disperse in the Tris-HCl buffer of step (3) to handle
1min obtains solution B；Solution B is added in solution A and reaction 10h obtains Fe under the conditions of stirring rate is 350rpm3O4@
PDA particle collects nanometer Fe by external magnetic field3O4@PDA particle uses deionized water and ethanol washing 2 times or more, in temperature respectively
The magnetic nanoparticle Fe that vacuum drying 4h modifies under the conditions of degree is 50 DEG C up to poly-dopamine3O4@PDA；Wherein received in solution A
Rice Fe3O4The concentration of particle is 0.006g/mL, and the concentration of dopamine hydrochloride is 0.003g/mL in solution B；Nanometer Fe3O4?
The mass ratio of grain and dopamine hydrochloride is 1:1；
Magnetic Fe3O4And Fe3O4The TEM figure of@PDA nanoparticle is shown in Fig. 1, Fe in the present embodiment3O4The PDA packet of@PDA particle
It covers with a thickness of 10~14nm；
By magnetic Fe3O4@PDA nanoparticle adsorbent is applied in sewage in the absorption of heavy metal cadmium ion: compound concentration
The cadmium-ion solution for being 5 for 20mg/L, pH value, by Fe3O4(i.e. every 50mL is added with the feed ratio of 20mg/50mL in@PDA adsorbent
20mg Fe is added in cadmium-ion solution3O4@PDA adsorbent), 2 are vibrated under the conditions of temperature is 25 DEG C, stirring rate is 250rpm
~2.5h collects supernatant after Magneto separate adsorbent, and the concentration of residual cadmium ion, gained knot are detected using Atomic absorption (AAS)
Fruit shows that the adsorbent under conditions of temperature is 25 DEG C, pH value is 5, holds the absorption for the cadmium-ion solution that concentration is 20mg/L
Amount is 4.73mg/g.
A kind of embodiment 2: preparation method of the magnetic nanoparticle of poly-dopamine modification, the specific steps are as follows:
(1) by FeCl3·6H2O、Na3C6H5O7·2H2O and CH3COONa is added in ethylene glycol solution and in ultrasound condition
Lower dissolution, then reaction 35min obtains precursor solution under the conditions of stirring rate is 780rpm；Wherein FeCl3·6H2O、
Na3C6H5O7·2H2O and CH3The mass ratio of COONa is 1.35:1.00:3.60；
(2) step (1) precursor solution is placed in reaction 9h under the conditions of temperature is 190 DEG C and obtains nanometer Fe3O4Particle, it is cold
But to room temperature, nanometer Fe is collected by external magnetic field3O4Ethyl alcohol and deionized water washing 2 times or more are respectively adopted in particle；
(3) concentrated hydrochloric acid is add to deionized water and is configured to dilute hydrochloric acid solution, trishydroxymethylaminomethane is dissolved in
Tris solution is obtained in deionized water, is used dilute hydrochloric acid solution to adjust the pH value of Tris solution and is obtained Tris-HCl buffering for 8.2
Liquid；Wherein the concentration of dilute hydrochloric acid solution is 0.15mol/L, and the concentration of Tris solution is 0.012mol/L；
(4) nanometer Fe for washing step (2)3O4Particle is added to ultrasonic disperse in the Tris-HCl buffer of step (3)
Processing 8min obtains solution A；Dopamine hydrochloride is added to ultrasonic disperse in the Tris-HCl buffer of step (3) to handle
1.5min obtains solution B；Solution B is added in solution A and reaction 12h is obtained under the conditions of stirring rate is 350rpm
Fe3O4@PDA particle, collects nanometer Fe by external magnetic field3O4@PDA particle, respectively with deionized water and ethanol washing 2 times with
On, the magnetic nanoparticle Fe that 4h modifies up to poly-dopamine is dried in vacuo under the conditions of temperature is 50 DEG C3O4@PDA；It is wherein molten
Nanometer Fe in liquid A3O4The concentration of particle is 0.0075g/mL, and the concentration of dopamine hydrochloride is 0.0038g/mL in solution B；It receives
Rice Fe3O4The mass ratio of particle and dopamine hydrochloride is 1:1；
Magnetic Fe3O4And Fe3O4The TEM figure of@PDA nanoparticle is shown in Fig. 1, Fe in the present embodiment3O4The PDA packet of@PDA particle
It covers with a thickness of 16~25nm；
By magnetic Fe3O4@PDA nanoparticle adsorbent is applied in sewage in the absorption of heavy metal cadmium ion: compound concentration
The cadmium-ion solution for being 6 for 20mg/L, pH value, by Fe3O4(i.e. every 50mL is added with the feed ratio of 20mg/50mL in@PDA adsorbent
20mg Fe is added in cadmium-ion solution3O4@PDA adsorbent), 2 are vibrated under the conditions of temperature is 25 DEG C, stirring rate is 250rpm
~2.5h collects supernatant after Magneto separate adsorbent, and the concentration of residual cadmium ion, gained knot are detected using Atomic absorption (AAS)
Fruit shows that the adsorbent under conditions of temperature is 25 DEG C, pH value is 6, holds the absorption for the cadmium-ion solution that concentration is 20mg/L
Amount is 5.32mg/g.
A kind of embodiment 3: preparation method of the magnetic nanoparticle of poly-dopamine modification, the specific steps are as follows:
(1) by FeCl3·6H2O、Na3C6H5O7·2H2O and CH3COONa is added in ethylene glycol solution and in ultrasound condition
Lower dissolution, then reaction 45min obtains precursor solution under the conditions of stirring rate is 800rpm；Wherein FeCl3·6H2O、
Na3C6H5O7·2H2O and CH3The mass ratio of COONa is 1.35:1.00:3.60；
(2) step (1) precursor solution is placed in reaction 8h under the conditions of temperature is 200 DEG C and obtains nanometer Fe3O4Particle, it is cold
But to room temperature, nanometer Fe is collected by external magnetic field3O4Ethyl alcohol and deionized water washing 2 times or more are respectively adopted in particle；
(3) concentrated hydrochloric acid is add to deionized water and is configured to dilute hydrochloric acid solution, trishydroxymethylaminomethane is dissolved in
Tris solution is obtained in deionized water, is used dilute hydrochloric acid solution to adjust the pH value of Tris solution and is obtained Tris-HCl buffering for 8.5
Liquid；Wherein the concentration of dilute hydrochloric acid solution is 0.2mol/L, and the concentration of Tris solution is 0.015mol/L；
(4) nanometer Fe for washing step (2)3O4Particle is added to ultrasonic disperse in the Tris-HCl buffer of step (3)
Processing 10min obtains solution A；Dopamine hydrochloride is added to ultrasonic disperse in the Tris-HCl buffer of step (3) to handle
2min obtains solution B；Solution B is added in solution A and is reacted under the conditions of stirring rate is 300rpm and obtains Fe for 24 hours3O4@
PDA particle collects nanometer Fe by external magnetic field3O4@PDA particle uses deionized water and ethanol washing 2 times or more, in temperature respectively
The magnetic nanoparticle Fe that vacuum drying 4h modifies under the conditions of degree is 50 DEG C up to poly-dopamine3O4@PDA；Wherein received in solution A
Rice Fe3O4The concentration of particle is 0.0135g/mL, and the concentration of dopamine hydrochloride is 0.005g/mL in solution B)；Nanometer Fe3O4
The mass ratio of particle and dopamine hydrochloride is 1.35:1；
Magnetic Fe3O4And Fe3O4The TEM figure of@PDA nanoparticle is shown in Fig. 1, Fe in the present embodiment3O4The PDA packet of@PDA particle
It covers with a thickness of 40~50nm；
By magnetic Fe3O4@PDA nanoparticle adsorbent is applied in sewage in the absorption of heavy metal cadmium ion: compound concentration
The cadmium-ion solution for being 7 for 20mg/L, pH value, by Fe3O4(i.e. every 50mL is added with the feed ratio of 20mg/50mL in@PDA adsorbent
20mg Fe is added in cadmium-ion solution3O4@PDA adsorbent), 2 are vibrated under the conditions of temperature is 25 DEG C, stirring rate is 250rpm
~2.5h collects supernatant after Magneto separate adsorbent, and the concentration of residual cadmium ion, gained knot are detected using Atomic absorption (AAS)
Fruit shows that the adsorbent under conditions of temperature is 25 DEG C, pH value is 7, holds the absorption for the cadmium-ion solution that concentration is 20mg/L
Amount is 7.98mg/g；The exposed Fe than under this condition3O4It is high to the adsorption capacity (4.0mg/g) of cadmium, show Fe3O4@PDA absorption
Agent can efficiently remove the cadmium ion in cadmium waste water.
A kind of embodiment 4: application of the magnetic nanoparticle of poly-dopamine modification, the specific steps are as follows:
Magnetic Fe prepared by embodiment 33O4@PDA nanoparticle adsorbent is applied to the suction of heavy metal cadmium ion in sewage
Attached middle school: the cadmium-ion solution that compound concentration 5mg/L, pH value are 7, by Fe3O4@PDA adsorbent is with the feed ratio of 20mg/50mL
It is added and (20mg Fe is added in i.e. every 50mL cadmium-ion solution3O4@PDA adsorbent), temperature is 25 DEG C, stirring rate is
2h is vibrated under the conditions of 250rpm, collects supernatant after Magneto separate adsorbent, and residual cadmium ion is detected using Atomic absorption (AAS)
Concentration, acquired results show the adsorbent under conditions of temperature is 25 DEG C, pH value is 7, to concentration be 5mg/L cadmium ion it is molten
The adsorption capacity of liquid is 2.93mg/g.
A kind of embodiment 5: application of the magnetic nanoparticle of poly-dopamine modification, the specific steps are as follows:
Magnetic Fe prepared by embodiment 33O4@PDA nanoparticle adsorbent is applied to the suction of heavy metal cadmium ion in sewage
Attached middle school: the cadmium-ion solution that compound concentration 10mg/L, pH value are 7, by Fe3O4@PDA adsorbent is with the feed ratio of 20mg/50mL
It is added and (20mg Fe is added in i.e. every 50mL cadmium-ion solution3O4@PDA adsorbent), temperature is 25 DEG C, stirring rate is
2.2h is vibrated under the conditions of 250rpm, collects supernatant after Magneto separate adsorbent, and residual cadmium ion is detected using Atomic absorption (AAS)
Concentration, acquired results show the adsorbent under conditions of temperature is 25 DEG C, pH value is 7, to concentration be 10mg/L cadmium from
The adsorption capacity of sub- solution is 5.08mg/g.
A kind of embodiment 6: application of the magnetic nanoparticle of poly-dopamine modification, the specific steps are as follows:
Magnetic Fe prepared by embodiment 33O4@PDA nanoparticle adsorbent is applied to the suction of heavy metal cadmium ion in sewage
Attached middle school: the cadmium-ion solution that compound concentration 15mg/L, pH value are 7, by Fe3O4@PDA adsorbent is with the feed ratio of 20mg/50mL
It is added and (20mg Fe is added in i.e. every 50mL cadmium-ion solution3O4@PDA adsorbent), temperature is 25 DEG C, stirring rate is
2.5h is vibrated under the conditions of 250rpm, collects supernatant after Magneto separate adsorbent, and residual cadmium ion is detected using Atomic absorption (AAS)
Concentration, acquired results show the adsorbent under conditions of temperature is 25 DEG C, pH value is 7, to concentration be 15mg/L cadmium from
The adsorption capacity of sub- solution is 6.70mg/g.
Claims (6)
1. a kind of preparation method of the magnetic nanoparticle of poly-dopamine modification, which is characterized in that specific step is as follows:
(1) by FeCl3·6H2O、Na3C6H5O7·2H2O and CH3COONa is added in ethylene glycol solution and molten under ultrasound condition
Solution, then 30~45min of reaction obtains precursor solution under agitation；
(2) step (1) precursor solution is placed in reaction kettle, and reacts 8~10h under conditions of temperature is 180~200 DEG C
Obtain nanometer Fe3O4Particle is cooled to room temperature, and collects nanometer Fe by external magnetic field3O4Particle uses ethyl alcohol and deionization respectively
Water washing 2 times or more；
(3) concentrated hydrochloric acid is add to deionized water and is configured to dilute hydrochloric acid solution, by trishydroxymethylaminomethane be dissolved in from
Tris solution is obtained in sub- water, is used dilute hydrochloric acid solution to adjust the pH value of Tris solution and is obtained Tris-HCl buffering for 8.0~8.5
Liquid；
(4) nanometer Fe for washing step (2)3O4Particle is added to ultrasonic disperse in the Tris-HCl buffer of step (3) and handles
5~10min obtains solution A；Dopamine hydrochloride is added to ultrasonic disperse processing 1 in the Tris-HCl buffer of step (3)
~2min obtains solution B；Solution B is added in solution A and under agitation reaction 10~obtain Fe for 24 hours3O4@PDA
Grain, collects nanometer Fe by external magnetic field3O4@PDA particle, respectively with deionized water and ethanol washing 2 times or more, vacuum drying
Up to the magnetic nanoparticle of poly-dopamine modification.
2. the preparation method of the magnetic nanoparticle of poly-dopamine modification according to claim 1, it is characterised in that: step
(1) FeCl in3·6H2O、Na3C6H5O7·2H2O and CH3The mass ratio of COONa is 1.35:1.00:3.60.
3. the preparation method of the magnetic nanoparticle of poly-dopamine modification according to claim 1, it is characterised in that: step
(3) concentration of dilute hydrochloric acid solution is 0.1~0.2mol/L, and the concentration of Tris solution is 0.01~0.015mol/L.
4. the preparation method of the magnetic nanoparticle of poly-dopamine modification according to claim 1, it is characterised in that: step
(4) nanometer Fe in solution A3O4The concentration of particle is 0.006~0.0135g/mL, and the concentration of dopamine hydrochloride is in solution B
0.003~0.005g/mL.
5. the preparation method of the magnetic nanoparticle of poly-dopamine modification according to claim 1, it is characterised in that: step
(4) nanometer Fe3O4The mass ratio of particle and dopamine hydrochloride is (1.2~2.7): (1.2~2.0).
6. the magnetic nanoparticle of the modification of poly-dopamine prepared by any one of Claims 1 to 5 preparation method is being handled
It is applied in heavy metal cadmium ion in sewage.
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